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Sample records for resolution transmission electron

  1. Image Resolution in Scanning Transmission Electron Microscopy

    SciTech Connect

    Pennycook, S. J.; Lupini, A.R.

    2008-06-26

    Digital images captured with electron microscopes are corrupted by two fundamental effects: shot noise resulting from electron counting statistics and blur resulting from the nonzero width of the focused electron beam. The generic problem of computationally undoing these effects is called image reconstruction and for decades has proved to be one of the most challenging and important problems in imaging science. This proposal concerned the application of the Pixon method, the highest-performance image-reconstruction algorithm yet devised, to the enhancement of images obtained from the highest-resolution electron microscopes in the world, now in operation at Oak Ridge National Laboratory.

  2. High Resolution Transmission Electron Microscopy (HRTEM) of nanophase ferric oxides

    NASA Technical Reports Server (NTRS)

    Golden, D. C.; Morris, R. V.; Ming, D. W.; Lauer, H. V., Jr.

    1994-01-01

    Iron oxide minerals are the prime candidates for Fe(III) signatures in remotely sensed Martian surface spectra. Magnetic, Mossbauer, and reflectance spectroscopy have been carried out in the laboratory in order to understand the mineralogical nature of Martian analog ferric oxide minerals of submicron or nanometer size range. Out of the iron oxide minerals studied, nanometer sized ferric oxides are promising candidates for possible Martian spectral analogs. 'Nanophase ferric oxide (np-Ox)' is a generic term for ferric oxide/oxihydroxide particles having nanoscale (less than 10 nm) particle dimensions. Ferrihydrite, superparamagnetic particles of hematite, maghemite and goethite, and nanometer sized particles of inherently paramagnetic lepidocrocite are all examples of nanophase ferric oxides. np-Ox particles in general do not give X-ray diffraction (XRD) patterns with well defined peaks and would often be classified as X-ray amorphous. Therefore, different np-Oxs preparations should be characterized using a more sensitive technique e.g., high resolution transmission electron microscopy (HRTEM). The purpose of this study is to report the particle size, morphology and crystalline order, of five np-Ox samples by HRTEM imaging and electron diffraction (ED).

  3. Computer simulation of high resolution transmission electron micrographs: theory and analysis

    SciTech Connect

    Kilaas, R.

    1985-03-01

    Computer simulation of electron micrographs is an invaluable aid in their proper interpretation and in defining optimum conditions for obtaining images experimentally. Since modern instruments are capable of atomic resolution, simulation techniques employing high precision are required. This thesis makes contributions to four specific areas of this field. First, the validity of a new method for simulating high resolution electron microscope images has been critically examined. Second, three different methods for computing scattering amplitudes in High Resolution Transmission Electron Microscopy (HRTEM) have been investigated as to their ability to include upper Laue layer (ULL) interaction. Third, a new method for computing scattering amplitudes in high resolution transmission electron microscopy has been examined. Fourth, the effect of a surface layer of amorphous silicon dioxide on images of crystalline silicon has been investigated for a range of crystal thicknesses varying from zero to 2 1/2 times that of the surface layer.

  4. Practical Considerations for High Spatial and Temporal Resolution Dynamic Transmission Electron Microscopy

    SciTech Connect

    Armstrong, M; Boyden, K; Browning, N D; Campbell, G H; Colvin, J D; DeHope, B; Frank, A M; Gibson, D J; Hartemann, F; Kim, J S; King, W E; LaGrange, T B; Pyke, B J; Reed, B W; Shuttlesworth, R M; Stuart, B C; Torralva, B R

    2006-05-01

    Although recent years have seen significant advances in the spatial resolution possible in the transmission electron microscope (TEM), the temporal resolution of most microscopes is limited to video rate at best. This lack of temporal resolution means that our understanding of dynamic processes in materials is extremely limited. High temporal resolution in the TEM can be achieved, however, by replacing the normal thermionic or field emission source with a photoemission source. In this case the temporal resolution is limited only by the ability to create a short pulse of photoexcited electrons in the source, and this can be as short as a few femtoseconds. The operation of the photo-emission source and the control of the subsequent pulse of electrons (containing as many as 5 x 10{sup 7} electrons) create significant challenges for a standard microscope column that is designed to operate with a single electron in the column at any one time. In this paper, the generation and control of electron pulses in the TEM to obtain a temporal resolution <10{sup -6} s will be described and the effect of the pulse duration and current density on the spatial resolution of the instrument will be examined. The potential of these levels of temporal and spatial resolution for the study of dynamic materials processes will also be discussed.

  5. Installation of electric field electron beam blanker in high-resolution transmission electron microscopy

    SciTech Connect

    Hayashida, Misa; Kimura, Yoshihide; Taniguchi, Yoshifumi; Otsuka, Masayuki; Takai, Yoshizo

    2006-11-15

    We have newly installed an electric field electron beam blanker in a transmission electron microscopy, which chops an electron beam very quickly without the effect of hysteresis. The electric field, which is generated by the electron beam blanker, deflects the electron beam, and the electron beam is intercepted by an aperture. The response time of the beam blanker is 50 {mu}s. Therefore, a very short pulsed electron beam enables a charge-coupled device camera to directly expose an electron beam spot or diffraction pattern. Moreover, we measured the response of a deflector coil, which is usually used as an electron beam blanker, using our electron beam blanker. Our beam blanker will become a key component in a computer-assisted minimal dose system, which enables us to reduce the electron dose of the sample.

  6. New area detector for atomic-resolution scanning transmission electron microscopy.

    PubMed

    Shibata, Naoya; Kohno, Yuji; Findlay, Scott D; Sawada, Hidetaka; Kondo, Yukihito; Ikuhara, Yuichi

    2010-01-01

    A new area detector for atomic-resolution scanning transmission electron microscopy (STEM) is developed and tested. The circular detector is divided into 16 segments which are individually optically coupled with photomultiplier tubes. Thus, 16 atomic-resolution STEM images which are sensitive to the spatial distribution of scattered electrons on the detector plane can be simultaneously obtained. This new detector can be potentially used not only for the simultaneous formation of common bright-field, low-angle annular dark-field and high-angle annular dark-field images, but also for the quantification of images by detecting the full range of scattered electrons and even for exploring novel atomic-resolution imaging modes by post-processing combination of the individual images. PMID:20406732

  7. Atomic-resolution scanning transmission electron microscopy through 50-nm-thick silicon nitride membranes

    SciTech Connect

    Ramachandra, Ranjan; Jonge, Niels de; Demers, Hendrix

    2011-02-28

    Silicon nitride membranes can be used for windows of environmental chambers for in situ electron microscopy. We report that aberration corrected scanning transmission electron microscopy (STEM) achieved atomic resolution on gold nanoparticles placed on both sides of a 50-nm-thick silicon nitride membrane at 200 keV electron beam energy. Spatial frequencies of 1/1.2 A were visible for a beam semi-angle of 26.5 mrad. Imaging though a 100-nm-thick membrane was also tested. The achieved imaging contrast was evaluated using Monte Carlo simulations of the STEM imaging of a sample of with a representative geometry and composition.

  8. Nanoscale deformation analysis with high-resolution transmission electron microscopy and digital image correlation

    DOE PAGESBeta

    Wang, Xueju; Pan, Zhipeng; Fan, Feifei; Wang, Jiangwei; Liu, Yang; Mao, Scott X.; Zhu, Ting; Xia, Shuman

    2015-09-10

    We present an application of the digital image correlation (DIC) method to high-resolution transmission electron microscopy (HRTEM) images for nanoscale deformation analysis. The combination of DIC and HRTEM offers both the ultrahigh spatial resolution and high displacement detection sensitivity that are not possible with other microscope-based DIC techniques. We demonstrate the accuracy and utility of the HRTEM-DIC technique through displacement and strain analysis on amorphous silicon. Two types of error sources resulting from the transmission electron microscopy (TEM) image noise and electromagnetic-lens distortions are quantitatively investigated via rigid-body translation experiments. The local and global DIC approaches are applied for themore » analysis of diffusion- and reaction-induced deformation fields in electrochemically lithiated amorphous silicon. As a result, the DIC technique coupled with HRTEM provides a new avenue for the deformation analysis of materials at the nanometer length scales.« less

  9. Nanoscale deformation analysis with high-resolution transmission electron microscopy and digital image correlation

    SciTech Connect

    Wang, Xueju; Pan, Zhipeng; Fan, Feifei; Wang, Jiangwei; Liu, Yang; Mao, Scott X.; Zhu, Ting; Xia, Shuman

    2015-09-10

    We present an application of the digital image correlation (DIC) method to high-resolution transmission electron microscopy (HRTEM) images for nanoscale deformation analysis. The combination of DIC and HRTEM offers both the ultrahigh spatial resolution and high displacement detection sensitivity that are not possible with other microscope-based DIC techniques. We demonstrate the accuracy and utility of the HRTEM-DIC technique through displacement and strain analysis on amorphous silicon. Two types of error sources resulting from the transmission electron microscopy (TEM) image noise and electromagnetic-lens distortions are quantitatively investigated via rigid-body translation experiments. The local and global DIC approaches are applied for the analysis of diffusion- and reaction-induced deformation fields in electrochemically lithiated amorphous silicon. As a result, the DIC technique coupled with HRTEM provides a new avenue for the deformation analysis of materials at the nanometer length scales.

  10. Correlative super-resolution fluorescence and metal replica transmission electron microscopy

    PubMed Central

    Sochacki, Kem A.; Shtengel, Gleb; van Engelenburg, Schuyler B.; Hess, Harald F.; Taraska, Justin W.

    2014-01-01

    Super-resolution localization microscopy is combined with a complementary imaging technique, transmission electron microscopy of metal replicas, to locate proteins on the landscape of the cellular plasma membrane at the nanoscale. Robust correlation on the scale of 20 nm is validated by imaging endogenous clathrin (with 2D and 3D PALM/TEM) and the method is further used to find the previously unknown 3D position of epsin on clathrin coated structures. PMID:24464288

  11. Atomic Resolution Transmission Electron Microscopy of Defects in Hexagonal Boron Nitride and Graphene

    NASA Astrophysics Data System (ADS)

    Gibb, Ashley; Alem, Nasim; Song, Chengyu; Ciston, Jim; Zettl, Alex

    2014-03-01

    Monolayer sheets of sp2-bonded materials such as graphene and hexagonal boron nitride (h-BN) have been studied extensively due to their properties including high mechanical strength, thermal conductivity, stability, interesting electronic properties, and potential for integration into novel devices. Understanding the atomic scale structure of defects in these materials is important because defects can significantly affect the physical properties in these materials. In particular, understanding the dynamics of these defects explains much about the material's stability. We have synthesized h-BN and graphene using low pressure chemical vapor deposition and imaged defects using atomic resolution aberration corrected transmission electron microscopy.

  12. The probe profile and lateral resolution of scanning transmission electron microscopy of thick specimens.

    PubMed

    Demers, Hendrix; Ramachandra, Ranjan; Drouin, Dominique; de Jonge, Niels

    2012-06-01

    Lateral profiles of the electron probe of scanning transmission electron microscopy (STEM) were simulated at different vertical positions in a micrometers-thick carbon sample. The simulations were carried out using the Monte Carlo method in CASINO software. A model was developed to fit the probe profiles. The model consisted of the sum of a Gaussian function describing the central peak of the profile and two exponential decay functions describing the tail of the profile. Calculations were performed to investigate the fraction of unscattered electrons as a function of the vertical position of the probe in the sample. Line scans were also simulated over gold nanoparticles at the bottom of a carbon film to calculate the achievable resolution as a function of the sample thickness and the number of electrons. The resolution was shown to be noise limited for film thicknesses less than 1 μm. Probe broadening limited the resolution for thicker films. The validity of the simulation method was verified by comparing simulated data with experimental data. The simulation method can be used as quantitative method to predict STEM performance or to interpret STEM images of thick specimens. PMID:22564444

  13. Soot Nanostructure: Using Fringe Analysis Software on High Resolution Transmission Electron Microscopy of Carbon Soot

    NASA Technical Reports Server (NTRS)

    King, James D.

    2004-01-01

    Using high resolution transmission electron images of carbon nanotubes and carbon particles, we are able to use image analysis program to determine several carbon fringe properties, including length, separation, curvature and orientation. Results are shown in the form of histograms for each of those quantities. The combination of those measurements can give a better indication of the graphic structure within nanotubes and particles of carbon and can distinguish carbons based upon fringe properties. Carbon with longer, straighter and closer spaced fringes are considered graphite, while amorphous carbon contain shorter, less structured fringes.

  14. Crack tip shielding observed with high-resolution transmission electron microscopy

    PubMed Central

    Adhika, Damar Rastri; Tanaka, Masaki; Daio, Takeshi; Higashida, Kenji

    2015-01-01

    The dislocation shielding field at a crack tip was experimentally proven at the atomic scale by measuring the local strain in front of the crack tip using high-resolution transmission electron microscopy (HRTEM) and geometric phase analysis (GPA). Single crystalline (110) silicon wafers were employed. Cracks were introduced using a Vickers indenter at room temperature. The crack tip region was observed using HRTEM followed by strain measurements using GPA. The measured strain field at the crack tip was compressive owing to dislocation shielding, which is in good agreement with the strain field calculated from elastic theory. PMID:26115957

  15. High-resolution transmission electron microscopy with an electrostatic Zach phase plate

    NASA Astrophysics Data System (ADS)

    Hettler, S.; Dries, M.; Zeelen, J.; Oster, M.; Schröder, R. R.; Gerthsen, D.

    2016-05-01

    A new method to control lattice-fringe contrast in high-resolution transmission electron microscopy (HRTEM) images by the implementation of a physical phase plate (PP) is proposed. PPs are commonly used in analogy to Zernike PPs in light microscopy to enhance the phase contrast of weak-phase objects with nm-sized features, which often occur in life science applications. Such objects otherwise require strong defocusing, which leads to a degradation of the instrumental resolution and impedes intuitive image interpretation. The successful application of an electrostatic Zach PP in HRTEM is demonstrated by the investigation of single crystalline Si and Ge samples. The influence of the Zach PP on the image formation process is assessed by analyzing the amplitudes of (111) reflections in power spectra which show a cosine-type dependence on the induced phase shift under certain conditions as predicted by theory.

  16. Computer Simulation of High Resolution Transmission Electron Micrographs: Theory and Analysis.

    NASA Astrophysics Data System (ADS)

    Kilaas, Roar

    Computer simulation of electron micrographs is an invaluable aid in their proper interpretation and in defining optimum conditions for obtaining images experimentally. Since modern instruments are capable of atomic resolution, simulation techniques employing high precision are required. This thesis makes contributions to four specific areas of this field. First, the validity of a new method for simulating high resolution electron microscope images has been critically examined. This method, which has been termed the real space method (RSP) since the entire calculation is performed without any Fourier transforms, offers a considerable reduction in computing time over the conventional multislice approach when identical sampling conditions are employed. However, for the same level of accuracy the real space method requires more sampling points and more computing time than the conventional multislice method. These characteristics are illustrated with calculated results using both methods to identify practical limitations. Second, three different methods for computing scattering amplitudes in High Resolution Transmission Electron Microscopy (HRTEM) have been investigated as to their ability to include upper Laue layer (ULL) interaction. The conventional first order multislice method using fast Fourier transform (FFT) and the second order multislice (SOM) method are shown to yield calculated intensities of first order Laue reflections with the use of slice thicknesses smaller than the crystal periodicity along the incident electron beam direction. It is argued that the calculated intensities of ULL reflections approach the correct values in the limiting case of vanishing slice thickness and electron wavelength. The third method, the improved phasegrating method (IPG) does also in principle include ULL effects, but is severely limited as to choice of slice thickness and sampling interval. A practical way to use slice thicknesses less than the crystal periodicity along the

  17. Contrast transfer and resolution limits for sub-angstrom high-resolution transmission electron microscopy.

    PubMed

    Lentzen, Markus

    2008-02-01

    The optimum imaging of an object structure at the sub-angstrom length scale requires precise adjustment of the lens aberrations of a high-resolution instrument up to the fifth order. A least-squares optimization of defocus aberration C1, third-order spherical aberration C3, and fifth-order spherical aberration C5 yields two sets of aberration coefficients for strong phase contrast up to the information limit: one for variable C1 and C3, at fixed C5, another for variable C1, C3, and C5. An additional correction to the defocus aberration, dependent on object thickness, is described, which becomes important for the use of image simulation programs in predicting optimum high-resolution contrast from thin objects at the sub-angstrom scale. For instruments with a sub-angstrom information limit the ultimate structure resolution, the power to resolve adjacent atom columns in a crystalline object, depends on both the instrumental pointspread and an object pointspread due to finite width of the atomic column potentials. A simulation study on a simple double-column model yields a range for structure resolutions, dependent on the atomic scattering power, from 0.070 nm down to 0.059 nm, for a hypothetical 300-kV instrument with an information limit of 0.050 nm. PMID:18096097

  18. Transient Thermometry and High-Resolution Transmission Electron Microscopy Analysis of Filamentary Resistive Switches.

    PubMed

    Kwon, Jonghan; Sharma, Abhishek A; Chen, Chao-Yang; Fantini, Andrea; Jurczak, Malgorzata; Herzing, Andrew A; Bain, James A; Picard, Yoosuf N; Skowronski, Marek

    2016-08-10

    We present data on the filament size and temperature distribution in Hf0.82Al0.18Ox-based Resistive Random Access Memory (RRAM) devices obtained by transient thermometry and high-resolution transmission electron microscopy (HRTEM). The thermometry shows that the temperature of the nonvolatile conducting filament can reach temperatures as high as 1600 K at the onset of RESET at voltage of 0.8 V and power of 40 μW. The size of the filament was estimated at about 1 nm in diameter. Hot filament increases the temperature of the surrounding high resistivity oxide, causing it to conduct and carry a significant fraction of the total current. The current spreading results in slowing down the filament temperature increase at higher power. The results of thermometry have been corroborated by HRTEM analysis of the as-fabricated and switched RRAM devices. The functional HfAlOx layer in as-fabricated devices is amorphous. In devices that were switched, we detected a small crystalline region of 10-15 nm in size. The crystallization temperature of the HfAlOx was determined to be 850 K in an independent annealing experiment. The size of the crystalline region agrees with thermal modeling based on the thermometry data. Scanning transmission electron microscopy (TEM) coordinated with electron energy loss spectroscopy could not detect changes in the chemical makeup of the filament. PMID:27351065

  19. Application of high-resolution transmission electron microscopy to the study of aragonite crystallography and diagenesis

    SciTech Connect

    Haywick, D.W. . Geology Dept.); Ness, S.E. . Instrumentation Centre)

    1993-03-01

    High-resolution transmission electron microscopy (HRTEM) is a valuable technique by which to study the ultrastructure of various organic and inorganic compounds. Some biogeological minerals, including skeletal aragonite, have proven to be relatively unstable under an electron beam. Nevertheless, these compounds can be examined by HRTEM provided that minimal exposure techniques are employed. The authors have successfully applied HRTEM to examine diagenetically altered Plio-Pleistocene aragonitic faunas from New Zealand. To date, they have obtained high-resolution images of lattice-fringes with a spacing of 3.7 [angstrom] using a defocused, low-intensity electron beam. At least two of the samples imaged revealed clusters of lattice planes which together, form an interlocking mosaic of variably oriented micro-domains between 5 and 100 nm across. These micro-domains suggest that at least some of the aragonite is heterogeneous at a nm-scale; however, the individual micro-domains, when averaged together, generate single crystal electron diffraction patterns typical of well-ordered aragonite. The origin of the micro-domains is presently unclear. They may be an artifact of diagenetic alteration of an ultrastructurally homogeneous crystal. It is more likely, however, that the micro-domains were produced during aragonite precipitation. If this scenario is correct, it could have major implications for carbonate diagenesis, particularly if micro-domains prove to be ubiquitous within biogenic carbonate minerals. Inter-domains boundaries would be zones of comparative weakness and may provide nucleation points for diagenetic alteration. The intent now is to apply HRTEM in conjunction with other analytical techniques (e.g. x-ray diffraction, electron microprobe, stable isotope geochemistry) to characterize crystallographic changes during progressive diagenesis of aragonite, especially the aragonite-calcite transformation.

  20. Nano features of Al/Au ultrasonic bond interface observed by high resolution transmission electron microscopy

    SciTech Connect

    Ji Hongjun; Li Mingyu Kim, Jong-Myung; Kim, Dae-Won; Wang Chunqing

    2008-10-15

    Nano-scale interfacial details of ultrasonic AlSi1 wire wedge bonding to a Au/Ni/Cu pad were investigated using high resolution transmission electron microscopy (HRTEM). The intermetallic phase Au{sub 8}Al{sub 3} formed locally due to diffusion and reaction activated by ultrasound at the Al/Au bond interface. Multilayer sub-interfaces roughly parallel to the wire/pad interface were observed among this phase, and interdiffusional features near the Au pad resembled interference patterns, alternately dark and bright bars. Solid-state diffusion theory cannot be used to explain why such a thick compound formed within milliseconds at room temperature. The major formation of metallurgical bonds was attributed to ultrasonic cyclic vibration.

  1. High resolution transmission electron microscopic in-situ observations of plastic deformation of compressed nanocrystalline gold

    SciTech Connect

    Wang, Guoyong; Lian, Jianshe; Jiang, Qing; Sun, Sheng; Zhang, Tong-Yi

    2014-09-14

    Nanocrystalline (nc) metals possess extremely high strength, while their capability to deform plastically has been debated for decades. Low ductility has hitherto been considered an intrinsic behavior for most nc metals, due to the lack of five independent slip systems actively operating during deformation in each nanograin. Here we report in situ high resolution transmission electron microscopic (HRTEM) observations of deformation process of nc gold under compression, showing the excellent ductility of individual and aggregate nanograins. Compression causes permanent change in the profile of individual nanograins, which is mediated by dislocation slip and grain rotation. The high rate of grain boundary sliding and large extent of widely exited grain rotation may meet the boundary compatibility requirements during plastic deformation. The in situ HRTEM observations suggest that nc gold is not intrinsically brittle under compressive loading.

  2. High resolution transmission electron microscopy of two stony meteorites - Murchison and Kenna

    NASA Technical Reports Server (NTRS)

    Mackinnon, I. D. R.; Buseck, P. R.

    1979-01-01

    Matrix material from the Murchison C2(M) carbonaceous chondrite and less than micrometer-size pyroxene inclusions in an olivine from the Kenna ureilite have been characterized using high resolution transmission electron microscopy. A diversity of textures and mineral associations, including serpentine-type and brucite-type mixed-layering, occur in the Murchison matrix. Such mixed layer structures are new types of layer silicate. Their presence in the matrix may prove to be genetically significant. The Kenna inclusions, formed at the olivine grain margins, are of two types: (1) a disordered orthopyroxene-clinopyroxene which may have inverted from protopyroxene and (2) a pigeonite with narrow anti-phase domains (80 A to 250 A) and boundaries parallel to (100).

  3. The first observation of titanate nanotubes by spherical aberration corrected high-resolution transmission electron microscopy

    NASA Astrophysics Data System (ADS)

    Miao, L.; Tanemura, S.; Jiang, T.; Tanemura, M.; Yoshida, K.; Tanaka, N.; Xu, G.

    2009-07-01

    Multi-wall titanate nanotubes (MW-TNNTs) with high aspect ratio, large surface area and good uniformity were produced by alkaline hydrothermal treatment of grounded TiO 2 aerogels and further by applying freeze-drying. Not only the crystal phase and diameter, but also morphology of the starting materials impact on the aspect ratio and transformation efficiency of the obtained nanotubes. Other parameters, such as pH value during neutralization process and drying method for the final products, are important to control length and dispersion of MW-TNNTs. By spherical aberration corrected high-resolution transmission-electron-microscopy (Cs-corrected HRTEM) with lateral space resolution of 0.14 nm at 200 kV accelerating voltage and electron energy loss spectrum (EELS), the detailed structural analysis of MW-TNNTs reveals that (1) diameters of inner and outer tubes are about 4-7 nm and 10 nm, respectively, (2) numbers of layers are different from part to part along the longitudinal tube axis, (3) the walls of the tubes have interlayer spacing of 0.70-0.80 nm and the lateral fringes which are vertical to the walls have spacing of 0.32 nm, (4) each layer of MW-TNNT is the nanosheet composed by the arrayed TiO 6 octahedrons, and respective octahedron being slightly strained, and (5) no chirality of MW-TNNT tubular structure is observed.

  4. Development of a sub-eV resolution soft-X-ray spectrometer for a transmission electron microscope.

    PubMed

    Terauchi, M; Yamamoto, H; Tanaka, M

    2001-01-01

    We constructed a grazing-incidence soft-X-ray spectrometer for a transmission electron microscope. The spectrometer, which was composed of a grating and a CCD detector, was attached to a JEM2000FX transmission electron microscope. B K-emission spectra of hexagonal boron-nitride, which give the density of states of the valence band of the material, were obtained with an energy resolution of about 0.6 eV. PMID:11347710

  5. High resolution transmission electron microscopy of melamine-formaldehyde aerogels and silica aerogels

    SciTech Connect

    Ruben, G.C. . Dept. of Biological Sciences)

    1991-09-01

    The goal of the high resolution transmission electron microscopy (HRTEM) was to image the structure of two tetramethyl orthosilicate (TMOS) and two melamine-formaldehyde (MF) aerogels at the single polymer chain level{sup 1,2}. With this level of structural resolution we hoped to interrelate each aerogel's structure with its physical properties and its method of synthesis. Conventional single-step base catalysed TMOS aerogels show strings of spheroidal particles linked together with minimal necking. The spheroidal particles range from 86--132 {Angstrom} and average 113{plus minus}10 {Angstrom} in diameter{sup 2}. In contrast the TMOS aerogels reported on here were made by a two step method. After extended silica chains are grown in solution under acidic conditions with a substoichiometric amount of water, the reaction is stopped and the methanol hydrolysed from TMOS is removed. Then base catalysis and additional water are added to cause gel formation is a nonalcoholic solvent. The MF aerogels were prepared for HRTEM by fracturing them on a stereo microscope stage with razor knife so that fractured pieces with smooth flat surfaces could be selected for platinum-carbon replication. The two silica (TMOS) aerogels were both transparent and difficult to see. These aerogels were fractured on a stereo microscope stage with tweezers. 6 refs., 4 figs.

  6. High resolution transmission electron microscopy study of diamond films grown from fullerene precursors

    SciTech Connect

    Luo, J.S.; Gruen, D.M.; Krauss, A.R.

    1995-07-01

    High-resolution transmission electron microscopy (HRTEM) has been used to investigate the microstructure of diamond films grown by plasma-assisted chemical vapor deposition using fullerene precursors. HRTEM observations of as-grown films revealed an array of larger crystals (>200 nm) within a polycrystalline matrix of much smaller crystallites (<20 nm). The randomly oriented small crystallites were nearly free of structural imperfections such as stacking faults or twins, while the larger ones had preferred <110> orientations with respect to the Si (100) substrate and showed evidence of structural defects on the periphery of the crystals. The most common defects were V-shaped {Sigma}9 twin boundaries, which are generally believed to serve as re-entrant sites for diamond nucleation and growth. The observation of growth steps on both (111) and (110) surfaces seems to support a reaction model in which fragments of C{sub 60}, including C{sub 2}, are considered the growth species. In particular, the nanocrystallinity of the films is most likely due to a high carbon cluster density from C{sub 60} fragmentation at or near the diamond surface, which can serve as nucleation sites for the growth of new crystallites.

  7. In-Situ High-Resolution Transmission Electron Microscopy Investigation of Overheating of Cu Nanoparticles

    PubMed Central

    Chen, Chunlin; Hu, Ziyu; Li, Yanfen; Liu, Limin; Mori, Hirotaro; Wang, Zhangchang

    2016-01-01

    Synthesizing and functionalizing metal nanoparticles supported on substrates is currently the subject of intensive study owing to their outstanding catalytic performances for heterogeneous catalysis. Revealing the fundamental effect of the substrates on metal nanoparticles represents a key step in clarifying mechanisms of stability and catalytic properties of these heterogeneous systems. However, direct identification of these effects still poses a significant challenge due to the complicacy of interactions between substrates and nanoparticles and also for the technical difficulty, restraining our understanding of these heterogeneous systems. Here, we combine in situ high-resolution transmission electron microscopy with molecular dynamics simulations to investigate Cu nanoparticles supported on graphite and Cu2O substrates, and demonstrate that melting behavior and thermal stability of Cu nanoparticles can be markedly influenced by substrates. The graphite-supported Cu nanoparticles do not melt during annealing at 1073 K until they vanish completely, i.e. only the sublimation occurs, while the Cu2O-supported Cu nanoparticles suffer melting during annealing at 973 K. Such selective superheating of the Cu nanoparticles can be attributed to the adsorption of a thin carbon layer on the surface of the Cu nanoparticles, which helps guide further stability enhancement of functional nanoparticles for realistic applications. PMID:26785839

  8. Extended depth of field for high-resolution scanning transmission electron microscopy.

    PubMed

    Hovden, Robert; Xin, Huolin L; Muller, David A

    2011-02-01

    Aberration-corrected scanning transmission electron microscopes (STEMs) provide sub-Angstrom lateral resolution; however, the large convergence angle greatly reduces the depth of field. For microscopes with a small depth of field, information outside of the focal plane quickly becomes blurred and less defined. It may not be possible to image some samples entirely in focus. Extended depth-of-field techniques, however, allow a single image, with all areas in focus, to be extracted from a series of images focused at a range of depths. In recent years, a variety of algorithmic approaches have been employed for bright-field optical microscopy. Here, we demonstrate that some established optical microscopy methods can also be applied to extend the ∼ 6 nm depth of focus of a 100 kV 5th-order aberration-corrected STEM (α max = 33 mrad) to image Pt-Co nanoparticles on a thick vulcanized carbon support. These techniques allow us to automatically obtain a single image with all the particles in focus as well as a complimentary topography map. PMID:21122192

  9. Extended Depth of Field for High-Resolution Scanning Transmission Electron Microscopy

    SciTech Connect

    Hovden, Robert; Xin, Huolin L.; Muller, David A.

    2010-12-02

    Aberration-corrected scanning transmission electron microscopes (STEMs) provide sub-Angstrom lateral resolution; however, the large convergence angle greatly reduces the depth of field. For microscopes with a small depth of field, information outside of the focal plane quickly becomes blurred and less defined. It may not be possible to image some samples entirely in focus. Extended depth-of-field techniques, however, allow a single image, with all areas in focus, to be extracted from a series of images focused at a range of depths. In recent years, a variety of algorithmic approaches have been employed for bright-field optical microscopy. Here, we demonstrate that some established optical microscopy methods can also be applied to extend the ~6 nm depth of focus of a 100 kV 5th-order aberration-corrected STEM (α{sub max} = 33 mrad) to image Pt-Co nanoparticles on a thick vulcanized carbon support. These techniques allow us to automatically obtain a single image with all the particles in focus as well as a complimentary topography map.

  10. In-Situ High-Resolution Transmission Electron Microscopy Investigation of Overheating of Cu Nanoparticles

    NASA Astrophysics Data System (ADS)

    Chen, Chunlin; Hu, Ziyu; Li, Yanfen; Liu, Limin; Mori, Hirotaro; Wang, Zhangchang

    2016-01-01

    Synthesizing and functionalizing metal nanoparticles supported on substrates is currently the subject of intensive study owing to their outstanding catalytic performances for heterogeneous catalysis. Revealing the fundamental effect of the substrates on metal nanoparticles represents a key step in clarifying mechanisms of stability and catalytic properties of these heterogeneous systems. However, direct identification of these effects still poses a significant challenge due to the complicacy of interactions between substrates and nanoparticles and also for the technical difficulty, restraining our understanding of these heterogeneous systems. Here, we combine in situ high-resolution transmission electron microscopy with molecular dynamics simulations to investigate Cu nanoparticles supported on graphite and Cu2O substrates, and demonstrate that melting behavior and thermal stability of Cu nanoparticles can be markedly influenced by substrates. The graphite-supported Cu nanoparticles do not melt during annealing at 1073 K until they vanish completely, i.e. only the sublimation occurs, while the Cu2O-supported Cu nanoparticles suffer melting during annealing at 973 K. Such selective superheating of the Cu nanoparticles can be attributed to the adsorption of a thin carbon layer on the surface of the Cu nanoparticles, which helps guide further stability enhancement of functional nanoparticles for realistic applications.

  11. High-Resolution Transmission Electron Microscopy Observation of Colloidal Nanocrystal Growth Mechanisms using Graphene Liquid Cells

    SciTech Connect

    Yuk, Jong Min; Park, Jungwon; Ercius, Peter; Kim, Kwanpyo; Hellebusch, Danny J.; Crommie, Michael F.; Lee, Jeong Yong; Zettl, A.; Alivisatos, A. Paul

    2011-12-12

    We introduce a new type of liquid cell for in-situ electron microscopy based upon entrapment of a liquid film between layers of graphene. We employ this cell to achieve high-resolution imaging of colloidal platinum nanocrystal growth. The ability to directly image and resolve critical steps at atomic resolution provides new insights into nanocrystal coalescence and reshaping during growth.

  12. High-Resolution Transmission Electron Microscopy Calibration of Critical Dimension (CD) Reference Materials

    SciTech Connect

    ALLEN, RICHARD A.; CRESSWELL, MICHAEL W.; EVERIST, SARAH C.; GHOSHTAGORE, RATHINDRA N.; HEADLEY, THOMAS J.; LINHOLM, LOREN W.

    1999-09-21

    NIST and Sandia have developed a procedure for producing and calibrating critical dimension (CD), or linewidth, reference materials. These reference materials will be used to calibrate metrology instruments used in semiconductor manufacturing. The artifacts, with widths down to 100 nm, are produced in monocrystalline silicon with all feature edges aligned to specific crystal planes. A two-part calibration of these linewidths is used: the primary calibration, with accuracy to within a few lattice plane thicknesses, is accomplished by counting the lattice planes across the sample as-imaged through use of high-resolution transmission electron microscopy (HRTEM). The secondary calibration is the high-precision electrical CD technique. NIST and Sandia are developing critical dimension (CD), or linewidth, reference materials for use by the semiconductor industry. To meet the current requirements of this rapidly changing industry, the widths of the reference features must be at or below the widths of the finest features in production and/or development. Further, these features must produce consistent results no matter which metrology tool (e.g., scanning electron microscope, scanned probe microscope, electrical metrology) is used to make the measurement. This leads to a requirement for the samples to have planar surfaces, known sidewall angles, and uniform material composition. None of the production techniques in use in semiconductor manufacturing can produce features with all these characteristics. In addition, requirements specified in the National Technology Roadmap for Semiconductors indicate that the width of the feature must be accurately calibrated to approximately 1-2 nm, a value well beyond the current capabilities of the instruments used for semiconductor metrology.

  13. Atomic resolution transmission electron microscopy of the intergranular structure of a Y{sub 2}O{sub 3}-silicon nitride ceramic

    SciTech Connect

    Ziegler, A.; Kisielowski, C.; Hoffmann, M.J.; Ritchie, R.O.

    2002-05-01

    High-resolution transmission electron microscopy (HRTEM) employing focus-variation phase-reconstruction methods is used to image the atomic structure of grain boundaries in a silicon nitride ceramic at a resolution of 0.8 Angstrom

  14. Method and apparatus for a high-resolution three dimensional confocal scanning transmission electron microscope

    DOEpatents

    de Jonge, Niels [Oak Ridge, TN

    2010-08-17

    A confocal scanning transmission electron microscope which includes an electron illumination device providing an incident electron beam propagating in a direction defining a propagation axis, and a precision specimen scanning stage positioned along the propagation axis and movable in at least one direction transverse to the propagation axis. The precision specimen scanning stage is configured for positioning a specimen relative to the incident electron beam. A projector lens receives a transmitted electron beam transmitted through at least part of the specimen and focuses this transmitted beam onto an image plane, where the transmitted beam results from the specimen being illuminated by the incident electron beam. A detection system is placed approximately in the image plane.

  15. Strain mapping of semiconductor specimens with nm-scale resolution in a transmission electron microscope.

    PubMed

    Cooper, David; Denneulin, Thibaud; Bernier, Nicolas; Béché, Armand; Rouvière, Jean-Luc

    2016-01-01

    The last few years have seen a great deal of progress in the development of transmission electron microscopy based techniques for strain mapping. New techniques have appeared such as dark field electron holography and nanobeam diffraction and better known ones such as geometrical phase analysis have been improved by using aberration corrected ultra-stable modern electron microscopes. In this paper we apply dark field electron holography, the geometrical phase analysis of high angle annular dark field scanning transmission electron microscopy images, nanobeam diffraction and precession diffraction, all performed at the state-of-the-art to five different types of semiconductor samples. These include a simple calibration structure comprising 10-nm-thick SiGe layers to benchmark the techniques. A SiGe recessed source and drain device has been examined in order to test their capabilities on 2D structures. Devices that have been strained using a nitride stressor have been examined to test the sensitivity of the different techniques when applied to systems containing low values of deformation. To test the techniques on modern semiconductors, an electrically tested device grown on a SOI wafer has been examined. Finally a GaN/AlN superlattice was tested in order to assess the different methods of measuring deformation on specimens that do not have a perfect crystalline structure. The different deformation mapping techniques have been compared to one another and the strengths and weaknesses of each are discussed. PMID:26606463

  16. New and unconventional approaches for advancing resolution in biological transmission electron microscopy by improving macromolecular specimen preparation and preservation.

    SciTech Connect

    Massover, W.; Materials Science Division

    2011-02-01

    Resolution in transmission electron microscopy (TEM) now is limited by the properties of specimens, rather than by those of instrumentation. The long-standing difficulties in obtaining truly high-resolution structure from biological macromolecules with TEM demand the development, testing, and application of new ideas and unconventional approaches. This review concisely describes some new concepts and innovative methodologies for TEM that deal with unsolved problems in the preparation and preservation of macromolecular specimens. The selected topics include use of better support films, a more protective multi-component matrix surrounding specimens for cryo-TEM and negative staining, and, several quite different changes in microscopy and micrography that should decrease the effects of electron radiation damage; all these practical approaches are non-traditional, but have promise to advance resolution for specimens of biological macromolecules beyond its present level of 3-10 {angstrom} (0.3-1.0 nm). The result of achieving truly high resolution will be a fulfillment of the still unrealized potential of transmission electron microscopy for directly revealing the structure of biological macromolecules down to the atomic level.

  17. Carbon Nanostructure Examined by Lattice Fringe Analysis of High Resolution Transmission Electron Microscopy Images

    NASA Technical Reports Server (NTRS)

    VanderWal, Randy L.; Tomasek, Aaron J.; Street, Kenneth; Thompson, William K.; Hull, David R.

    2003-01-01

    The dimensions of graphitic layer planes directly affect the reactivity of soot towards oxidation and growth. Quantification of graphitic structure could be used to develop and test correlations between the soot nanostructure and its reactivity. Based upon transmission electron microscopy images, this paper provides a demonstration of the robustness of a fringe image analysis code for determining the level of graphitic structure within nanoscale carbon, i.e., soot. Results, in the form of histograms of graphitic layer plane lengths, are compared to their determination through Raman analysis.

  18. Carbon Nanostructure Examined by Lattice Fringe Analysis of High Resolution Transmission Electron Microscopy Images

    NASA Technical Reports Server (NTRS)

    VanderWal, Randy L.; Tomasek, Aaron J.; Street, Kenneth; Thompson, William K.

    2002-01-01

    The dimensions of graphitic layer planes directly affect the reactivity of soot towards oxidation and growth. Quantification of graphitic structure could be used to develop and test correlations between the soot nanostructure and its reactivity. Based upon transmission electron microscopy images, this paper provides a demonstration of the robustness of a fringe image analysis code for determining the level of graphitic structure within nanoscale carbon, i.e. soot. Results, in the form of histograms of graphitic layer plane lengths, are compared to their determination through Raman analysis.

  19. Robust atomic resolution imaging of light elements using scanning transmission electron microscopy

    SciTech Connect

    Findlay, S. D.; Shibata, N.; Sawada, H.; Okunishi, E.; Kondo, Y.; Yamamoto, T.; Ikuhara, Y.

    2009-11-09

    We show that an annular detector placed within the bright field cone in scanning transmission electron microscopy allows direct imaging of light elements in crystals. In contrast to common high angle annular dark field imaging, both light and heavy atom columns are visible simultaneously. In contrast to common bright field imaging, the images are directly and robustly interpretable over a large range of thicknesses. We demonstrate this through systematic simulations and present a simple physical model to obtain some insight into the scattering dynamics.

  20. Dynamic Transmission Electron Microscopy

    SciTech Connect

    Evans, James E.; Jungjohann, K. L.; Browning, Nigel D.

    2012-10-12

    Dynamic transmission electron microscopy (DTEM) combines the benefits of high spatial resolution electron microscopy with the high temporal resolution of ultrafast lasers. The incorporation of these two components into a single instrument provides a perfect platform for in situ observations of material processes. However, previous DTEM applications have focused on observing structural changes occurring in samples exposed to high vacuum. Therefore, in order to expand the pump-probe experimental regime to more natural environmental conditions, in situ gas and liquid chambers must be coupled with Dynamic TEM. This chapter describes the current and future applications of in situ liquid DTEM to permit time-resolved atomic scale observations in an aqueous environment, Although this chapter focuses mostly on in situ liquid imaging, the same research potential exists for in situ gas experiments and the successful integration of these techniques promises new insights for understanding nanoparticle, catalyst and biological protein dynamics with unprecedented spatiotemporal resolution.

  1. Understanding the structure of nanocatalysts with high resolution scanning/transmission electron microscopy

    NASA Astrophysics Data System (ADS)

    Francis, L. D.; Rivas, J.; José-Yacamán, M.

    2014-03-01

    Nanomaterials including nanoparticles, nanowires and nanotubes play an important role in heterogeneous catalysis. Thanks to the rapid improvement of the electron microscopic techniques and with the advent of aberration corrected electron microscopy as well as theoretical methodologies, the potential effects induced by nanocatalysts are better understood than before by unravelling their atomic structure. A brief introduction to advanced electron microscopic techniques namely aberration corrected scanning transmission electron microscopy (Cs-STEM) is presented and subsequently two examples of nanocatalysts are considered in the present review. The first example will focus on the study of bimetallic/core-shell nanoalloys. In heterogeneous catalysis, catalysts containing two or more metals might show significantly different catalytic properties compared to the parent metals and thus are widely utilized in several catalytic reactions. Atom-by-atom insights of the nanoalloy based catalysts ex: Au-Pd will be described in the present review using a combination of advanced electron microscopic and spectroscopic techniques. A related example on the understanding of bimetallic clusters by HAADF-STEM will also be presented in addition to nanoparticles. In the second case understanding the structure of transition metal chalcogenide based nanocatalysts by HRTEM and aberration corrected STEM, for the case of MoS2 will be discussed. MoS2-based catalysts serve as model catalysts and are employed in the hydrodesulphurisations (HDS) reactions in the removal of sulphur from gasoline and related petrochemical products. They have been studied in various forms including nanowires, nanotubes and nanoplates. Their structure, atomic insights and as a consequence elucidation of their corresponding catalytic activity are thus important.

  2. Aberration corrected 1.2-MV cold field-emission transmission electron microscope with a sub-50-pm resolution

    SciTech Connect

    Akashi, Tetsuya; Takahashi, Yoshio; Tanigaki, Toshiaki Shimakura, Tomokazu; Kawasaki, Takeshi; Furutsu, Tadao; Shinada, Hiroyuki; Osakabe, Nobuyuki; Müller, Heiko; Haider, Maximilian; Tonomura, Akira

    2015-02-16

    Atomic-resolution electromagnetic field observation is critical to the development of advanced materials and to the unveiling of their fundamental physics. For this purpose, a spherical-aberration corrected 1.2-MV cold field-emission transmission electron microscope has been developed. The microscope has the following superior properties: stabilized accelerating voltage, minimized electrical and mechanical fluctuation, and coherent electron emission. These properties have enabled to obtain 43-pm information transfer. On the bases of these performances, a 43-pm resolution has been obtained by correcting lens aberrations up to the third order. Observations of GaN [411] thin crystal showed a projected atomic locations with a separation of 44 pm.

  3. Preparation of the planarian Schmidtea mediterranea for high-resolution histology and transmission electron microscopy

    PubMed Central

    Brubacher, John L.; Vieira, Ana P.; Newmark, Phillip A.

    2014-01-01

    The flatworm Schmidtea mediterranea is an emerging model species in such fields as stem-cell biology, regeneration, and evolutionary biology. Excellent molecular tools have been developed for S. mediterranea, but ultrastructural techniques have received far less attention. Processing specimens for histology and transmission electron microscopy is notoriously idiosyncratic for particular species or specimen types. Unfortunately however, most methods for S. mediterranea described in the literature lack numerous essential details, and those few that do provide them rely on specialized equipment that may not be readily available. Here we present an optimized protocol for ultrastructural preparation of S. mediterranea. The protocol can be completed in six days, much of which is “hands-off” time. To aid with troubleshooting, we also illustrate the significant effects of seemingly minor variations in fixative, buffer concentration, and dehydration steps. This procedure will be useful for all planarian researchers, particularly those with relatively little experience in tissue processing. PMID:24556788

  4. Automated transmission-mode scanning electron microscopy (tSEM) for large volume analysis at nanoscale resolution.

    PubMed

    Kuwajima, Masaaki; Mendenhall, John M; Lindsey, Laurence F; Harris, Kristen M

    2013-01-01

    Transmission-mode scanning electron microscopy (tSEM) on a field emission SEM platform was developed for efficient and cost-effective imaging of circuit-scale volumes from brain at nanoscale resolution. Image area was maximized while optimizing the resolution and dynamic range necessary for discriminating key subcellular structures, such as small axonal, dendritic and glial processes, synapses, smooth endoplasmic reticulum, vesicles, microtubules, polyribosomes, and endosomes which are critical for neuronal function. Individual image fields from the tSEM system were up to 4,295 µm(2) (65.54 µm per side) at 2 nm pixel size, contrasting with image fields from a modern transmission electron microscope (TEM) system, which were only 66.59 µm(2) (8.160 µm per side) at the same pixel size. The tSEM produced outstanding images and had reduced distortion and drift relative to TEM. Automated stage and scan control in tSEM easily provided unattended serial section imaging and montaging. Lens and scan properties on both TEM and SEM platforms revealed no significant nonlinear distortions within a central field of ∼100 µm(2) and produced near-perfect image registration across serial sections using the computational elastic alignment tool in Fiji/TrakEM2 software, and reliable geometric measurements from RECONSTRUCT™ or Fiji/TrakEM2 software. Axial resolution limits the analysis of small structures contained within a section (∼45 nm). Since this new tSEM is non-destructive, objects within a section can be explored at finer axial resolution in TEM tomography with current methods. Future development of tSEM tomography promises thinner axial resolution producing nearly isotropic voxels and should provide within-section analyses of structures without changing platforms. Brain was the test system given our interest in synaptic connectivity and plasticity; however, the new tSEM system is readily applicable to other biological systems. PMID:23555711

  5. High-resolution transmission electron microscopy study of carbon deposited on the NiO/MgO solid solution catalysts

    SciTech Connect

    Hu, Y.H.; Ruckenstein, E.

    1999-05-15

    The carbon deposition due to the CH{sub 4} decomposition at 790 C over NiO/MgO catalysts was investigated by high-resolution transmission electron microscopy. While no deposits could be detected over the catalysts with a NiO content smaller than 9.1 wt%, they were detected over the catalysts with NiO contents of 23 and 50 wt%. The carbon deposits are composed of platelets located at distances of about 0.34 nm, corresponding to the graphitic carbon. Various structures of the deposited carbon were observed: (a) carbon consisting of platelets parallel to the surface of the particle, which covers a catalyst particle, (b) nanotubes composed of platelets parallel to their axis, and (c) carbon vortexes consisting of platelets parallel to their axis.

  6. Observation of antisite domain boundaries in Cu2ZnSnS4 by atomic-resolution transmission electron microscopy.

    PubMed

    Kattan, N A; Griffiths, I J; Cherns, D; Fermín, D J

    2016-08-14

    Atomic resolution transmission electron microscopy has been used to examine antisite defects in Cu2ZnSnS4 (CZTS) kesterite crystals grown by a hot injection method. High angle annular dark field (HAADF) imaging at sub-0.1 nm resolution, and lower magnification dark field imaging using reflections sensitive to cation ordering, are used to reveal antisite domain boundaries (ADBs). These boundaries, typically 5-20 nm apart, and extending distances of 100 nm or more into the crystals, lie on a variety of planes and have displacements of the type ½[110] or ¼[201], which translate Sn, Cu and Zn cations into antisite positions. It is shown that some ADBs describe a change in the local stoichiometry by removing planes of S and either Cu or Zn atoms, implying that these boundaries can be electrically charged. The observations also showed a marked increase in cation disorder in regions within 1-2 nm of the grain surfaces suggesting that growth of the ordered crystal takes place at the interface with a disordered shell. It is estimated that the ADBs contribute on average ∼0.1 antisite defect pairs per unit cell. Although this is up to an order of magnitude less than the highest antisite defect densities reported, the presence of high densities of ADBs that may be charged suggests these defects may have a significant influence on the efficiency of CZTS solar cells. PMID:27405278

  7. Soot Structure and Reactivity Analysis by Raman Microspectroscopy, Temperature-Programmed Oxidation, and High-Resolution Transmission Electron Microscopy

    NASA Astrophysics Data System (ADS)

    Knauer, Markus; Schuster, Manfred E.; Su, Dangsheng; Schlögl, Robert; Niessner, Reinhard; Ivleva, Natalia P.

    2009-11-01

    Raman microspectroscopy (RM), temperature-programmed oxidation (TPO), high-resolution transmission electron microscopy (HRTEM), and electron energy loss spectroscopy (EELS) were combined to get comprehensive information on the relationship between structure and reactivity of soot in samples of spark discharge (GfG), heavy duty engine diesel (EURO VI and IV) soot, and graphite powder upon oxidation by oxygen at increasing temperatures. GfG soot and graphite powder represent the higher and lower reactivity limits. Raman microspectroscopic analysis was conducted by determination of spectral parameters using a five band fitting procedure (G, D1-D4) as well as by evaluation of the dispersive character of the D mode. The analysis of spectral parameters shows a higher degree of disorder and a higher amount of molecular carbon for untreated GfG soot samples than for samples of untreated EURO VI and EURO IV soot. The structural analysis based on the dispersive character of the D mode revealed substantial differences in ordering descending from graphite powder, EURO IV, VI to GfG soot. HRTEM images and EELS analysis of EURO IV and VI samples indicated a different morphology and a higher structural order as compared to GfG soot in full agreement with the Raman analysis. These findings are also confirmed by the reactivity of soot during oxidation (TPO), where GfG soot was found to be the most reactive and EURO IV and VI soot samples exhibited a moderate reactivity.

  8. Structural Characterization and Gas Reactions of Small Metal Particles by High Resolution In-situ TEM and TED. [Transmission Electron Microscopy and Transmission Electron Diffraction

    NASA Technical Reports Server (NTRS)

    Heinemann, K.

    1985-01-01

    A commercial electron microscope with flat-plate upper pole piece configuration of the objective lens and top entry specimen introduction was modified to obtain 5 x 10 to the minus 10th power mbar pressure at the site of the specimen while maintaining the convenience of a specimen airlock system that allows operation in the 10 to the 10th power mbar range within 15 minutes after specimen change. The specimen chamber contains three wire evaporation sources, a specimen heater, and facilities for oxygen or hydrogen plasma treatment to clean as-introduced specimens. Evacuation is achieved by dural differential pumping, with fine entrance and exit apertures for the electron beam. With the microscope operating at .000001 mbar, the first differential pumping stage features a high-speed cryopump operating in a stainless steel chamber that can be mildly baked and reaches 1 x 10 to the minus 8th power mbar. The second stage, containing the evaporation sources and a custom ionization gauge within 10 cm from the specimen, is a rigorously uncompromised all-metal uhv-system that is bakable to above 200 C throughout and is pumped with an 80-liter ion pump. Design operating pressures and image quality (resolution of metal particles smaller than 1 nm in size) was achieved.

  9. Observation of antisite domain boundaries in Cu2ZnSnS4 by atomic-resolution transmission electron microscopy

    NASA Astrophysics Data System (ADS)

    Kattan, N. A.; Griffiths, I. J.; Cherns, D.; Fermín, D. J.

    2016-07-01

    Atomic resolution transmission electron microscopy has been used to examine antisite defects in Cu2ZnSnS4 (CZTS) kesterite crystals grown by a hot injection method. High angle annular dark field (HAADF) imaging at sub-0.1 nm resolution, and lower magnification dark field imaging using reflections sensitive to cation ordering, are used to reveal antisite domain boundaries (ADBs). These boundaries, typically 5-20 nm apart, and extending distances of 100 nm or more into the crystals, lie on a variety of planes and have displacements of the type ½[110] or ¼[201], which translate Sn, Cu and Zn cations into antisite positions. It is shown that some ADBs describe a change in the local stoichiometry by removing planes of S and either Cu or Zn atoms, implying that these boundaries can be electrically charged. The observations also showed a marked increase in cation disorder in regions within 1-2 nm of the grain surfaces suggesting that growth of the ordered crystal takes place at the interface with a disordered shell. It is estimated that the ADBs contribute on average ~0.1 antisite defect pairs per unit cell. Although this is up to an order of magnitude less than the highest antisite defect densities reported, the presence of high densities of ADBs that may be charged suggests these defects may have a significant influence on the efficiency of CZTS solar cells.Atomic resolution transmission electron microscopy has been used to examine antisite defects in Cu2ZnSnS4 (CZTS) kesterite crystals grown by a hot injection method. High angle annular dark field (HAADF) imaging at sub-0.1 nm resolution, and lower magnification dark field imaging using reflections sensitive to cation ordering, are used to reveal antisite domain boundaries (ADBs). These boundaries, typically 5-20 nm apart, and extending distances of 100 nm or more into the crystals, lie on a variety of planes and have displacements of the type ½[110] or ¼[201], which translate Sn, Cu and Zn cations into antisite

  10. Investigations of atomic configurations of 60° basal dislocations in wurtzite GaN film by high-resolution transmission electron microscopy

    NASA Astrophysics Data System (ADS)

    Chang, Yunjie; Wang, Yumei; Deng, Zhen; Chen, Hong; Ge, Binghui

    2016-04-01

    GaN epitaxial films grown on Si (111) substrates were observed using a 200 kV high-resolution (HR) transmission electron microscope. Both perfect and dissociated 60° basal dislocations were found in ? HR images. By utilizing the image deconvolution method, the HR images were transformed into structure maps with an improved resolution, and then the atomic configurations of perfect and partial dislocations were determined. Afterwards, the possible dissociation schemes for the dissociated dislocations were derived.

  11. Genesis of presolar diamonds: Comparative high-resolution transmission electron microscopy study of meteoritic and terrestrial nano-diamonds

    SciTech Connect

    Daulton, T.L. |; Eisenhour, D.D.; Buseck, P.R.

    1996-12-01

    Nano-diamonds isolated from acid dissolution residues of primitive carbonaceous meteorites (Allende and Murchison) were studied using high-resolution transmission electron microscopy. To discriminate among their most likely formation mechanisms, high-pressure shock-induced metamorphism or low-pressure vapor condensation. the microstructures of presolar diamond crystallites were compared to those of (terrestrial) synthesized nano-diamonds. The synthesized diamonds used for comparison in this study were produced by high-pressure shock waves generated in controlled detonations and by direct nucleation and homoepitaxial growth from the vapor phase in low-pressure chemical vapor deposition (CVD)-type processes. Microstructural features were identified that appear unique to shock metamorphism and to nucleation from the vapor phase, respectively. A comparison of these features to the microstructures found in presolar diamonds indicates that the predominant mechanism for presolar diamond formation is a vapor deposition process, suggesting a circumstellar condensation origin. A new presolar grain component has also been identified in the meteoritic residues, the (2H) hexagonal polytype of diamond (lonsdaleite). 93 refs., 17 figs., 1 tab.

  12. Separating strain from composition in unit cell parameter maps obtained from aberration corrected high resolution transmission electron microscopy imaging

    SciTech Connect

    Schulz, T.; Remmele, T.; Korytov, M.; Markurt, T.; Albrecht, M.; Duff, A.; Lymperakis, L.; Neugebauer, J.; Chèze, C.

    2014-01-21

    Based on the evaluation of lattice parameter maps in aberration corrected high resolution transmission electron microscopy images, we propose a simple method that allows quantifying the composition and disorder of a semiconductor alloy at the unit cell scale with high accuracy. This is realized by considering, next to the out-of-plane, also the in-plane lattice parameter component allowing to separate the chemical composition from the strain field. Considering only the out-of-plane lattice parameter component not only yields large deviations from the true local alloy content but also carries the risk of identifying false ordering phenomena like formations of chains or platelets. Our method is demonstrated on image simulations of relaxed supercells, as well as on experimental images of an In{sub 0.20}Ga{sub 0.80}N quantum well. Principally, our approach is applicable to all epitaxially strained compounds in the form of quantum wells, free standing islands, quantum dots, or wires.

  13. High-resolution transmission electron microscopy observations on textured rapidly quenched NdFeB permanent magnets

    NASA Astrophysics Data System (ADS)

    Li, Lin; Luzzi, D. E.; Graham, C. D., Jr.

    1991-11-01

    High-resolution transmission electron microscopy (HRTEM) has been used to examine the microstructures of NdFeB magnets made by rapid solidification. The samples were General Motors MQ-3 magnets, and also MQ-3 magnets that had been recompressed perpendicular to the original compression axis. A major finding is that the Nd-rich grain-boundary phase is not uniformly distributed on all grain boundaries of the Nd2Fe14B phase. Some boundaries are completely clean, and where the Nd-rich phase does appear, its thickness varies widely. The grain-boundary phase (whose structure has been variously identified) is partially ordered at room temperature after slow cooling. Ordered domains and antiphase boundaries have been observed in this phase by HRTEM. Using the Nd2Fe14B fringe spacing as calibration, the lattice parameter of the grain-boundary phase is found to be 5.58 Å. In the completely ordered state, this phase is neither bcc nor fcc; it is simple cubic with a lower-symmetry space group Pm3m.

  14. Characterization of Al2O3 in High-Strength Mo Alloy Sheets by High-Resolution Transmission Electron Microscopy.

    PubMed

    Zhou, Yucheng; Gao, Yimin; Wei, Shizhong; Hu, Yajie

    2016-02-01

    A novel type of alumina (Al2O3)-doped molybdenum (Mo) alloy sheet was prepared by a hydrothermal method and a subsequent powder metallurgy process. Then the characterization of α-Al2O3 was investigated using high-resolution transmission electron microscopy as the research focus. The tensile strength of the Al2O3-doped Mo sheet is 43-85% higher than that of the pure Mo sheet, a very obvious reinforcement effect. The sub-micron and nanometer-scale Al2O3 particles can increase the recrystallization temperature by hindering grain boundary migration and improve the tensile strength by effectively blocking the motion of the dislocations. The Al2O3 particles have a good bond with the Mo matrix and there exists an amorphous transition layer at the interface between Al2O3 particles and the Mo matrix in the as-rolled sheet. The sub-structure of α-Al2O3 is characterized by a number of nanograins in the $\\left[ {2\\bar{2}1} \\right]$ direction. Lastly, a new computer-based method for indexing diffraction patterns of the hexagonal system is introduced, with 16 types of diffraction patterns of α-Al2O3 indexed. PMID:26914997

  15. High resolution transmission electron microscope Imaging and first-principles simulations of atomic-scale features in graphene membrane

    NASA Astrophysics Data System (ADS)

    Wang, Wei; Bhandari, Sagar; Yi, Wei; Bell, David; Westervelt, Robert; Kaxiras, Efthimios

    2012-02-01

    Ultra-thin membranes such as graphene[1] are of great importance for basic science and technology applications. Graphene sets the ultimate limit of thinness, demonstrating that a free-standing single atomic layer not only exists but can be extremely stable and strong [2--4]. However, both theory [5, 6] and experiments [3, 7] suggest that the existence of graphene relies on intrinsic ripples that suppress the long-wavelength thermal fluctuations which otherwise spontaneously destroy long range order in a two dimensional system. Here we show direct imaging of the atomic features in graphene including the ripples resolved using monochromatic aberration-corrected transmission electron microscopy (TEM). We compare the images observed in TEM with simulated images based on an accurate first-principles total potential. We show that these atomic scale features can be mapped through accurate first-principles simulations into high resolution TEM contrast. [1] Geim, A. K. & Novoselov, K. S. Nat. Mater. 6, 183-191, (2007). [2] Novoselov, K. S.et al. Science 306, 666-669, (2004). [3] Meyer, J. C. et al. Nature 446, 60-63, (2007). [4] Lee, C., Wei, X. D., Kysar, J. W. & Hone, J. Science 321, 385-388, (2008). [5] Nelson, D. R. & Peliti, L. J Phys-Paris 48, 1085-1092, (1987). [6] Fasolino, A., Los, J. H. & Katsnelson, M. I. Nat. Mater. 6, 858-861, (2007). [7] Meyer, J. C. et al. Solid State Commun. 143, 101-109, (2007).

  16. Neutron irradiation damage of nuclear graphite studied by high-resolution transmission electron microscopy and Raman spectroscopy

    NASA Astrophysics Data System (ADS)

    Krishna, R.; Jones, A. N.; McDermott, L.; Marsden, B. J.

    2015-12-01

    Nuclear graphite components are produced from polycrystalline artificial graphite manufacture from a binder and filler coke with approximately 20% porosity. During the operational lifetime, nuclear graphite moderator components are subjected to fast neutron irradiation which contributes to the change of material and physical properties such as thermal expansion co-efficient, young's modulus and dimensional change. These changes are directly driven by irradiation-induced changes to the crystal structure as reflected through the bulk microstructure. It is therefore of critical importance that these irradiation changes and there implication on component property changes are fully understood. This work examines a range of irradiated graphite samples removed from the British Experimental Pile Zero (BEPO) reactor; a low temperature, low fluence, air-cooled Materials Test Reactor which operated in the UK. Raman spectroscopy and high-resolution transmission electron microscopy (HRTEM) have been employed to characterise the effect of increased irradiation fluence on graphite microstructure and understand low temperature irradiation damage processes. HRTEM confirms the structural damage of the crystal lattice caused by irradiation attributed to a high number of defects generation with the accumulation of dislocation interactions at nano-scale range. Irradiation-induced crystal defects, lattice parameters and crystallite size compared to virgin nuclear graphite are characterised using selected area diffraction (SAD) patterns in TEM and Raman Spectroscopy. The consolidated 'D'peak in the Raman spectra confirms the formation of in-plane point defects and reflected as disordered regions in the lattice. The reduced intensity and broadened peaks of 'G' and 'D' in the Raman and HRTEM results confirm the appearance of turbulence and disordering of the basal planes whilst maintaining their coherent layered graphite structure.

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

    NASA Technical Reports Server (NTRS)

    Heinemann, K.

    1987-01-01

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

  18. Analytical transmission electron microscopy in materials science

    SciTech Connect

    Fraser, H.L.

    1980-01-01

    Microcharacterization of materials on a scale of less than 10 nm has been afforded by recent advances in analytical transmission electron microscopy. The factors limiting accurate analysis at the limit of spatial resolution for the case of a combination of scanning transmission electron microscopy and energy dispersive x-ray spectroscopy are examined in this paper.

  19. Oxidation-state sensitive imaging of cerium dioxide by atomic-resolution low-angle annular dark field scanning transmission electron microscopy.

    PubMed

    Johnston-Peck, Aaron C; Winterstein, Jonathan P; Roberts, Alan D; DuChene, Joseph S; Qian, Kun; Sweeny, Brendan C; Wei, Wei David; Sharma, Renu; Stach, Eric A; Herzing, Andrew A

    2016-03-01

    Low-angle annular dark field (LAADF) scanning transmission electron microscopy (STEM) imaging is presented as a method that is sensitive to the oxidation state of cerium ions in CeO2 nanoparticles. This relationship was validated through electron energy loss spectroscopy (EELS), in situ measurements, as well as multislice image simulations. Static displacements caused by the increased ionic radius of Ce(3+) influence the electron channeling process and increase electron scattering to low angles while reducing scatter to high angles. This process manifests itself by reducing the high-angle annular dark field (HAADF) signal intensity while increasing the LAADF signal intensity in close proximity to Ce(3+) ions. This technique can supplement STEM-EELS and in so doing, relax the experimental challenges associated with acquiring oxidation state information at high spatial resolutions. PMID:26744830

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

    NASA Astrophysics Data System (ADS)

    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.

  1. Optimal experimental design for the detection of light atoms from high-resolution scanning transmission electron microscopy images

    SciTech Connect

    Gonnissen, J.; De Backer, A.; Martinez, G. T.; Van Aert, S.; Dekker, A. J. den; Rosenauer, A.; Sijbers, J.

    2014-08-11

    We report an innovative method to explore the optimal experimental settings to detect light atoms from scanning transmission electron microscopy (STEM) images. Since light elements play a key role in many technologically important materials, such as lithium-battery devices or hydrogen storage applications, much effort has been made to optimize the STEM technique in order to detect light elements. Therefore, classical performance criteria, such as contrast or signal-to-noise ratio, are often discussed hereby aiming at improvements of the direct visual interpretability. However, when images are interpreted quantitatively, one needs an alternative criterion, which we derive based on statistical detection theory. Using realistic simulations of technologically important materials, we demonstrate the benefits of the proposed method and compare the results with existing approaches.

  2. Electronically controlled automatic transmission

    SciTech Connect

    Ohkubo, M.; Shiba, H.; Nakamura, K.

    1989-03-28

    This patent describes an electronically controlled automatic transmission having a manual valve working in connection with a manual shift lever, shift valves operated by solenoid valves which are driven by an electronic control circuit previously memorizing shift patterns, and a hydraulic circuit controlled by these manual valve and shift valves for driving brakes and a clutch in order to change speed. Shift patterns of 2-range and L-range, in addition to a shift pattern of D-range, are memorized previously in the electronic control circuit, an operation switch is provided which changes the shift pattern of the electronic control circuit to any shift pattern among those of D-range, 2-range and L-range at time of the manual shift lever being in a D-range position, a releasable lock mechanism is provided which prevents the manual shift lever from entering 2-range and L-range positions, and the hydraulic circuit is set to a third speed mode when the manual shift lever is in the D-range position. The circuit is set to a second speed mode when it is in the 2-range position, and the circuit is set to a first speed mode when it is in the L-range position, respectively, in case where the shift valves are not working.

  3. High-resolution transmission electron microscopy study of electrically-driven reversible phase change in ge2sb2te5 nanowires.

    PubMed

    Jung, Yeonwoong; Nam, Sung-Wook; Agarwal, Ritesh

    2011-03-01

    By combining high-resolution transmission electron microscopy (HRTEM) characterization and electrical measurements on a unique device platform, we study the reversible electrically-driven phase-change characteristics of self-assembled Ge(2)Sb(2)Te(5) nanowires. Detailed HRTEM analyses are used to correlate and understand the effect of full and intermediate structural transformations on the measured electrical properties of the nanowire devices. The study demonstrates that our unique approach has the potential to provide new information regarding the dynamic structural and electrical states of phase-change materials at the nanoscale, which will aid the design of future phase-change memory devices. PMID:21271735

  4. Real-time high-resolution transmission electron microscopy observation of the growth process of ( 0 0 1 ) surfaces on a nanometer-sized Si multiply twinned particle

    NASA Astrophysics Data System (ADS)

    Takeguchi, Masaki; Tanaka, Miyoko; Yasuda, Hidehiro; Furuya, Kazuo

    2001-11-01

    A nanometer-sized Si multiply twinned particle (MTP) was fabricated by electron-induced SiO 2-decomposition technique inside an ultrahigh vacuum electron microscope. Structure and growth kinetics of the (0 0 1) surface on the MTP were observed by profile imaging high-resolution transmission electron microscopy (HRTEM). Real-time HRTEM observation indicated that the (0 0 1) surfaces were covered with single domain of 1×2 reconstruction and that a new top-layer formation was accompanied by the break of dimer structure of its subsurface. It was also found that the layer growth on the (0 0 1) surfaces showed an unusual behavior, due to a strain field caused by elastic deformation of the MTP.

  5. Transmission electron microscope studies of extraterrestrial materials

    NASA Technical Reports Server (NTRS)

    Keller, Lindsay P.

    1995-01-01

    Transmission Electron Microscopy, X-Ray spectrometry and electron-energy-loss spectroscopy are used to analyse carbon in interplanetary dust particles. Optical micrographs are shown depicting cross sections of the dust particles embedded in sulphur. Selected-area electron diffraction patterns are shown. Transmission Electron Microscope specimens of lunar soil were prepared using two methods: ion-milling and ultramicrotomy. A combination of high resolution TEM imaging and electron diffraction is used to characterize the opaque assemblages. The opaque assemblages analyzed in this study are dominated by ilmenite with lesser rutile and spinel exsolutions, and traces of Fe metal.

  6. Identifying different stacking sequences in few-layer CVD-grown Mo S2 by low-energy atomic-resolution scanning transmission electron microscopy

    NASA Astrophysics Data System (ADS)

    Yan, Aiming; Chen, Wei; Ophus, Colin; Ciston, Jim; Lin, Yuyuan; Persson, Kristin; Zettl, Alex

    2016-01-01

    Atomically thin Mo S2 grown by chemical vapor deposition (CVD) is a promising candidate for next-generation electronics due to inherent CVD scalability and controllability. However, it is well known that the stacking sequence in few-layer Mo S2 can significantly impact electrical and optical properties. Herein we report different intrinsic stacking sequences in CVD-grown few-layer Mo S2 obtained by atomic-resolution annular-dark-field imaging in an aberration-corrected scanning transmission electron microscope operated at 50 keV. Trilayer Mo S2 displays a new stacking sequence distinct from the commonly observed 2 H and 3 R phases of Mo S2 . Density functional theory is used to examine the stability of different stacking sequences, and the findings are consistent with our experimental observations.

  7. Liquid Cell Transmission Electron Microscopy.

    PubMed

    Liao, Hong-Gang; Zheng, Haimei

    2016-05-27

    Liquid cell transmission electron microscopy (TEM) has attracted significant interest in recent years. With nanofabricated liquid cells, it has been possible to image through liquids using TEM with subnanometer resolution, and many previously unseen materials dynamics have been revealed. Liquid cell TEM has been applied to many areas of research, ranging from chemistry to physics, materials science, and biology. So far, topics of study include nanoparticle growth and assembly, electrochemical deposition and lithiation for batteries, tracking and manipulation of nanoparticles, catalysis, and imaging of biological materials. In this article, we first review the development of liquid cell TEM and then highlight progress in various areas of research. In the study of nanoparticle growth, the electron beam can serve both as the illumination source for imaging and as the input energy for reactions. However, many other research topics require the control of electron beam effects to minimize electron beam damage. We discuss efforts to understand electron beam-liquid matter interactions. Finally, we provide a perspective on future challenges and opportunities in liquid cell TEM. PMID:27215823

  8. Liquid Cell Transmission Electron Microscopy

    NASA Astrophysics Data System (ADS)

    Liao, Hong-Gang; Zheng, Haimei

    2016-05-01

    Liquid cell transmission electron microscopy (TEM) has attracted significant interest in recent years. With nanofabricated liquid cells, it has been possible to image through liquids using TEM with subnanometer resolution, and many previously unseen materials dynamics have been revealed. Liquid cell TEM has been applied to many areas of research, ranging from chemistry to physics, materials science, and biology. So far, topics of study include nanoparticle growth and assembly, electrochemical deposition and lithiation for batteries, tracking and manipulation of nanoparticles, catalysis, and imaging of biological materials. In this article, we first review the development of liquid cell TEM and then highlight progress in various areas of research. In the study of nanoparticle growth, the electron beam can serve both as the illumination source for imaging and as the input energy for reactions. However, many other research topics require the control of electron beam effects to minimize electron beam damage. We discuss efforts to understand electron beam-liquid matter interactions. Finally, we provide a perspective on future challenges and opportunities in liquid cell TEM.

  9. Identifying the crystallinity, phase, and arsenic uptake of the nanomineral schwertmannite using analytical high resolution transmission electron microscopy

    NASA Astrophysics Data System (ADS)

    French, R. A.; Kim, B.; Murayama, M.; Hochella, M. F.

    2010-12-01

    Schwertmannite, an iron oxyhydroxide sulfate nanomineral, plays a significant role in the geochemistry of acid mine drainage (AMD) as a metastable phase with respect to goethite and by retaining toxic metals, e.g. arsenic [1]. Schwertmannite’s characteristic morphology is needles 100-300 nm long and only 5-10 nm in diameter extending from a dense aggregate. The poorly-and nano-crystalline nature of this mineral requires using high resolution electron microscopy (HRTEM) to be fully characterized. We used HRTEM to identify the polyphasic nature of natural samples of schwertmannite collected from the Iberian Pyrite Belt in Spain. In order to analyze the dense core, samples were prepared in thin section using an ultramicrotome. Data on a sample identified as pure schwertmannite through powder XRD shows the presence of 5-10 nm goethite nanocrystals making up a significant portion of one of the nanoneedle tips (Figure 1). These nanocrystals exhibit lattice fringes and faceted surfaces, both of which match that expected for goethite. The great majority of the nanoneedles are poorly-crystalline (no lattice fringes) with atomically rough surfaces which may be highly active in the uptake of As. The presence of a range of phases and crystallinities in this sample demonstrate incipient stages of the mechanism that results in transformation of schwertmannite to goethite. Further analytical TEM analyses will help us track sorption/desorption, as well as the specific locations of As within these materials upon initial formation, as well as during transformation. [1] Acero et al. (2006) GCA 70, 4130-4139. Figure 1. HRTEM image of 'schwertmannite' nanoneedle with FFT data (inset).

  10. Local symmetry breaking of a thin crystal structure of β-Si3N4 as revealed by spherical aberration corrected high-resolution transmission electron microscopy images.

    PubMed

    Kim, Hwang Su; Zhang, Zaoli; Kaiser, Ute

    2012-06-01

    This report is an extension of the study for structural imaging of 5-6 nm thick β-Si(3)N(4) [0001] crystal with a spherical aberration corrected transmission electron microscope by Zhang and Kaiser [2009. Structure imaging of β-Si(3)N(4) by spherical aberration-corrected high-resolution transmission electron microscopy. Ultramicroscopy 109, 1114-1120]. In this work, a local symmetry breaking with an uneven resolution of dumbbells in the six-membered rings revealed in the reported images in the study of Zhang and Kaiser has been analyzed in detail. It is found that this local asymmetry in the image basically is not relevant to a slight mistilt of the specimen and/or a beam tilt (coma). Rather the certain variation of the tetrahedral bond length of Si-N(4) in the crystal structure is found to be responsible for the uneven resolution with a local structural variation from region to region. This characteristic of the variation is also supposed to give a distorted lattice of apparently 2°-2.5° deviations from the perfect hexagonal unit cell as observed in the reported image in the work of Zhang and Kaiser. It is discussed that this variation may prevail only in a thin specimen with a thickness ranging ~≤ 5-6 nm. At the same time, it is noted that the average of the bond length variation is close to the fixed length known in a bulk crystal of β-Si(3)N(4). PMID:22499470

  11. Determination of crystal growth rates during rapid solidification of polycrystalline aluminum by nano-scale spatio-temporal resolution in situ transmission electron microscopy

    NASA Astrophysics Data System (ADS)

    Zweiacker, K.; McKeown, J. T.; Liu, C.; LaGrange, T.; Reed, B. W.; Campbell, G. H.; Wiezorek, J. M. K.

    2016-08-01

    In situ investigations of rapid solidification in polycrystalline Al thin films were conducted using nano-scale spatio-temporal resolution dynamic transmission electron microscopy. Differences in crystal growth rates and asymmetries in melt pool development were observed as the heat extraction geometry was varied by controlling the proximity of the laser-pulse irradiation and the associated induced melt pools to the edge of the transmission electron microscopy support grid, which acts as a large heat sink. Experimental parameters have been established to maximize the reproducibility of the material response to the laser-pulse-related heating and to ensure that observations of the dynamical behavior of the metal are free from artifacts, leading to accurate interpretations and quantifiable measurements with improved precision. Interface migration rate measurements revealed solidification velocities that increased consistently from ˜1.3 m s-1 to ˜2.5 m s-1 during the rapid solidification process of the Al thin films. Under the influence of an additional large heat sink, increased crystal growth rates as high as 3.3 m s-1 have been measured. The in situ experiments also provided evidence for development of a partially melted, two-phase region prior to the onset of rapid solidification facilitated crystal growth. Using the experimental observations and associated measurements as benchmarks, finite-element modeling based calculations of the melt pool evolution after pulsed laser irradiation have been performed to obtain estimates of the temperature evolution in the thin films.

  12. Preparation and Loading Process of Single Crystalline Samples into a Gas Environmental Cell Holder for In Situ Atomic Resolution Scanning Transmission Electron Microscopic Observation.

    PubMed

    Straubinger, Rainer; Beyer, Andreas; Volz, Kerstin

    2016-06-01

    A reproducible way to transfer a single crystalline sample into a gas environmental cell holder for in situ transmission electron microscopic (TEM) analysis is shown in this study. As in situ holders have only single-tilt capability, it is necessary to prepare the sample precisely along a specific zone axis. This can be achieved by a very accurate focused ion beam lift-out preparation. We show a step-by-step procedure to prepare the sample and transfer it into the gas environmental cell. The sample material is a GaP/Ga(NAsP)/GaP multi-quantum well structure on Si. Scanning TEM observations prove that it is possible to achieve atomic resolution at very high temperatures in a nitrogen environment of 100,000 Pa. PMID:27026281

  13. Atomic arrangement at ZnTe/CdSe interfaces determined by high resolution scanning transmission electron microscopy and atom probe tomography

    SciTech Connect

    Bonef, Bastien; Rouvière, Jean-Luc; Jouneau, Pierre-Henri; Bellet-Amalric, Edith; Gérard, Lionel; Mariette, Henri; André, Régis; Bougerol, Catherine; Grenier, Adeline

    2015-02-02

    High resolution scanning transmission electron microscopy and atom probe tomography experiments reveal the presence of an intermediate layer at the interface between two binary compounds with no common atom, namely, ZnTe and CdSe for samples grown by Molecular Beam Epitaxy under standard conditions. This thin transition layer, of the order of 1 to 3 atomic planes, contains typically one monolayer of ZnSe. Even if it occurs at each interface, the direct interface, i.e., ZnTe on CdSe, is sharper than the reverse one, where the ZnSe layer is likely surrounded by alloyed layers. On the other hand, a CdTe-like interface was never observed. This interface knowledge is crucial to properly design superlattices for optoelectronic applications and to master band-gap engineering.

  14. Restoring defect structures in 3C-SiC/Si (001) from spherical aberration-corrected high-resolution transmission electron microscope images by means of deconvolution processing.

    PubMed

    Wen, C; Wan, W; Li, F H; Tang, D

    2015-04-01

    The [110] cross-sectional samples of 3C-SiC/Si (001) were observed with a spherical aberration-corrected 300 kV high-resolution transmission electron microscope. Two images taken not close to the Scherzer focus condition and not representing the projected structures intuitively were utilized for performing the deconvolution. The principle and procedure of image deconvolution and atomic sort recognition are summarized. The defect structure restoration together with the recognition of Si and C atoms from the experimental images has been illustrated. The structure maps of an intrinsic stacking fault in the area of SiC, and of Lomer and 60° shuffle dislocations at the interface have been obtained at atomic level. PMID:25637810

  15. Opto-mechano-electrical tripling in ZnO nanowires probed by photocurrent spectroscopy in a high-resolution transmission electron microscope

    SciTech Connect

    Zhang, C.; Golberg, D. E-mail: golberg.dmitri@nims.go.jp; Xu, Z. E-mail: golberg.dmitri@nims.go.jp; Kvashnin, D. G.; Tang, D.-M.; Xue, Y. M.; Bando, Y.; Sorokin, P. B.

    2015-08-31

    Photocurrent spectroscopy of individual free-standing ZnO nanowires inside a high-resolution transmission electron microscope (TEM) is reported. By using specially designed optical in situ TEM system capable of scanning tunneling microscopy probing paired with light illumination, opto-mechano-electrical tripling phenomenon in ZnO nanowires is demonstrated. Splitting of photocurrent spectra at around 3.3 eV under in situ TEM bending of ZnO nanowires directly corresponds to nanowire deformation and appearance of expanded and compressed nanowire sides. Theoretical simulation of a bent ZnO nanowire has an excellent agreement with the experimental data. The splitting effect could be explained by a change in the valence band structure of ZnO nanowires due to a lattice strain. The strain-induced splitting provides important clues for future flexible piezo-phototronics.

  16. Nanouric acid or nanocalcium phosphate as central nidus to induce calcium oxalate stone formation: a high-resolution transmission electron microscopy study on urinary nanocrystallites

    PubMed Central

    Gao, Jie; Xue, Jun-Fa; Xu, Meng; Gui, Bao-Song; Wang, Feng-Xin; Ouyang, Jian-Ming

    2014-01-01

    Purpose This study aimed to accurately analyze the relationship between calcium oxalate (CaOx) stone formation and the components of urinary nanocrystallites. Method High-resolution transmission electron microscopy (HRTEM), selected area electron diffraction, fast Fourier transformation of HRTEM, and energy dispersive X-ray spectroscopy were performed to analyze the components of these nanocrystallites. Results The main components of CaOx stones are calcium oxalate monohydrate and a small amount of dehydrate, while those of urinary nanocrystallites are calcium oxalate monohydrate, uric acid, and calcium phosphate. The mechanism of formation of CaOx stones was discussed based on the components of urinary nanocrystallites. Conclusion The formation of CaOx stones is closely related both to the properties of urinary nanocrystallites and to the urinary components. The combination of HRTEM, fast Fourier transformation, selected area electron diffraction, and energy dispersive X-ray spectroscopy could be accurately performed to analyze the components of single urinary nanocrystallites. This result provides evidence for nanouric acid and/or nanocalcium phosphate crystallites as the central nidus to induce CaOx stone formation. PMID:25258530

  17. Determination of crystal growth rates during rapid solidification of polycrystalline aluminum by nano-scale spatio-temporal resolution in situ transmission electron microscopy

    DOE PAGESBeta

    Zweiacker, K.; McKeown, J. T.; Liu, C.; LaGrange, T.; Reed, B. W.; Campbell, G. H.; Wiezorek, J. M. K.

    2016-08-04

    In situ investigations of rapid solidification in polycrystalline Al thin films were conducted using nano-scale spatio-temporal resolution dynamic transmission electron microscopy. Differences in crystal growth rates and asymmetries in melt pool development were observed as the heat extraction geometry was varied by controlling the proximity of the laser-pulse irradiation and the associated induced melt pools to the edge of the transmission electron microscopy support grid, which acts as a large heat sink. Experimental parameters have been established to maximize the reproducibility of the material response to the laser-pulse-related heating and to ensure that observations of the dynamical behavior of themore » metal are free from artifacts, leading to accurate interpretations and quantifiable measurements with improved precision. Interface migration rate measurements revealed solidification velocities that increased consistently from ~1.3 m s–1 to ~2.5 m s–1 during the rapid solidification process of the Al thin films. Under the influence of an additional large heat sink, increased crystal growth rates as high as 3.3 m s–1 have been measured. The in situ experiments also provided evidence for development of a partially melted, two-phase region prior to the onset of rapid solidification facilitated crystal growth. As a result, using the experimental observations and associated measurements as benchmarks, finite-element modeling based calculations of the melt pool evolution after pulsed laser irradiation have been performed to obtain estimates of the temperature evolution in the thin films.« less

  18. Electron Diffraction Using Transmission Electron Microscopy

    PubMed Central

    Bendersky, Leonid A.; Gayle, Frank W.

    2001-01-01

    Electron diffraction via the transmission electron microscope is a powerful method for characterizing the structure of materials, including perfect crystals and defect structures. The advantages of electron diffraction over other methods, e.g., x-ray or neutron, arise from the extremely short wavelength (≈2 pm), the strong atomic scattering, and the ability to examine tiny volumes of matter (≈10 nm3). The NIST Materials Science and Engineering Laboratory has a history of discovery and characterization of new structures through electron diffraction, alone or in combination with other diffraction methods. This paper provides a survey of some of this work enabled through electron microscopy.

  19. High resolution transmission electron microscopy study of the hardening mechanism through phase separation in a beta-Ti-35Nb-7Zr-5Ta alloy for implant applications.

    PubMed

    Afonso, Conrado R M; Ferrandini, Peterson L; Ramirez, Antonio J; Caram, Rubens

    2010-04-01

    beta-Ti alloys are highly attractive metallic materials for biomedical applications due to their high specific strength, high corrosion resistance and excellent biocompatibility, including low elastic modulus. This work aims to clarify the hardening mechanism of a beta-Ti-Nb-Zr-Ta alloy using different characterization techniques. Ingots (50 g) of Ti-35Nb-7Zr-5Ta (wt.%) alloy were arc furnace melted in an Ar((g)) atmosphere, homogenized, hot rolled, solubilized and finally aged at several temperatures from 200 to 700 degrees C for 4 h. Microstructure characterization was performed using X-ray diffraction, optical microscopy, scanning and high resolution transmission electron microscopy (HR-TEM). The 4 h aging showed that the highest hardness values were found when aged at 400 degrees C and the HR-TEM images confirmed splitting of spots on the Fourier space map, which indicated the presence of a coherent interface between separated phases (beta and beta') and explains the hardening mechanism of the alloy. Through geometric phase analysis analysis, using the HR-TEM image, the localized strain map showed 5-10 nm domains of the beta and beta' phases. The combination of suitable values of yield strength, hardness and low Young's modulus makes Ti-35Nb-7Zr-5Ta alloy suitable for medical applications as a metallic orthopedic implant. PMID:19913645

  20. Evaluation of stacking faults and associated partial dislocations in AlSb/GaAs (001) interface by aberration-corrected high-resolution transmission electron microscopy

    SciTech Connect

    Wen, C.; Ge, B. H.; Cui, Y. X.; Li, F. H.; Zhu, J.; Yu, R.; Cheng, Z. Y.

    2014-11-15

    The stacking faults (SFs) in an AlSb/GaAs (001) interface were investigated using a 300 kV spherical aberration-corrected high-resolution transmission electron microscope (HRTEM). The structure and strain distribution of the single and intersecting (V-shaped) SFs associated with partial dislocations (PDs) were characterized by the [110] HRTEM images and geometric phase analysis, respectively. In the biaxial strain maps ε{sub xx} and ε{sub yy}, a SF can be divided into several sections under different strain states (positive or negative strain values). Furthermore, the strain state for the same section of a SF is in contrast to each other in ε{sub xx} and ε{sub yy} strain maps. The modification in the strain states was attributed to the variation in the local atomic displacements for the SF in the AlSb film on the GaAs substrate recorded in the lattice image. Finally, the single SF was found to be bounded by two 30° PDs. A pair of 30° PDs near the heteroepitaxial interface reacted to form a Lomer-Cottrell sessile dislocation located at the vertices of V-shaped SFs with opposite screw components. The roles of misfit dislocations, such as the PDs, in strain relaxation were also discussed.

  1. Microstructure analysis of epitaxially grown self-assembled Ge islands on nanometer-scale patterned SiO2/Si substrates by high-resolution transmission electron microscopy

    NASA Astrophysics Data System (ADS)

    Yoon, Tae-Sik; Kim, Hyun-Mi; Kim, Ki-Bum; Ryu, Du Yeol; Russell, Thomas P.; Zhao, Zuoming; Liu, Jian; Xie, Ya-Hong

    2007-11-01

    The microstructure of epitaxially grown self-assembled Ge islands on patterned SiO2/Si substrates was analyzed using high resolution transmission electron microscopy. The Ge islands were grown by molecular beam epitaxy on hexagonally ordered Si hole arrays with ˜25 nm diameter and ˜40 nm center-to-center distance, which are covered by 30 nm thick SiO2 mask layer patterned using self-assembled diblock copolymers. The Ge islands nucleate preferentially at the edge of overetched Si surface, and subsequently grow selectively on Si surface as opposed to SiO2 surface with increasing coverage. The lattice planes of some Ge islands are tilted from those of Si substrates. This is believed to be the reason for the observed misalignment of moiré fringes. The diameter of the Ge islands is identical to that of Si holes for large Ge coverage due to the selective growth behavior. These islands are found to have dislocations at the interface with the Si substrate. These results highlight the important microstructural issues and growth behavior of quantum dots on patterned substrates.

  2. Wavelet encoding and variable resolution progressive transmission

    NASA Technical Reports Server (NTRS)

    Blanford, Ronald P.

    1993-01-01

    Progressive transmission is a method of transmitting and displaying imagery in stages of successively improving quality. The subsampled lowpass image representations generated by a wavelet transformation suit this purpose well, but for best results the order of presentation is critical. Candidate data for transmission are best selected using dynamic prioritization criteria generated from image contents and viewer guidance. We show that wavelets are not only suitable but superior when used to encode data for progressive transmission at non-uniform resolutions. This application does not preclude additional compression using quantization of highpass coefficients, which to the contrary results in superior image approximations at low data rates.

  3. Evidence for anisotropic dielectric properties of monoclinic hafnia using valence electron energy-loss spectroscopy in high-resolution transmission electron microscopy and ab initio time-dependent density-functional theory

    NASA Astrophysics Data System (ADS)

    Guedj, C.; Hung, L.; Zobelli, A.; Blaise, P.; Sottile, F.; Olevano, V.

    2014-12-01

    The effect of nanocrystal orientation on the energy loss spectra of monoclinic hafnia (m-HfO2) is measured by high resolution transmission electron microscopy (HRTEM) and valence energy loss spectroscopy (VEELS) on high quality samples. For the same momentum-transfer directions, the dielectric properties are also calculated ab initio by time-dependent density-functional theory (TDDFT). Experiments and simulations evidence anisotropy in the dielectric properties of m-HfO2, most notably with the direction-dependent oscillator strength of the main bulk plasmon. The anisotropic nature of m-HfO2 may contribute to the differences among VEELS spectra reported in literature. The good agreement between the complex dielectric permittivity extracted from VEELS with nanometer spatial resolution, TDDFT modeling, and past literature demonstrates that the present HRTEM-VEELS device-oriented methodology is a possible solution to the difficult nanocharacterization challenges given in the International Technology Roadmap for Semiconductors.

  4. Evidence for anisotropic dielectric properties of monoclinic hafnia using valence electron energy-loss spectroscopy in high-resolution transmission electron microscopy and ab initio time-dependent density-functional theory

    SciTech Connect

    Guedj, C.; Hung, L.; Sottile, F.; Zobelli, A.; Blaise, P.; Olevano, V.

    2014-12-01

    The effect of nanocrystal orientation on the energy loss spectra of monoclinic hafnia (m-HfO{sub 2}) is measured by high resolution transmission electron microscopy (HRTEM) and valence energy loss spectroscopy (VEELS) on high quality samples. For the same momentum-transfer directions, the dielectric properties are also calculated ab initio by time-dependent density-functional theory (TDDFT). Experiments and simulations evidence anisotropy in the dielectric properties of m-HfO{sub 2}, most notably with the direction-dependent oscillator strength of the main bulk plasmon. The anisotropic nature of m-HfO{sub 2} may contribute to the differences among VEELS spectra reported in literature. The good agreement between the complex dielectric permittivity extracted from VEELS with nanometer spatial resolution, TDDFT modeling, and past literature demonstrates that the present HRTEM-VEELS device-oriented methodology is a possible solution to the difficult nanocharacterization challenges given in the International Technology Roadmap for Semiconductors.

  5. Ponderomotive phase plate for transmission electron microscopes

    DOEpatents

    Reed, Bryan W.

    2012-07-10

    A ponderomotive phase plate system and method for controllably producing highly tunable phase contrast transfer functions in a transmission electron microscope (TEM) for high resolution and biological phase contrast imaging. The system and method includes a laser source and a beam transport system to produce a focused laser crossover as a phase plate, so that a ponderomotive potential of the focused laser crossover produces a scattering-angle-dependent phase shift in the electrons of the post-sample electron beam corresponding to a desired phase contrast transfer function.

  6. High resolution low dose transmission electron microscopy real-time imaging and manipulation of nano-scale objects in the electron beam

    DOEpatents

    Brown, Jr., R. Malcolm; Barnes, Zack; Sawatari, Chie; Kondo, Tetsuo

    2008-02-26

    The present invention includes a method, apparatus and system for nanofabrication in which one or more target molecules are identified for manipulation with an electron beam and the one or more target molecules are manipulated with the electron beam to produce new useful materials.

  7. Crystal Structures of U(Ta,W) 5O 16and U(Ta,W) 2O 8Revealed by High-Resolution Transmission Electron Microscopy

    NASA Astrophysics Data System (ADS)

    Askeljung, Charlotta; Sundberg, Margareta

    1999-04-01

    Two new phases, U(Ta,W)5O16and U(Ta,W)2O8, were formed by solid state reaction of the binary oxides (U3O8, Ta2O5, and WO3) and Ta metal powder. They were characterized by high-resolution transmission electron microscopy and X-ray powder diffraction techniques. The phases are orthorhombic with the following unit cell dimensions: U(Ta,W)5O16,a=10.052(1),b=7.3207(5), andc=7.9600(4) Å; and U(Ta,W)2O8,a= 20.232(2),b=7.4520(4), andc=4.0652(2) Å. Both structures are built up of (Ta,W)O6-octahedra arranged as ReO3-type slabs two octahedra wide. In U(Ta,W)5O16these slabs are connected by a thin lamella consisting of hexagonal UO8-bipyramids and (Ta,W)O6-octahedra alternating along both thebandcaxes. EDS analysis indicated a composition of UTa1.5W3.5O16. The structure is related to UMo5O16, but with every other layer displaced through {1}/{2}b. The second phase, U(Ta,W)2O8, is isotypic with the orthorhombic modification of UMo2O8, in which the ReO3-type slabs are intergrown with lamellas of edge-sharing pentagonal UO7-bipyramids. The composition UTa0.5W1.5O8was obtained by EDS analysis. Some defects in terms of three-octahedra-wide ReO3-type slabs have been observed in U(Ta,W)5O16crystals. EDS analyses of such crystals showed a high-tungsten and a low-tantalum content.

  8. Characterization of the (0110) {alpha}-Ti/{gamma}-TiH interface using high-resolution Transmission Electron Microscopy (TEM) and Electron Energy Loss Spectroscopy (EELS)

    SciTech Connect

    Tsai, M.M.; Howe, J.M.

    1996-12-31

    Precipitation of {gamma}-TiH in {alpha}-Ti-H alloys involves a hcp {r_arrow} fct lattice transformation with hydrogen as an interstitial diffusing element. Results obtained from a previous TEM study have shown that the lengthening rate of {gamma}-TiH is diffusionally controlled at 25{degrees}C, and possibly interfacially controlled at temperatures of 50{degrees}C and higher. Therefore, it is essential to ascertain the presence or absence of hydrogen atoms at the interface. TEM foils from a 800 ppm wt.% Ti-H alloy were analyzed using high-resolution TEM and image simulations in order to determine the effects of hydrogen on high-resolution images of the {alpha}-Ti/{gamma}-TiH interface, and EELS was used to determine the whether the hydride structure was fully formed up to the interface.

  9. Large-Volume Reconstruction of Brain Tissue from High-Resolution Serial Section Images Acquired by SEM-Based Scanning Transmission Electron Microscopy

    PubMed Central

    Kuwajima, Masaaki; Mendenhall, John M.; Harris, Kristen M.

    2013-01-01

    With recent improvements in instrumentation and computational tools, serial section electron microscopy has become increasingly straightforward. A new method for imaging ultrathin serial sections is developed based on a field emission scanning electron microscope fitted with a transmitted electron detector. This method is capable of automatically acquiring high-resolution serial images with a large field size and very little optical and physical distortions. In this chapter, we describe the procedures leading to the generation and analyses of a large-volume stack of high-resolution images (64 μm × 64 μm × 10 μm, or larger, at 2 nm pixel size), including how to obtain large-area serial sections of uniform thickness from well-preserved brain tissue that is rapidly perfusion-fixed with mixed aldehydes, processed with a microwave-enhanced method, and embedded into epoxy resin. PMID:23086880

  10. Evolution of titania nanotubes-supported WO{sub x} species by in situ thermo-Raman spectroscopy, X-ray diffraction and high resolution transmission electron microscopy

    SciTech Connect

    Cortes-Jacome, M.A.; Angeles-Chavez, C.; Morales, M.; Lopez-Salinas, E.; Toledo-Antonio, J.A.

    2007-10-15

    Structural evolution of WO{sub x} species on the surface of titania nanotubes was followed by in situ thermo-Raman spectroscopy. A total of 15 wt% of W atoms were loaded on the surface of a hydroxylated titania nanotubes by impregnation with ammonium metatungstate solution and then, the sample was thermally treated in a Linkam cell at different temperatures in nitrogen flow. The band characteristic of the W=O bond was observed at 962 cm{sup -1} in the dried sample, which vanished between 300 and 700 deg. C, and reappear again after annealing at 800 deg. C, along with a broad band centered at 935 cm{sup -1}, attributed to the v{sub 1} vibration of W=O in tetrahedral coordination. At 900 and 1000 deg. C, the broad band decomposed into four bands at 923, 934, 940 and 950 cm{sup -1}, corresponding to the symmetric and asymmetric vibration of W=O bonds in Na{sub 2}WO{sub 4} and Na{sub 2}W{sub 2}O{sub 7} phases as determined by X-ray diffraction and High resolution transmission electron microscopy (HRTEM). The structure of the nanotubular support was kept at temperatures below 450 deg. C, thereafter, it transformed into anatase being stabilized at temperatures as high as 900 deg. C. At 1000 deg. C, anatase phase partially converted into rutile. After annealing at 1000 deg. C, a core-shell model material was obtained, with a shell of ca. 5 nm thickness, composed of sodium tungstate nanoclusters, and a core composed mainly of rutile TiO{sub 2} phase. - Graphical abstract: Titania nanotubes loaded with 15 wt% W atoms were characterized from room temperature (rt) to 1000 deg. C by thermo-Raman spectroscopy in N{sub 2}. At 1000 deg. C, a core-shell model material was obtained, with a shell thickness of ca. 5 nm composed by nanoclusters of sodium tungstate, and a core composed mainly of rutile TiO{sub 2} phase.

  11. A high-resolution transmission electron microscopy study of interfaces between the γ, B2, and α2 phases in a Ti-Al-Mo alloy

    NASA Astrophysics Data System (ADS)

    Das, S.; Howe, J. M.; Perepezko, J. H.

    1996-06-01

    Conventional and high-resolution transmission electron microscopy (HRTEM) were used to examine the interfacial structures in a Ti-50Al-5Mo (at. pct) alloy which was processed to produce combinations of γ, B2, and α2 phases in a single sample. A small amount of a fourth phase labeled ζ was also found in the microstructure. It may be the phase Ti2AlN but confirmation requires analysis of the N content in the phase.In this alloy, the orientation relationship between the γ and B2 phases is {111}γ ∥}110}B2 and <101]γ ∥ <111>B2 with a coherent habit-plane interface parallel to (474)γ. The orientation relationship between the B2 and α2 (and also the ζ @#@) phases is {110}B2 ∥(0001)α2/ζ and <111>B2 ∥<11-20>α2/ζ with a coherent interface parallel to the close-packed planes and along other orientations. The orientation relationship between the α2 (and also the ζ @#@) and γ phases is (0001)α2/ζ ∥{lll}γ and (11•20)α2/ζ ∥<10•1]γ. The α2 phase has a coherent interface parallel to the close-packed planes, while the ζ phase appears to adopt the (474)γ interface plane of the γ phase, similar to the B2 phase. In some cases, the interface configuration between the γ and B2 phases appears to be altered by the presence of α2 phase, resulting in a semicoherent interface. The phase labeled ζ in this study has the same orientation relationship with the γ and B2 phases as α2 but consists of an ABABAC... stacking of close-packed basal planes. The (474)γ habit plane interface between the γ and B2 phases is analyzed by several different theories of interfacial structure, and microstructural evolution in this system is also discussed.

  12. Understanding the promotion effect: A density functional theory study based on high resolution transmission electron microscopy images for molybdenum disulfide-cobalt promoted interfaces

    NASA Astrophysics Data System (ADS)

    Ramos Murillo, Manuel Antonio

    could expect. The meaning could be understood in terms of energetic limits required to nucleate at the MoS2 basal planes. In recent years, in the literature a complete study made by Scanning Tunneling Microscope and DFT calculations for specific herringbone structure on MoS2/Au crystallites, indicating with this the latest results in advance characterization, this research path let catalysis experts to look over new techniques to achieve a complete characterization in nano structured materials. Finally we present here a complete density functional theory and HRTEM study to indicate how two structures MoS2 and Co9S 8 acted together in the formation of the so-called CoMoS phase. In this particular work one can find data based on Density of States and Band Structure calculations of MoS2/Co9S8 interface as well as real time images of high resolution transmission electron microscope (HRTEM), and finally a proposed computational molecular structure to explain the promotion effect in MoS2 nano-structures.

  13. Electron diffraction and high-resolution transmission electron microscopy of the high temperature crystal structures of GexSb2Te3+x (x=1,2,3) phase change material

    NASA Astrophysics Data System (ADS)

    Kooi, B. J.; De Hosson, J. Th. M.

    2002-10-01

    The crystal structures of GeSb2Te4, Ge2Sb2Te5, and Ge3Sb2Te6 were determined using electron diffraction and high-resolution transmission electron microscopy. The structure determined for the former two crystals deviates from the ones proposed in the literature. These crystal structures were developed jointly upon cooling of liquid Ge2Sb2Te5. A stacking disorder parallel to the basal plane was observed that increases with increasing cooling rates. For the GexSb2Te3+x (x=1,2,3) crystals it is shown that an a,b,c stacking holds with an alternating stacking of x GeTe double layers identically present in binary GeTe and one Te-Sb-Te-Te-Sb- repeat unit also present in binary Sb2Te3. A stacking disorder is a logical consequence of building crystals with these two principal units. On the other hand, it is likely that all stable crystals of the Ge-Sb-Te systems are an ordered sequence of these two units. Some of the implications of these findings of the stable and metastable crystal structures that develop from amorphous Ge2Sb2Te5 are presented so as to understand the crucial crystallization process in Ge2Sb2Te5 phase change material.

  14. Low Resolution Picture Transmission (LRPT) Demonstration System

    NASA Technical Reports Server (NTRS)

    Fong, Wai; Yeh, Pen-Shu; Sank, Victor; Nyugen, Xuan; Xia, Wei; Duran, Steve; Day, John H. (Technical Monitor)

    2002-01-01

    Low-Resolution Picture Transmission (LRPT) is a proposed standard for direct broadcast transmission of satellite weather images. This standard is a joint effort by the European Organization for the Exploitation of Meteorological Satellites (EUMETSAT) and the National Oceanic Atmospheric Administration (NOAA). As a digital transmission scheme, its purpose is to replace the current analog Automatic Picture Transmission (APT) system for use in the Meteorological Operational (METOP) satellites. Goddard Space Flight Center has been tasked to build an LRPT Demonstration System (LDS). It's main objective is to develop or demonstrate the feasibility of a low-cost receiver utilizing a Personal Computer (PC) as the primary processing component and determine the performance of the protocol in the simulated Radio Frequency (RF) environment. The approach would consist of two phases. In the phase 1, a Commercial-off-the-Shelf (COTS) Modulator-Demodulator (MODEM) board that would perform RF demodulation would be purchased allowing the Central Processing Unit (CPU) to perform the Consultative Committee for Space Data Systems (CCSDS) protocol processing. Also since the weather images are compressed the PC would perform the decompression. Phase 1 was successfully demonstrated on December 1997. Phase 2 consists of developing a high-fidelity receiver, transmitter and environment simulator. Its goal is to find out how the METOP Specification performs in a simulated noise environment in a cost-effective receiver. The approach would be to produce a receiver using as much software as possible to perform front-end processing to take advantage of the latest high-speed PCs. Thus the COTS MODEM used in Phase 1 is performing RF demodulation along with data acquisition providing data to the receiving software. Also, environment simulator is produced using the noise patterns generated by Institute for Telecommunications Sciences (ITS) from their noise environment study.

  15. Characterization of a high resolution transmission grating

    NASA Astrophysics Data System (ADS)

    Desauté, P.; Merdji, H.; Greiner, V.; Missalla, T.; Chenais-Popovics, C.; Troussel, P.

    2000-01-01

    Three 5000 lines/mm gold transmission gratings have been tested with the radiation from the Super-ACO synchrotron in the range 250 eV< E<850 eV. Typical results for the spectral dependence of the grating efficiency at different diffraction orders are presented. This grating theoretically built to have no second order exhibits second order as high as 15-20% of first order. The very thin 5000 L/mm gratings are supported by a larger grid which perturbs the recorded data by separating each order in three peaks. Fraunhofer diffraction of the support grid has been modelled and can explain this effect. The high resolution gratings were used to measure the harmonics of the beamline monochromator grating (550 L/mm) and to measure the emission and absorption of laser-produced plasmas in the XUV range.

  16. Oxidation products of the niobium tungsten oxide Nb{sub 4}W{sub 13}O{sub 47}: A high-resolution scanning transmission electron microscopy study

    SciTech Connect

    Krumeich, Frank . E-mail: krumeich@inorg.chem.ethz.ch; Nesper, Reinhard

    2006-06-15

    Nb{sub 4}W{sub 13}O{sub 47}, a member of the solid solution series Nb{sub 8-n}W{sub 9+n}O{sub 47} (0=transmission electron microscopy applying a high-angle annular dark field detector. At the selected imaging conditions (Z contrast), not only the metal positions are revealed by this technique but valuable additional information about the elemental distribution can be obtained simultaneously.

  17. High-resolution transmission electron microscopy study on the growth modes of GaSb islands grown on a semi-insulating GaAs (001) substrate

    NASA Astrophysics Data System (ADS)

    Kim, Y. H.; Lee, J. Y.; Noh, Y. G.; Kim, M. D.; Oh, J. E.

    2007-06-01

    The initial growth behaviors of GaSb on a GaAs substrate were studied using a high-resolution electron microscope (HRTEM). Four types of GaSb islands were observed by HRTEM. HRTEM micrographs showed that strain relaxation mechanisms were different in the four types of islands. Although 90° misfit dislocations relieve misfit strain in the islands, additional mechanisms are required to relax the remaining strain. The existence of elastic deformation near the surface related to dislocations and intermediate layers between GaSb and GaAs were demonstrated in island growths. Finally, the generation of planar defects to relieve strain was observed in a specific GaSb growth.

  18. Quantitative Phase Retrieval in Transmission Electron Microscopy

    NASA Astrophysics Data System (ADS)

    McLeod, Robert Alexander

    Phase retrieval in the transmission electron microscope offers the unique potential to collect quantitative data regarding the electric and magnetic properties of materials at the nanoscale. Substantial progress in the field of quantitative phase imaging was made by improvements to the technique of off-axis electron holography. In this thesis, several breakthroughs have been achieved that improve the quantitative analysis of phase retrieval. An accurate means of measuring the electron wavefront coherence in two-dimensions was developed and pratical applications demonstrated. The detector modulation-transfer function (MTF) was assessed by slanted-edge, noise, and the novel holographic techniques. It was shown the traditional slanted-edge technique underestimates the MTF. In addition, progress was made in dark and gain reference normalization of images, and it was shown that incomplete read-out is a concern for slow-scan CCD detectors. Last, the phase error due to electron shot noise was reduced by the technique of summation of hologram series. The phase error, which limits the finest electric and magnetic phenomena which can be investigated, was reduced by over 900 % with no loss of spatial resolution. Quantitative agreement between the experimental root-mean-square phase error and the analytical prediction of phase error was achieved.

  19. Defining Electron Backscatter Diffraction Resolution

    SciTech Connect

    El-Dasher, B S; Rollett, A D

    2005-02-07

    Automated electron backscatter diffraction (EBSD) mapping systems have existed for more than 10 years [1,2], and due to their versatility in characterizing multiple aspects of microstructure, they have become an important tool in microscale crystallographic studies. Their increasingly widespread use however raises questions about their accuracy in both determining crystallographic orientations, as well as ensuring that the orientation information is spatially correct. The issue of orientation accuracy (as defined by angular resolution) has been addressed previously [3-5]. While the resolution of EBSD systems is typically quoted to be on the order of 1{sup o}, it has been shown that by increasing the pattern quality via acquisition parameter adjustment, the angular resolution can be improved to sub-degree levels. Ultimately, the resolution is dependent on how it is identified. In some cases it can be identified as the orientation relative to a known absolute, in others as the misorientation between nearest neighbor points in a scan. Naturally, the resulting values can be significantly different. Therefore, a consistent and universal definition of resolution that can be applied to characterize any EBSD system is necessary, and is the focus of the current study. In this work, a Phillips (FEI) XL-40 FEGSEM coupled to a TexSEM Laboratories OIM system was used. The pattern capturing hardware consisted of both a 512 by 512 pixel SIT CCD camera and a 1300 by 1030 pixel Peltier cooled CCD camera. Automated scans of various sizes, each consisting of 2500 points, were performed on a commercial-grade single crystal silicon wafer used for angular resolution measurements. To adequately quantify angular resolution for all possible EBSD applications we define two angular values. The first is {omega}{sub center}, the mean of the misorientation angle distribution between all scan points and the scan point coincident to the calibration source (typically the scan center). The {omega

  20. Transmission electron microscope CCD camera

    DOEpatents

    Downing, Kenneth H.

    1999-01-01

    In order to improve the performance of a CCD camera on a high voltage electron microscope, an electron decelerator is inserted between the microscope column and the CCD. This arrangement optimizes the interaction of the electron beam with the scintillator of the CCD camera while retaining optimization of the microscope optics and of the interaction of the beam with the specimen. Changing the electron beam energy between the specimen and camera allows both to be optimized.

  1. Quantification of the Information Limit of Transmission Electron Microscopes

    SciTech Connect

    Barthel, J.; Thust, A.

    2008-11-14

    The resolving power of high-resolution transmission electron microscopes is characterized by the information limit, which reflects the size of the smallest object detail observable with a particular instrument. We introduce a highly accurate measurement method for the information limit, which is suitable for modern aberration-corrected electron microscopes. An experimental comparison with the traditionally applied Young's fringe method yields severe discrepancies and confirms theoretical considerations according to which the Young's fringe method does not reveal the information limit.

  2. Analysis of the complexity of the sperm acrosomal membrane by super-resolution stimulated emission depletion microscopy compared with transmission electron microscopy.

    PubMed

    Ito, Chizuru; Yamatoya, Kenji; Toshimori, Kiyotaka

    2015-08-01

    The acrosome is a Golgi-derived sperm cell organelle enclosed by a continuous acrosomal membrane. The acrosomal membrane complexes with surrounding matrices containing molecules necessary for fertilization; however, the complex of acrosomal membrane and associating matrices (CAMAM) has not been visualized in detail under living conditions. Here, we analyzed the CAMAM at the nanometer level using super-resolution stimulated emission depletion (STED) fluorescence microscopy and equatorin-enhanced green fluorescent protein transgenic mice. The STED images were compared with the corresponding images taken by immunoelectron microscopy. Consequently, the substructure of CAMAM could be differentiated at nanometer-scale resolution by STED microscopy without the need for sectioning. The information obtained in this study will be beneficial not only for understanding the molecular mechanism of fertilization but also for cell imaging under living conditions. PMID:25430742

  3. A method to determine fault vectors in 4H-SiC from stacking sequences observed on high resolution transmission electron microscopy images

    SciTech Connect

    Wu, Fangzhen; Wang, Huanhuan; Raghothamachar, Balaji; Dudley, Michael; Mueller, Stephan G.; Chung, Gil; Sanchez, Edward K.; Hansen, Darren; Loboda, Mark J.; Zhang, Lihua; Su, Dong; Kisslinger, Kim; Stach, Eric

    2014-09-14

    A new method has been developed to determine the fault vectors associated with stacking faults in 4H-SiC from their stacking sequences observed on high resolution TEM images. This method, analogous to the Burgers circuit technique for determination of dislocation Burgers vector, involves determination of the vectors required in the projection of the perfect lattice to correct the deviated path constructed in the faulted material. Results for several different stacking faults were compared with fault vectors determined from X-ray topographic contrast analysis and were found to be consistent. This technique is expected to applicable to all structures comprising corner shared tetrahedra.

  4. Atomic-resolution scanning transmission electron microscopy study of the valence state transition in (Pr0.85Y0.15)0.7Ca0.3CoO3

    NASA Astrophysics Data System (ADS)

    Klie, Robert; Gulec, Ahmet; Phelan, Daniel; Leighton, Chris

    2015-03-01

    The observation of a first-order magnetic/electronic transition in certain Pr-based perovskite cobaltites, such as Pr0.5Ca0.5CoO3, has attracted significant attention. A simultaneous metal to insulator transition, a sharp drop in the magnetic moment and a change in the electronic structure has been reported to occur below TMIT. It was suggested that the low-temperature phase is stabilized by a shift of the mixed valence Co3+/Co4+ toward pure Co3+, enabled by a valence change of Pr3+ to Pr4+. We present an atomic-scale study of (Pr1-yYy)0.7Ca0.3CoO3 using atomic-resolution imaging, electron energy-loss spectroscopy and in-situ cooling experiments in a scanning transmission electron microscope. The valence state transition in (Pr1-yYy)0.7Ca0.3CoO3 occurs at a transition temperature TMIT ~ 135K for y = 0.15 and the in-situ cooling experiments are conducted at 90 K. At room temperature, we find oxygen vacancy ordering associated with a Co valence state ordering and we will demonstrate that the electron transfer occurs from Pr to Co below the transition temperature. The oxygen vacancy ordering disappears as a result of the Co valence state transition. The effects of oxygen mobility, sample homogeneity and the impact on the observed transition will be discussed. This work is supported by a grant from the National Science Foundation (NSF-DMR1408427).

  5. Improved methods for high resolution electron microscopy

    SciTech Connect

    Taylor, J.R.

    1987-04-01

    Existing methods of making support films for high resolution transmission electron microscopy are investigated and novel methods are developed. Existing methods of fabricating fenestrated, metal reinforced specimen supports (microgrids) are evaluated for their potential to reduce beam induced movement of monolamellar crystals of C/sub 44/H/sub 90/ paraffin supported on thin carbon films. Improved methods of producing hydrophobic carbon films by vacuum evaporation, and improved methods of depositing well ordered monolamellar paraffin crystals on carbon films are developed. A novel technique for vacuum evaporation of metals is described which is used to reinforce microgrids. A technique is also developed to bond thin carbon films to microgrids with a polymer bonding agent. Unique biochemical methods are described to accomplish site specific covalent modification of membrane proteins. Protocols are given which covalently convert the carboxy terminus of papain cleaved bacteriorhodopsin to a free thiol. 53 refs., 19 figs., 1 tab.

  6. Improved methods for high resolution electron microscopy

    NASA Astrophysics Data System (ADS)

    Taylor, J. R.

    1987-04-01

    Existing methods of making support films for high resolution transmission electron microscopy are investigated and novel methods are developed. Existing methods of fabricating fenestrated, metal reinforced specimen supports (microgrids) are evaluated for their potential to reduce beam induced movement of monolamellar crystals of C44H90 paraffin supported on thin carbon films. Improved methods of producing hydrophobic carbon films by vacuum evaporation, and improved methods of depositing well ordered monolamellar paraffin crystals on carbon films are developed. A novel technique for vacuum evaporation of metals is described which is used to reinforce microgrids. A technique is also developed to bond thin carbon films to microgrids with a polymer bonding agent. Unique biochemical methods are described to accomplish site specific covalent modification of membrane proteins. Protocols are given which covalently convert the carboxy terminus of papain cleaved bacteriorhodopsin to a free thiol.

  7. High-resolution electron microscopy of advanced materials

    SciTech Connect

    Mitchell, T.E.; Kung, H.H.; Sickafus, K.E.; Gray, G.T. III; Field, R.D.; Smith, J.F.

    1997-11-01

    This final report chronicles a three-year, Laboratory Directed Research and Development (LDRD) project at Los Alamos National Laboratory (LANL). The High-Resolution Electron Microscopy Facility has doubled in size and tripled in quality since the beginning of the three-year period. The facility now includes a field-emission scanning electron microscope, a 100 kV field-emission scanning transmission electron microscope (FE-STEM), a 300 kV field-emission high-resolution transmission electron microscope (FE-HRTEM), and a 300 kV analytical transmission electron microscope. A new orientation imaging microscope is being installed. X-ray energy dispersive spectrometers for chemical analysis are available on all four microscopes; parallel electron energy loss spectrometers are operational on the FE-STEM and FE-HRTEM. These systems enable evaluation of local atomic bonding, as well as chemical composition in nanometer-scale regions. The FE-HRTEM has a point-to-point resolution of 1.6 {angstrom}, but the resolution can be pushed to its information limit of 1 {angstrom} by computer reconstruction of a focal series of images. HRTEM has been used to image the atomic structure of defects such as dislocations, grain boundaries, and interfaces in a variety of materials from superconductors and ferroelectrics to structural ceramics and intermetallics.

  8. Transmission Electron Microscope Measures Lattice Parameters

    NASA Technical Reports Server (NTRS)

    Pike, William T.

    1996-01-01

    Convergent-beam microdiffraction (CBM) in thermionic-emission transmission electron microscope (TEM) is technique for measuring lattice parameters of nanometer-sized specimens of crystalline materials. Lattice parameters determined by use of CBM accurate to within few parts in thousand. Technique developed especially for use in quantifying lattice parameters, and thus strains, in epitaxial mismatched-crystal-lattice multilayer structures in multiple-quantum-well and other advanced semiconductor electronic devices. Ability to determine strains in indivdual layers contributes to understanding of novel electronic behaviors of devices.

  9. Three-Dimensional Scanning Transmission Electron Microscopy of Biological Specimens

    PubMed Central

    de Jonge, Niels; Sougrat, Rachid; Northan, Brian M.; Pennycook, Stephen J.

    2010-01-01

    A three-dimensional (3D) reconstruction of the cytoskeleton and a clathrin-coated pit in mammalian cells has been achieved from a focal-series of images recorded in an aberration-corrected scanning transmission electron microscope (STEM). The specimen was a metallic replica of the biological structure comprising Pt nanoparticles 2–3 nm in diameter, with a high stability under electron beam radiation. The 3D dataset was processed by an automated deconvolution procedure. The lateral resolution was 1.1 nm, set by pixel size. Particles differing by only 10 nm in vertical position were identified as separate objects with greater than 20% dip in contrast between them. We refer to this value as the axial resolution of the deconvolution or reconstruction, the ability to recognize two objects, which were unresolved in the original dataset. The resolution of the reconstruction is comparable to that achieved by tilt-series transmission electron microscopy. However, the focal-series method does not require mechanical tilting and is therefore much faster. 3D STEM images were also recorded of the Golgi ribbon in conventional thin sections containing 3T3 cells with a comparable axial resolution in the deconvolved dataset. PMID:20082729

  10. Coherent Chromatic Effect in the Transmission Electron Microscope.

    PubMed

    Erni, Rolf

    2016-03-18

    Under the assumption of local atomic scattering, elastic electron scattering at finite scattering angles implies a small but finite energy loss. This energy loss, which under conventional imaging conditions in high-resolution transmission electron microscopy is of the order of 0.1 meV and thus negligible, increases by more than 2 orders of magnitude if light elements are investigated at sub-Ångström resolution. For a microscope of finite chromatic aberration, the energy loss leads to an element-specific chromatic effect which increases with the instrument resolution and with decreasing mass of the scattering atom. Despite that this effect is small, it can degrade the achievable image contrast. However, the effect can be considered in the optimization of the phase-contrast imaging conditions and even be beneficial to enhance the relative image contrast of light atoms in the presence of heavy atoms. PMID:27035311

  11. High-resolution transmission electron microscopy investigation of the face-centered cubic/hexagonal close-packed martensite transformation in Co-31.8 wt pct Ni alloy: Part 2. Plate intersections, extended defects, and nucleation mechanisms

    NASA Astrophysics Data System (ADS)

    Bray, D. W.; Howe, J. M.

    1996-11-01

    The face-centered cubic/hexagonal close-packed (fcc/hcp) martensite phase transformation in a Co-31.8 wt pct Ni alloy was studied by high-resolution transmission electron microscopy (HRTEM). The HRTEM was used to study the structure and properties of intersections between martensite plates and other defects observed in the alloy such as stacking fault tetrahedra (SFT) and Z-type defects. The HRTEM was also used to attempt to determine if various proposed mechanisms for the fcc/hcp martensite transformation were operating. There is evidence to suggest that the reflection mechanism proposed by Bollmann and the dipole mechanism proposed by Hirth are active in the fcc/hcp martensitic transformation, although the evidence is not completely certain in either case. Growth of the hcp phase by a four- or six-plane mechanism as proposed by Mahajan et al. is possible in theory but was not observed in this study. Transformation by previously proposed pole mechanisms was also not observed in this study, although evidence for a new type of pole mechanism was found. The formation of SFT along the fcc/hcp martensite interface was observed to occur by the cross-slip of Shockley partial dislocations out of the fcc/hcp interface onto conjugate fcc matrix planes, followed by further cross-slip to form the SFT, as previously observed for grain boundaries in fcc alloys.

  12. High resolution transmission electron microscopy of aluminophosphates

    SciTech Connect

    Ulan, J.G.; Gronsky, R. ); Szostak, R. ); Sorby, K. . Dept. of Chemistry)

    1990-04-01

    VPI-5 transforms to AlPO{sub 4}-8 under mild thermal treatment (100{degree}C, 18 hrs). HRTEM micrographs, oriented normal to the c axis, show extensive defect-free regions in VPI-5, while slip planes normal to the c axis are found in AlPO{sub 4}-8. Analysis of the HRTEM data, in conjunction with infrared and thermal analysis, adsorption studies and x-ray powder diffraction, has lead to a proposed structure for AlPO{sub 4}-8. Though the sheets containing the 18 member rings which define the pores in VPI-5 remain intact in AlPO{sub 4}-8, reduction in the porosity is attributed to blockages created by the movement of these sheets relative to each other. 8 refs., 7 figs.

  13. Concurrent in situ ion irradiation transmission electron microscope

    DOE PAGESBeta

    Hattar, K.; Bufford, D. C.; Buller, D. L.

    2014-08-29

    An in situ ion irradiation transmission electron microscope has been developed and is operational at Sandia National Laboratories. This facility permits high spatial resolution, real time observation of electron transparent samples under ion irradiation, implantation, mechanical loading, corrosive environments, and combinations thereof. This includes the simultaneous implantation of low-energy gas ions (0.8–30 keV) during high-energy heavy ion irradiation (0.8–48 MeV). In addition, initial results in polycrystalline gold foils are provided to demonstrate the range of capabilities.

  14. Imaging Nanobubbles in Water with Scanning Transmission Electron Microscopy

    NASA Astrophysics Data System (ADS)

    White, Edward R.; Mecklenburg, Matthew; Singer, Scott B.; Aloni, Shaul; Regan, Brian Christopher

    2011-05-01

    We present a technique based on scanning transmission electron microscopy (STEM) that is capable of probing nanobubble dynamics with nanometer spatial resolution. A vacuum-tight vessel holds a sub-micrometer layer of water between two electron-transparent dielectric membranes. Electrical current pulses passing through a platinum wire on one of the membranes inject sufficient heat locally to initiate single bubble formation. In the absence of power input, all bubbles are observed to be unstable against collapse, but the STEM beam alone can cause a shrinking bubble to grow.

  15. Transmission electron microscopy of mercury metal.

    PubMed

    Anjum, Dalaver H; Sougrat, Rachid

    2016-09-01

    Transmission electron microcopy (TEM) analysis of liquid metals, especially mercury (Hg), is difficult to carry out because their specimen preparation poses a daunting task due to the unique surface properties of these metals. This paper reports a cryoTEM study on Hg using a novel specimen preparation technique. Hg metal is mixed with water using sonication and quenched in liquid ethane cryogen. This technique permits research into the morphological, phase and structural properties of Hg at nanoscale dimensions. PMID:27018645

  16. 7 CFR 400.209 - Electronic transmission and receiving system.

    Code of Federal Regulations, 2012 CFR

    2012-01-01

    ... 7 Agriculture 6 2012-01-01 2012-01-01 false Electronic transmission and receiving system. 400.209... Contract-Standards for Approval § 400.209 Electronic transmission and receiving system. Any Contractor... Corporation approval of the electronic system as a condition to the electronic transmission and reception...

  17. 7 CFR 400.209 - Electronic transmission and receiving system.

    Code of Federal Regulations, 2013 CFR

    2013-01-01

    ... 7 Agriculture 6 2013-01-01 2013-01-01 false Electronic transmission and receiving system. 400.209... Contract-Standards for Approval § 400.209 Electronic transmission and receiving system. Any Contractor... Corporation approval of the electronic system as a condition to the electronic transmission and reception...

  18. 7 CFR 400.209 - Electronic transmission and receiving system.

    Code of Federal Regulations, 2014 CFR

    2014-01-01

    ... 7 Agriculture 6 2014-01-01 2014-01-01 false Electronic transmission and receiving system. 400.209... Contract-Standards for Approval § 400.209 Electronic transmission and receiving system. Any Contractor... Corporation approval of the electronic system as a condition to the electronic transmission and reception...

  19. Quantitative Scanning Transmission Electron Microscopy of Electronic and Nanostructured Materials

    NASA Astrophysics Data System (ADS)

    Yankovich, Andrew B.

    Electronic and nanostructured materials have been investigated using advanced scanning transmission electron microscopy (STEM) techniques. The first topic is the microstructure of Ga and Sb-doped ZnO. Ga-doped ZnO is a candidate transparent conducting oxide material. The microstructure of GZO thin films grown by MBE under different growth conditions and different substrates were examined using various electron microscopy (EM) techniques. The microstructure, prevalent defects, and polarity in these films strongly depend on the growth conditions and substrate. Sb-doped ZnO nanowires have been shown to be the first route to stable p-type ZnO. Using Z-contrast STEM, I have showed that an unusual microstructure of Sb-decorated head-to-head inversion domain boundaries and internal voids contain all the Sb in the nanowires and cause the p-type conduction. InGaN thin films and InGaN / GaN quantum wells (QW) for light emitting diodes are the second topic. Low-dose Z-contrast STEM, PACBED, and EDS on InGaN QW LED structures grown by MOCVD show no evidence for nanoscale composition variations, contradicting previous reports. In addition, a new extended defect in GaN and InGaN was discovered. The defect consists of a faceted pyramid-shaped void that produces a threading dislocation along the [0001] growth direction, and is likely caused by carbon contamination during growth. Non-rigid registration (NRR) and high-precision STEM of nanoparticles is the final topic. NRR is a new image processing technique that corrects distortions arising from the serial nature of STEM acquisition that previously limited the precision of locating atomic columns and counting the number of atoms in images. NRR was used to demonstrate sub-picometer precision in STEM images of single crystal Si and GaN, the best achieved in EM. NRR was used to measure the atomic surface structure of Pt nanoacatalysts and Au nanoparticles, which revealed new bond length variation phenomenon of surface atoms. In

  20. Insights into complexation of dissolved organic matter and Al(III) and nanominerals formation in soils under contrasting fertilizations using two-dimensional correlation spectroscopy and high resolution-transmission electron microscopy techniques.

    PubMed

    Wen, Yongli; Li, Huan; Xiao, Jian; Wang, Chang; Shen, Qirong; Ran, Wei; He, Xinhua; Zhou, Quansuo; Yu, Guanghui

    2014-09-01

    Understanding the organomineral associations in soils is of great importance. Using two-dimensional correlation spectroscopy (2DCOS) and high resolution-transmission electron microscopy (HRTEM) techniques, this study compared the binding characteristics of organic ligands to Al(III) in dissolved organic matter (DOM) from soils under short-term (3-years) and long-term (22-years) fertilizations. Three fertilization treatments were examined: (i) no fertilization (Control), (ii) chemical nitrogen, phosphorus and potassium (NPK), and (iii) NPK plus swine manure (NPKM). Soil spectra detected by the 2DCOS Fourier transform infrared (FTIR) spectroscopy showed that fertilization modified the binding characteristics of organic ligands to Al(III) in soil DOM at both short- and long- term location sites. The CH deformations in aliphatic groups played an important role in binding to Al(III) but with minor differences among the Control, NPK and NPKM at the short-term site. While at the long-term site both C-O stretching of polysaccharides or polysaccharide-like substances and aliphatic O-H were bound to Al(III) under the Control, whereas only aliphatic O-H, and only polysaccharides and silicates, were bound to Al(III) under NPK and NPKM, respectively. Images from HRTEM demonstrated that crystalline nanominerals, composed of Fe and O, were predominant in soil DOM under NPK, while amorphous nanominerals, predominant in Al, Si, and O, were dominant in soil DOM under Control and NPKM. In conclusion, fertilization strategies, especially under long-term, could affect the binding of organic ligands to Al(III) in soil DOM, which resulted in alterations in the turnover, reactivity, and bioavailability of soil organic matter. Our results demonstrated that the FTIR-2DCOS combined with HRTEM techniques could enhance our understanding in the binding characteristics of DOM to Al(III) and the resulted nanominerals in soils. PMID:24997950

  1. Transmission Electron Microscopy of Itokawa Regolith Grains

    NASA Technical Reports Server (NTRS)

    Keller, Lindsay P.; Berger, E. L.

    2013-01-01

    Introduction: In a remarkable engineering achievement, the JAXA space agency successfully recovered the Hayabusa space-craft in June 2010, following a non-optimal encounter and sur-face sampling mission to asteroid 25143 Itokawa. These are the first direct samples ever obtained and returned from the surface of an asteroid. The Hayabusa samples thus present a special op-portunity to directly investigate the evolution of asteroidal sur-faces, from the development of the regolith to the study of the effects of space weathering. Here we report on our preliminary TEM measurements on two Itokawa samples. Methods: We were allocated particles RA-QD02-0125 and RA-QD02-0211. Both particles were embedded in low viscosity epoxy and thin sections were prepared using ultramicrotomy. High resolution images and electron diffraction data were ob-tained using a JEOL 2500SE 200 kV field-emission scanning-transmission electron microscope. Quantitative maps and anal-yses were obtained using a Thermo thin-window energy-dispersive x-ray (EDX) spectrometer. Results: Both particles are olivine-rich (Fo70) with µm-sized inclusions of FeS and have microstructurally complex rims. Par-ticle RA-QD02-0125 is rounded and has numerous sub-µm grains attached to its surface including FeS, albite, olivine, and rare melt droplets. Solar flare tracks have not been observed, but the particle is surrounded by a continuous 50 nm thick, stuctur-ally disordered rim that is compositionally similar to the core of the grain. One of the surface adhering grains is pyrrhotite show-ing a S-depleted rim (8-10 nm thick) with nanophase Fe metal grains (<5 nm) decorating the outermost surface. The pyrrhotite displays a complex superstructure in its core that is absent in the S-depleted rim. Particle RA-QD02-0211 contains solar flare particle tracks (2x109 cm-2) and shows a structurally disordered rim 100 nm thick. The track density corresponds to a surface exposure of 103-104 years based on the track production rate

  2. Resolution measures in molecular electron microscopy

    PubMed Central

    Penczek, Pawel A.

    2011-01-01

    Resolution measures in molecular electron microscopy provide means to evaluate quality of macromolecular structures computed from sets of their two-dimensional line projections. When the amount of detail in the computed density map is low there are no external standards by which the resolution of the result can be judged. Instead, resolution measures in molecular electron microscopy evaluate consistency of the results in reciprocal space and present it as a one-dimensional function of the modulus of spatial frequency. Here we provide description of standard resolution measures commonly used in electron microscopy. We point out that the organizing principle is the relationship between these measures and the Spectral Signal-to-Noise Ratio of the computed density map. Within this framework it becomes straightforward to describe the connection between the outcome of resolution evaluations and the quality of electron microscopy maps, in particular, the optimum filtration, in the Wiener sense, of the computed map. We also provide a discussion of practical difficulties of evaluation of resolution in electron microscopy, particularly in terms of its sensitivity to data processing operations used during structure determination process in single particle analysis and in electron tomography. PMID:20888958

  3. Atomic Resolution Imaging with a sub-50 pm Electron Probe

    SciTech Connect

    Erni, Rolf P.; Rossell, Marta D.; Kisielowski, Christian; Dahmen, Ulrich

    2009-03-02

    Using a highly coherent focused electron probe in a 5th order aberration-corrected transmission electron microscope, we report on resolving a crystal spacing less than 50 pm. Based on the geometrical source size and residual coherent and incoherent axial lens aberrations, an electron probe is calculated, which is theoretically capable of resolving an ideal 47 pm spacing with 29percent contrast. Our experimental data show the 47 pm spacing of a Ge 114 crystal imaged with 11-18percent contrast at a 60-95percent confidence level, providing the first direct evidence for sub 50-pm resolution in ADF STEM imaging.

  4. Quantitative characterization of electron detectors for transmission electron microscopy

    PubMed Central

    Ruskin, Rachel S.; Yu, Zhiheng; Grigorieff, Nikolaus

    2013-01-01

    A new generation of direct electron detectors for transmission electron microscopy (TEM) promises significant improvement over previous detectors in terms of their modulation transfer function (MTF) and detective quantum efficiency (DQE). However, the performance of these new detectors needs to be carefully monitored in order to optimize imaging conditions and check for degradation over time. We have developed an easy-to-use software tool, FindDQE, to measure MTF and DQE of electron detectors using images of a microscope’s built-in beam stop. Using this software, we have determined the DQE curves of four direct electron detectors currently available: the Gatan K2 Summit, the FEI Falcon I and II, and the Direct Electron DE-12, under a variety of total dose and dose rate conditions. We have additionally measured the curves for the Gatan US4000 and TVIPS F416 scintillator-based cameras. We compare the results from our new method with published curves. PMID:24189638

  5. Transmission electron microscopy of undermined passive films on stainless steel

    SciTech Connect

    Isaacs, H.S.; Zhu, Y.; Sabatini, R.L.; Ryan, M.P.

    1999-06-01

    A study has been made of the passive film remaining over pits on stainless steel using a high resolution transmission electron microscope. Type 305 stainless steel was passivated in a borate buffer solution and pitted in ferric chloride. Passive films formed at 0.2 V relative to a saturated calomel electrode were found to be amorphous. Films formed at higher potentials showed only broad diffraction rings. The passive film was found to cover a remnant lacy structure formed over pits passivated at 0.8 V. The metallic strands of the lace were roughly hemitubular in shape with the curved surface facing the center of the pit.

  6. Nonlinear transmission line based electron beam driver.

    PubMed

    French, David M; Hoff, Brad W; Tang, Wilkin; Heidger, Susan; Allen-Flowers, Jordan; Shiffler, Don

    2012-12-01

    Gated field emission cathodes can provide short electron pulses without the requirement of laser systems or cathode heating required by photoemission or thermionic cathodes. The large electric field requirement for field emission to take place can be achieved by using a high aspect ratio cathode with a large field enhancement factor which reduces the voltage requirement for emission. In this paper, a cathode gate driver based on the output pulse train from a nonlinear transmission line is experimentally demonstrated. The application of the pulse train to a tufted carbon fiber field emission cathode generates short electron pulses. The pulses are approximately 2 ns in duration with emission currents of several mA, and the train contains up to 6 pulses at a frequency of 100 MHz. Particle-in-cell simulation is used to predict the characteristic of the current pulse train generated from a single carbon fiber field emission cathode using the same technique. PMID:23277977

  7. Nonlinear transmission line based electron beam driver

    NASA Astrophysics Data System (ADS)

    French, David M.; Hoff, Brad W.; Tang, Wilkin; Heidger, Susan; Allen-Flowers, Jordan; Shiffler, Don

    2012-12-01

    Gated field emission cathodes can provide short electron pulses without the requirement of laser systems or cathode heating required by photoemission or thermionic cathodes. The large electric field requirement for field emission to take place can be achieved by using a high aspect ratio cathode with a large field enhancement factor which reduces the voltage requirement for emission. In this paper, a cathode gate driver based on the output pulse train from a nonlinear transmission line is experimentally demonstrated. The application of the pulse train to a tufted carbon fiber field emission cathode generates short electron pulses. The pulses are approximately 2 ns in duration with emission currents of several mA, and the train contains up to 6 pulses at a frequency of 100 MHz. Particle-in-cell simulation is used to predict the characteristic of the current pulse train generated from a single carbon fiber field emission cathode using the same technique.

  8. Nonlinear transmission line based electron beam driver

    SciTech Connect

    French, David M.; Hoff, Brad W.; Tang Wilkin; Heidger, Susan; Shiffler, Don; Allen-Flowers, Jordan

    2012-12-15

    Gated field emission cathodes can provide short electron pulses without the requirement of laser systems or cathode heating required by photoemission or thermionic cathodes. The large electric field requirement for field emission to take place can be achieved by using a high aspect ratio cathode with a large field enhancement factor which reduces the voltage requirement for emission. In this paper, a cathode gate driver based on the output pulse train from a nonlinear transmission line is experimentally demonstrated. The application of the pulse train to a tufted carbon fiber field emission cathode generates short electron pulses. The pulses are approximately 2 ns in duration with emission currents of several mA, and the train contains up to 6 pulses at a frequency of 100 MHz. Particle-in-cell simulation is used to predict the characteristic of the current pulse train generated from a single carbon fiber field emission cathode using the same technique.

  9. Pushing the envelope of in situ transmission electron microscopy.

    PubMed

    Ramachandramoorthy, Rajaprakash; Bernal, Rodrigo; Espinosa, Horacio D

    2015-05-26

    Recent major improvements to the transmission electron microscope (TEM) including aberration-corrected electron optics, light-element-sensitive analytical instrumentation, sample environmental control, and high-speed and sensitive direct electron detectors are becoming more widely available. When these advances are combined with in situ TEM tools, such as multimodal testing based on microelectromechanical systems, key measurements and insights on nanoscale material phenomena become possible. In particular, these advances enable metrology that allows for unprecedented correlation to quantum mechanics and the predictions of atomistic models. In this Perspective, we provide a summary of recent in situ TEM research that has leveraged these new TEM capabilities as well as an outlook of the opportunities that exist in the different areas of in situ TEM experimentation. Although these advances have improved the spatial and temporal resolution of TEM, a critical analysis of the various in situ TEM fields reveals that further progress is needed to achieve the full potential of the technology. PMID:25942405

  10. Time Resolved Phase Transitions via Dynamic Transmission Electron Microscopy

    SciTech Connect

    Reed, B W; Armstrong, M R; Blobaum, K J; Browning, N D; Burnham, A K; Campbell, G H; Gee, R; Kim, J S; King, W E; Maiti, A; Piggott, W T; Torralva, B R

    2007-02-22

    The Dynamic Transmission Electron Microscope (DTEM) project is developing an in situ electron microscope with nanometer- and nanosecond-scale resolution for the study of rapid laser-driven processes in materials. We report on the results obtained in a year-long LDRD-supported effort to develop DTEM techniques and results for phase transitions in molecular crystals, reactive multilayer foils, and melting and resolidification of bismuth. We report the first in situ TEM observation of the HMX {beta}-{delta} phase transformation in sub-{micro}m crystals, computational results suggesting the importance of voids and free surfaces in the HMX transformation kinetics, and the first electron diffraction patterns of intermediate states in fast multilayer foil reactions. This project developed techniques which are applicable to many materials systems and will continue to be employed within the larger DTEM effort.

  11. Pulsed Power for a Dynamic Transmission Electron Microscope

    SciTech Connect

    dehope, w j; browning, n; campbell, g; cook, e; king, w; lagrange, t; reed, b; stuart, b; Shuttlesworth, R; Pyke, B

    2009-06-25

    Lawrence Livermore National Laboratory (LLNL) has converted a commercial 200kV transmission electron microscope (TEM) into an ultrafast, nanoscale diagnostic tool for material science studies. The resulting Dynamic Transmission Electron Microscope (DTEM) has provided a unique tool for the study of material phase transitions, reaction front analyses, and other studies in the fields of chemistry, materials science, and biology. The TEM's thermionic electron emission source was replaced with a fast photocathode and a laser beam path was provided for ultraviolet surface illumination. The resulting photoelectron beam gives downstream images of 2 and 20 ns exposure times at 100 and 10 nm spatial resolution. A separate laser, used as a pump pulse, is used to heat, ignite, or shock samples while the photocathode electron pulses, carefully time-synchronized with the pump, function as probe in fast transient studies. The device functions in both imaging and diffraction modes. A laser upgrade is underway to make arbitrary cathode pulse trains of variable pulse width of 10-1000 ns. Along with a fast e-beam deflection scheme, a 'movie mode' capability will be added to this unique diagnostic tool. This talk will review conventional electron microscopy and its limitations, discuss the development and capabilities of DTEM, in particularly addressing the prime and pulsed power considerations in the design and fabrication of the DTEM, and conclude with the presentation of a deflector and solid-state pulser design for Movie-Mode DTEM.

  12. Photocathode Optimization for a Dynamic Transmission Electron Microscope: Final Report

    SciTech Connect

    Ellis, P; Flom, Z; Heinselman, K; Nguyen, T; Tung, S; Haskell, R; Reed, B W; LaGrange, T

    2011-08-04

    The Dynamic Transmission Electron Microscope (DTEM) team at Harvey Mudd College has been sponsored by LLNL to design and build a test setup for optimizing the performance of the DTEM's electron source. Unlike a traditional TEM, the DTEM achieves much faster exposure times by using photoemission from a photocathode to produce electrons for imaging. The DTEM team's work is motivated by the need to improve the coherence and current density of the electron cloud produced by the electron gun in order to increase the image resolution and contrast achievable by DTEM. The photoemission test setup is nearly complete and the team will soon complete baseline tests of electron gun performance. The photoemission laser and high voltage power supply have been repaired; the optics path for relaying the laser to the photocathode has been finalized, assembled, and aligned; the internal setup of the vacuum chamber has been finalized and mostly implemented; and system control, synchronization, and data acquisition has been implemented in LabVIEW. Immediate future work includes determining a consistent alignment procedure to place the laser waist on the photocathode, and taking baseline performance measurements of the tantalum photocathode. Future research will examine the performance of the electron gun as a function of the photoemission laser profile, the photocathode material, and the geometry and voltages of the accelerating and focusing components in the electron gun. This report presents the team's progress and outlines the work that remains.

  13. Thin dielectric film thickness determination by advanced transmission electron microscopy

    SciTech Connect

    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.

  14. Phase contrast in high resolution electron microscopy

    DOEpatents

    Rose, H.H.

    1975-09-23

    This patent relates to a device for developing a phase contrast signal for a scanning transmission electron microscope. The lens system of the microscope is operated in a condition of defocus so that predictable alternate concentric regions of high and low electron density exist in the cone of illumination. Two phase detectors are placed beneath the object inside the cone of illumination, with the first detector having the form of a zone plate, each of its rings covering alternate regions of either higher or lower electron density. The second detector is so configured that it covers the regions of electron density not covered by the first detector. Each detector measures the number of electrons incident thereon and the signal developed by the first detector is subtracted from the signal developed by the record detector to provide a phase contrast signal. (auth)

  15. Combined Scanning Transmission Electron Microscopy Tilt- and Focal Series

    SciTech Connect

    Dahmen, Tim; Baudoin, Jean-Pierre G; Lupini, Andrew R; Kubel, Christian; Slusallek, Phillip; De Jonge, Niels

    2014-01-01

    In this study, a combined tilt- and focal series is proposed as a new recording scheme for high-angle annular dark-field scanning transmission electron microscopy (STEM) tomography. Three-dimensional (3D) data were acquired by mechanically tilting the specimen, and recording a through-focal series at each tilt direction. The sample was a whole-mount macrophage cell with embedded gold nanoparticles. The tilt focal algebraic reconstruction technique (TF-ART) is introduced as a new algorithm to reconstruct tomograms from such combined tilt- and focal series. The feasibility of TF-ART was demonstrated by 3D reconstruction of the experimental 3D data. The results were compared with a conventional STEM tilt series of a similar sample. The combined tilt- and focal series led to smaller missing wedge artifacts, and a higher axial resolution than obtained for the STEM tilt series, thus improving on one of the main issues of tilt series-based electron tomography.

  16. ELECTRONICS UPGRADE OF HIGH RESOLUTION MASS SPECTROMETERS

    SciTech Connect

    Mcintosh, J; Joe Cordaro, J

    2008-03-10

    High resolution mass spectrometers are specialized systems that allow researchers to determine the exact mass of samples to four significant digits by using magnetic and electronic sector mass analyzers. Many of the systems in use today at research laboratories and universities were designed and built more than two decades ago. The manufacturers of these systems have abandoned the support for some of the mass spectrometers and parts to power and control them have become scarce or obsolete. The Savannah River National Laboratory has been involved in the upgrade of the electronics and software for these legacy machines. The Electronics Upgrade of High Resolution Mass Spectrometers consists of assembling high-end commercial instrumentation from reputable manufacturers with a minimal amount of customization to replace the electronics for the older systems. By taking advantage of advances in instrumentation, precise magnet control can be achieved using high resolution current sources and continuous feedback from a high resolution hall-effect probe. The custom equipment include a precision voltage divider/summing amplifier chassis, high voltage power supply chassis and a chassis for controlling the voltage emission for the mass spectrometer source tube. The upgrade package is versatile enough to interface with valve control, vacuum and other instrumentation. Instrument communication is via a combination of Ethernet and traditional IEEE-488 GPIB protocols. The system software upgrades include precision control, feedback and spectral waveform analysis tools.

  17. High resolution electron crystallography of protein molecules

    SciTech Connect

    Glaeser, R.M. |; Downing, K.H.

    1993-06-01

    Electron diffraction data and high resolution images can now be used to obtain accurate, three-dimensional density maps of biological macromolecules. These density maps can be interpreted by building an atomic-resolution model of the structure into the experimental density. The Cowley-Moodie formalism of dynamical diffraction theory has been used to validate the use of kinematic diffraction theory, strictly the weak phase object approximation, in producing such 3-D density maps. Further improvements in the preparation of very flat specimens and in the retention of diffraction to a resolution of 0.2 nm or better could result in electron crystallography becoming as important a technique as x-ray crystallography currently is for the field of structural molecular biology.

  18. Quantitative characterization of electron detectors for transmission electron microscopy.

    PubMed

    Ruskin, Rachel S; Yu, Zhiheng; Grigorieff, Nikolaus

    2013-12-01

    A new generation of direct electron detectors for transmission electron microscopy (TEM) promises significant improvement over previous detectors in terms of their modulation transfer function (MTF) and detective quantum efficiency (DQE). However, the performance of these new detectors needs to be carefully monitored in order to optimize imaging conditions and check for degradation over time. We have developed an easy-to-use software tool, FindDQE, to measure MTF and DQE of electron detectors using images of a microscope's built-in beam stop. Using this software, we have determined the DQE curves of four direct electron detectors currently available: the Gatan K2 Summit, the FEI Falcon I and II, and the Direct Electron DE-12, under a variety of total dose and dose rate conditions. We have additionally measured the curves for the Gatan US4000 and TVIPS TemCam-F416 scintillator-based cameras. We compare the results from our new method with published curves. PMID:24189638

  19. Structural Fingerprinting of Nanocrystals in the Transmission Electron Microscope

    NASA Astrophysics Data System (ADS)

    Rouvimov, Sergei; Plachinda, Pavel; Moeck, Peter

    2010-03-01

    Three novel strategies for the structurally identification of nanocrystals in a transmission electron microscope are presented. Either a single high-resolution transmission electron microscopy image [1] or a single precession electron diffractogram (PED) [2] may be employed. PEDs from fine-grained crystal powders may also be utilized. Automation of the former two strategies is in progress and shall lead to statistically significant results on ensembles of nanocrystals. Open-access databases such as the Crystallography Open Database which provides more than 81,500 crystal structure data sets [3] or its mainly inorganic and educational subsets [4] may be utilized. [1] http://www.scientificjournals.org/journals 2007/j/of/dissertation.htm [2] P. Moeck and S. Rouvimov, in: {Drugs and the Pharmaceutical Sciences}, Vol. 191, 2009, 270-313 [3] http://cod.ibt.lt, http://www.crystallography.net, http://cod.ensicaen.fr, http://nanocrystallography.org, http://nanocrystallography.net, http://journals.iucr.org/j/issues/2009/04/00/kk5039/kk5039.pdf [4] http://nanocrystallography.research.pdx.edu/CIF-searchable

  20. 7 CFR 400.209 - Electronic transmission and receiving system.

    Code of Federal Regulations, 2011 CFR

    2011-01-01

    ... 7 Agriculture 6 2011-01-01 2011-01-01 false Electronic transmission and receiving system. 400.209... Contract-Standards for Approval § 400.209 Electronic transmission and receiving system. Any Contractor...; (b) Maintain an electronic system which must be tested and approved by the Corporation; (c)...

  1. Scanning transmission electron microscopy strain measurement from millisecond frames of a direct electron charge coupled device

    SciTech Connect

    Mueller, Knut; Rosenauer, Andreas; Ryll, Henning; Ordavo, Ivan; Ihle, Sebastian; Soltau, Heike; Strueder, Lothar; Volz, Kerstin; Zweck, Josef

    2012-11-19

    A high-speed direct electron detection system is introduced to the field of transmission electron microscopy and applied to strain measurements in semiconductor nanostructures. In particular, a focused electron probe with a diameter of 0.5 nm was scanned over a fourfold quantum layer stack with alternating compressive and tensile strain and diffracted discs have been recorded on a scintillator-free direct electron detector with a frame time of 1 ms. We show that the applied algorithms can accurately detect Bragg beam positions despite a significant point spread each 300 kV electron causes during detection on the scintillator-free camera. For millisecond exposures, we find that strain can be measured with a precision of 1.3 Multiplication-Sign 10{sup -3}, enabling, e.g., strain mapping in a 100 Multiplication-Sign 100 nm{sup 2} region with 0.5 nm resolution in 40 s.

  2. Computer synthesis of high resolution electron micrographs

    NASA Technical Reports Server (NTRS)

    Nathan, R.

    1976-01-01

    Specimen damage, spherical aberration, low contrast and noisy sensors combine to prevent direct atomic viewing in a conventional electron microscope. The paper describes two methods for obtaining ultra-high resolution in biological specimens under the electron microscope. The first method assumes the physical limits of the electron objective lens and uses a series of dark field images of biological crystals to obtain direct information on the phases of the Fourier diffraction maxima; this information is used in an appropriate computer to synthesize a large aperture lens for a 1-A resolution. The second method assumes there is sufficient amplitude scatter from images recorded in focus which can be utilized with a sensitive densitometer and computer contrast stretching to yield fine structure image details. Cancer virus characterization is discussed as an illustrative example. Numerous photographs supplement the text.

  3. Nanoscale 3D cellular imaging by axial scanning transmission electron tomography

    PubMed Central

    Hohmann-Marriott, Martin F.; Sousa, Alioscka A.; Azari, Afrouz A.; Glushakova, Svetlana; Zhang, Guofeng; Zimmerberg, Joshua; Leapman, Richard D.

    2009-01-01

    Electron tomography provides three-dimensional structural information about supramolecular assemblies and organelles in a cellular context but image degradation, caused by scattering of transmitted electrons, limits applicability in specimens thicker than 300 nm. We show that scanning transmission electron tomography of 1000 nm thick samples using axial detection provides resolution comparable to conventional electron tomography. The method is demonstrated by reconstructing a human erythrocyte infected with the malaria parasite Plasmodium falciparum. PMID:19718033

  4. Data processing for atomic resolution electron energy loss spectroscopy.

    PubMed

    Cueva, Paul; Hovden, Robert; Mundy, Julia A; Xin, Huolin L; Muller, David A

    2012-08-01

    The high beam current and subangstrom resolution of aberration-corrected scanning transmission electron microscopes has enabled electron energy loss spectroscopy (EELS) mapping with atomic resolution. These spectral maps are often dose limited and spatially oversampled, leading to low counts/channel and are thus highly sensitive to errors in background estimation. However, by taking advantage of redundancy in the dataset map, one can improve background estimation and increase chemical sensitivity. We consider two such approaches--linear combination of power laws and local background averaging--that reduce background error and improve signal extraction. Principal component analysis (PCA) can also be used to analyze spectrum images, but the poor peak-to-background ratio in EELS can lead to serious artifacts if raw EELS data are PCA filtered. We identify common artifacts and discuss alternative approaches. These algorithms are implemented within the Cornell Spectrum Imager, an open source software package for spectroscopic analysis. PMID:22697429

  5. Electron microscopy of gold nanoparticles at atomic resolution

    PubMed Central

    Azubel, Maia; Koivisto, Jaakko; Malola, Sami; Bushnell, David; Hura, Greg L.; Koh, Ai Leen; Tsunoyama, Hironori; Tsukuda, Tatsuya; Pettersson, Mika; Häkkinen, Hannu; Kornberg, Roger D.

    2014-01-01

    Structure determination of gold nanoparticles (AuNPs) is necessary for understanding their physical and chemical properties, and only one AuNP larger than 1 nm in diameter, an Au102NP, has been solved to atomic resolution. Whereas the Au102NP structure was determined by X-ray crystallography, other large AuNPs have proved refractory to this approach. Here we report the structure determination of an Au68NP at atomic resolution by aberration-corrected transmission electron microscopy (AC-TEM), performed with the use of a minimal electron dose, an approach that should prove applicable to metal NPs in general. The structure of the Au68NP was supported by small angle X-ray scattering (SAXS) and by comparison of observed infrared (IR) absorption spectra with calculations by density functional theory (DFT). PMID:25146285

  6. Observations of Nanobubble Dynamics with Transmission Electron Microscopy

    NASA Astrophysics Data System (ADS)

    Mohan, Meera Kanakamma; Arora, Manish; Mirsaidov, Utkur; Ohl, Claus-Dieter

    2013-11-01

    Recent developments in transmission electron microscopy (TEM) allow the imaging of liquids with high spatial resolution. Here we report on novel studies of water trapped between two monolayers of graphene sheets. The geometry prevents evaporation of the liquid into the low pressure environment of the TEM while providing excellent electron-optical properties for investigations. The graphene sheets are supported by a conventional TEM grid. We report on the nucleation of bubbles, the coalescence between neighbouring bubbles, rupture of thin liquid filaments, and their slow shrinkage. At a dose rate of 100-155 e-Å-2s-1 these events are observed conveniently at video frame rate. The correlation with the local electron beam dose rate suggests that the radiolysis induced by the electron beam is the main driving force for most events. In general, we observed bubbles with lateral sizes between 20 nm and 100 nm and estimated heights between 6 nm and 30 nm. Likely, the bubbles connect both graphene sheets. In the absence of the electron beam the nanobubbles do not dissolve completely but surprisingly remain stable for even up to one hour. This resembles the stability of surface attached nanobubbles.

  7. Bragg reflection transmission filters for variable resolution monochromators

    SciTech Connect

    Chapman, D. )

    1989-01-01

    There are various methods for improving the angular and spectral resolution of monochromator and analyzer systems. The novel system described here, though limited to higher x-ray energies (>20keV), is based on a dynamical effect occurring on the transmitted beam with a thin perfect crystal plate set in the Bragg reflection case. In the case of Bragg reflection from a perfect crystal, the incident beam is rapidly attenuated as it penetrates the crystal in the range of reflection. This extinction length is of the order of microns. The attenuation length, which determines the amount of normal transmission through the plate is generally much longer. Thus, in the range of the Bragg reflection the attenuation of the transmitted beam can change by several orders of magnitude with a small change in energy or angle. This thin crystal plate cuts a notch in the transmitted beam with a width equal to its Darwin width, thus acting as a transmission filter. When used in a non-dispersive mode with other monochromator crystals, the filter when set at the Bragg angle will reflect the entire Darwin width of the incident beam and transmit the wings of the incident beam distribution. When the element is offset in angle by some fraction of the Darwin width, the filter becomes useful in adjusting the angular width of the transmitted beam and removing a wing. Used in pairs with a symmetric offset, the filters can be used to continuously adjust the intrinsic angular divergence of the beam with good wing reduction. Instances where such filters may be useful are in improving the angular resolution of a small angle scattering camera. These filters may be added to a Bonse-Hart camera with one pair on the incident beam to reduce the intrinsic beam divergence and a second pair on the analyzer arm to improve the analyzer resolution. 2 refs., 3 Figs.

  8. Electron-optic limitations on image resolution

    NASA Technical Reports Server (NTRS)

    Engstrom, R. W.

    1973-01-01

    Various approaches are considered to the solution of the electron-optical problem of designing an image tube configuration. Emphasis is placed on the method of computer design, and an illustration is given in which the technique is used in the design of an 80-mm image tube with a zoom capability of 3:1. The solutions are discussed to such problems as image distortion, magnification, and electron bundles striking the zoom electrode. Three types of an electron-optical configuration are examined for the electron-optic limitations to resolution: (1) the proximity image tube, (2) the magnetic-type image tube having uniform electric and magnetic fields, and (3) the electrostatic-type image tube such as the 80-mm zoom tube.

  9. Development of wavelength-dispersive soft X-ray emission spectrometers for transmission electron microscopes--an introduction of valence electron spectroscopy for transmission electron microscopy.

    PubMed

    Terauchi, Masami; Koike, Masato; Fukushima, Kurio; Kimura, Atsushi

    2010-01-01

    Two types of wavelength-dispersive soft X-ray spectrometers, a high-dispersion type and a conventional one, for transmission electron microscopes were constructed. Those spectrometers were used to study the electronic states of valence electrons (bonding electrons). Both spectrometers extended the acceptable energy regions to higher than 2000 eV. The best energy resolution of 0.08 eV was obtained for an Al L-emission spectrum by using the high-dispersion type spectrometer. By using the spectrometer, C K-emission of carbon allotropes, Cu L-emission of Cu(1-x)Zn(x) alloys and Pt M-emission spectra were presented. The FWHM value of 12 eV was obtained for the Pt Malpha-emission peak. The performance of the conventional one was also presented for ZnS and a section specimen of a multilayer device. W-M and Si-K emissions were clearly resolved. Soft X-ray emission spectroscopy based on transmission electron microscopy (TEM) has an advantage for obtaining spectra from a single crystalline specimen with a defined crystal setting. As an example of anisotropic soft X-ray emission, C K-emission spectra of single crystalline graphite with different crystal settings were presented. From the spectra, density of states of pi- and sigma-bondings were separately derived. These results demonstrated a method to analyse the electronic states of valence electrons of materials in the nanometre scale based on TEM. PMID:20371492

  10. Resolution and quantitative accuracy improvements in ultrasound transmission imaging

    NASA Astrophysics Data System (ADS)

    Chenevert, T. L.

    The type of ultrasound transmission imaging, referred to as ultrasonic computed tomography (UCT), reconstructs distributions of tissue speed of sound and sound attenuation properties from measurements of acoustic pulse time of flight (TCF) and energy received through tissue. Although clinical studies with experimental UCT scanners have demonstrated UCT is sensitive to certain tissue pathologies not easily detected with conventional ultrasound imaging, they have also shown UCT to suffer from artifacts due to physical differences between the acoustic beam and its ray model implicit in image reconstruction algorithms. Artifacts are expressed as large quantitative errors in attenuation images, and poor spatial resolution and size distortion (exaggerated size of high speed of sound regions) in speed of sound images. Methods are introduced and investigated which alleviate these problems in UCT imaging by providing improved measurements of pulse TCF and energy.

  11. [Multiple transmission electron microscopic image stitching based on sift features].

    PubMed

    Li, Mu; Lu, Yanmeng; Han, Shuaihu; Wu, Zhuobin; Chen, Jiajing; Liu, Zhexing; Cao, Lei

    2015-08-01

    We proposed a new stitching method based on sift features to obtain an enlarged view of transmission electron microscopic (TEM) images with a high resolution. The sift features were extracted from the images, which were then combined with fitted polynomial correction field to correct the images, followed by image alignment based on the sift features. The image seams at the junction were finally removed by Poisson image editing to achieve seamless stitching, which was validated on 60 local glomerular TEM images with an image alignment error of 62.5 to 187.5 nm. Compared with 3 other stitching methods, the proposed method could effectively reduce image deformation and avoid artifacts to facilitate renal biopsy pathological diagnosis. PMID:26403733

  12. Nanomaterial datasets to advance tomography in scanning transmission electron microscopy

    PubMed Central

    Levin, Barnaby D.A.; Padgett, Elliot; Chen, Chien-Chun; Scott, M.C.; Xu, Rui; Theis, Wolfgang; Jiang, Yi; Yang, Yongsoo; Ophus, Colin; Zhang, Haitao; Ha, Don-Hyung; Wang, Deli; Yu, Yingchao; Abruña, Hector D.; Robinson, Richard D.; Ercius, Peter; Kourkoutis, Lena F.; Miao, Jianwei; Muller, David A.; Hovden, Robert

    2016-01-01

    Electron tomography in materials science has flourished with the demand to characterize nanoscale materials in three dimensions (3D). Access to experimental data is vital for developing and validating reconstruction methods that improve resolution and reduce radiation dose requirements. This work presents five high-quality scanning transmission electron microscope (STEM) tomography datasets in order to address the critical need for open access data in this field. The datasets represent the current limits of experimental technique, are of high quality, and contain materials with structural complexity. Included are tomographic series of a hyperbranched Co2P nanocrystal, platinum nanoparticles on a carbon nanofibre imaged over the complete 180° tilt range, a platinum nanoparticle and a tungsten needle both imaged at atomic resolution by equal slope tomography, and a through-focal tilt series of PtCu nanoparticles. A volumetric reconstruction from every dataset is provided for comparison and development of post-processing and visualization techniques. Researchers interested in creating novel data processing and reconstruction algorithms will now have access to state of the art experimental test data. PMID:27272459

  13. Nanomaterial datasets to advance tomography in scanning transmission electron microscopy.

    PubMed

    Levin, Barnaby D A; Padgett, Elliot; Chen, Chien-Chun; Scott, M C; Xu, Rui; Theis, Wolfgang; Jiang, Yi; Yang, Yongsoo; Ophus, Colin; Zhang, Haitao; Ha, Don-Hyung; Wang, Deli; Yu, Yingchao; Abruña, Hector D; Robinson, Richard D; Ercius, Peter; Kourkoutis, Lena F; Miao, Jianwei; Muller, David A; Hovden, Robert

    2016-01-01

    Electron tomography in materials science has flourished with the demand to characterize nanoscale materials in three dimensions (3D). Access to experimental data is vital for developing and validating reconstruction methods that improve resolution and reduce radiation dose requirements. This work presents five high-quality scanning transmission electron microscope (STEM) tomography datasets in order to address the critical need for open access data in this field. The datasets represent the current limits of experimental technique, are of high quality, and contain materials with structural complexity. Included are tomographic series of a hyperbranched Co2P nanocrystal, platinum nanoparticles on a carbon nanofibre imaged over the complete 180° tilt range, a platinum nanoparticle and a tungsten needle both imaged at atomic resolution by equal slope tomography, and a through-focal tilt series of PtCu nanoparticles. A volumetric reconstruction from every dataset is provided for comparison and development of post-processing and visualization techniques. Researchers interested in creating novel data processing and reconstruction algorithms will now have access to state of the art experimental test data. PMID:27272459

  14. 7 CFR 400.209 - Electronic transmission and receiving system.

    Code of Federal Regulations, 2010 CFR

    2010-01-01

    ... Contract-Standards for Approval § 400.209 Electronic transmission and receiving system. Any Contractor under the Contract is required to: (a) Adopt a plan for the purpose of transmitting and receiving... 7 Agriculture 6 2010-01-01 2010-01-01 false Electronic transmission and receiving system....

  15. Transmission Kikuchi diffraction and transmission electron forescatter imaging of electropolished and FIB manufactured TEM specimens

    SciTech Connect

    Zieliński, W. Płociński, T.; Kurzydłowski, K.J.

    2015-06-15

    We present a study of the efficiency of the utility of scanning electron microscope (SEM)-based transmission methods for characterizing grain structure in thinned bulk metals. Foils of type 316 stainless steel were prepared by two methods commonly used for transmission electron microscopy — double-jet electropolishing and focused ion beam milling. A customized holder allowed positioning of the foils in a configuration appropriate for both transmission electron forward scatter diffraction, and for transmission imaging by the use of a forescatter detector with two diodes. We found that both crystallographic orientation maps and dark-field transmitted images could be obtained for specimens prepared by either method. However, for both methods, preparation-induced artifacts may affect the quality or accuracy of transmission SEM data, especially those acquired by the use of transmission Kikuchi diffraction. Generally, the quality of orientation data was better for specimens prepared by electropolishing, due to the absence of ion-induced damage. - Highlights: • The transmission imaging and diffraction techniques are emerging in scanning electron microscopy (SEM) as promising new field of materials characterization. • The manuscript titled: “Transmission Kikuchi Diffraction and Transmission Electron Forescatter Imaging of Electropolished and FIB Manufactured TEM Specimens” documents how different specimen thinning procedures can effect efficiency of transmission Kikuchi diffraction and transmission electron forescatter imaging. • The abilities to make precision crystallographic orientation maps and dark-field images in transmission was studied on electropolished versus focus ion beam manufactured TEM specimens. • Depending on the need, electropolished and focused ion beam technique may produce suitable specimens for transmission imaging and diffraction in SEM.

  16. Electron Gun Technologies for High Resolution Electron Microscopes

    NASA Astrophysics Data System (ADS)

    Fujita, Shin

    High-brightness electron gun technologies for high resolution electron microscopes are reviewed. High performance electron beam apparatuses today are equipped with either Schottky emission or field emission type cathodes, both of which have sharply etched tips for electric field enhancement that promotes electron emission. One of the key elements in these pointed cathodes is a proper control of the tip geometry. It substantially affects the emitter optics and performance. It is shown that the geometry is dictated by the faceting of the tip, which is in turn determined by the Equilibrium Crystal Shape (ECS). The ECS is the tip geometry that minimizes the surface free energy and dependent on the emitter operation environment. By proper choice of the tip field and temperature, one can control the degree of faceting and achieve optically desirable tip geometries.

  17. Depth Sectioning with the Aberration-Corrected Scanning Transmission Electron Microscope

    SciTech Connect

    Borisevich, Albina Y; Lupini, Andrew R; Pennycook, Stephen J

    2006-01-01

    The ability to correct the aberrations of the probe-forming lens in the scanning transmission electron microscope provides not only a significant improvement in transverse resolution but in addition brings depth resolution at the nanometer scale. Aberration correction therefore opens up the possibility of 3D imaging by optical sectioning. Here we develop a definition for the depth resolution for scanning transmission electron microscope depth sectioning and present initial results from this method. Objects such as catalytic metal clusters and single atoms on various support materials are imaged in three dimensions with a resolution of several nanometers. Effective focal depth is determined by statistical analysis and the contributing factors are discussed. Finally, current challenges and future capabilities available through new instruments are discussed.

  18. Mapping magnetism with atomic resolution using aberrated electron probes

    NASA Astrophysics Data System (ADS)

    Idrobo, Juan; Rusz, Ján; McGuire, Michael A.; Symons, Christopher T.; Vatsavai, Ranga Raju; Lupini, Andrew R.

    2015-03-01

    In this talk, we report a direct experimental real-space mapping of magnetic circular dichroism with atomic resolution in aberration-corrected scanning transmission electron microscopy (STEM). Using an aberrated electron probe with customized phase distribution, we reveal with electron energy-loss (EEL) spectroscopy the checkerboard antiferromagnetic ordering of Mn moments in LaMnAsO by observing a dichroic signal in the Mn L-edge. The aberrated probes allow the collection of EEL spectra using the transmitted beam, which results in a magnetic circular dichroic signal with intrinsically larger signal-to-noise ratios than those obtained via nanodiffraction techniques (where most of the transmitted electrons are discarded). The novel experimental setup presented here, which can easily be implemented in aberration-corrected STEM, opens new paths for probing dichroic signals in materials with unprecedented spatial resolution. This research was supported by DOE SUFD MSED, by UT-Battelle, LLC, under Contract No. DE-AC05-00OR22725 with the US DOE, and by the Swedish Research Council and Swedish National Infrastructure for Computing (NSC center)

  19. Aberrated electron probes for magnetic spectroscopy with atomic resolution: Theory and practical aspects

    DOE PAGESBeta

    Rusz, Ján; Idrobo, Juan Carlos

    2016-03-24

    It was recently proposed that electron magnetic circular dichroism (EMCD) can be measured in scanning transmission electron microscopy (STEM) with atomic resolution by tuning the phase distribution of a electron beam. Here, we describe the theoretical and practical aspects for the detection of out-of-plane and in-plane magnetization utilizing atomic size electron probes. Here we present the calculated optimized astigmatic probes and discuss how to achieve them experimentally.

  20. Aberrated electron probes for novel spectroscopy with atomic resolution: theory and practical aspects

    SciTech Connect

    Rusz, Jan; Idrobo Tapia, Juan Carlos

    2016-01-01

    It was recently proposed that electron magnetic circular dichroism (EMCD) can be measured in scanning transmission electron microscopy (STEM) with atomic resolution by tuning the phase distribution of a electron beam. Here, we describe the theoretical and practical aspects for the detection of out-of-plane and in-plane magnetization utilizing atomic size electron probes. We present the calculated optimized astigmatic probes and discuss how to achieve them experimentally.

  1. Aberrated electron probes for magnetic spectroscopy with atomic resolution: Theory and practical aspects

    NASA Astrophysics Data System (ADS)

    Rusz, Ján; Idrobo, Juan Carlos

    2016-03-01

    It was recently proposed that electron magnetic circular dichroism can be measured in scanning transmission electron microscopy with atomic resolution by tuning the phase distribution of an electron beam. Here, we describe the theoretical and practical aspects for the detection of out-of-plane and in-plane magnetization utilizing atomic size electron probes. We present the calculated optimized astigmatic probes and discuss how to achieve them experimentally.

  2. Time of flight secondary ion mass spectrometry and high-resolution transmission electron microscopy/energy dispersive spectroscopy: a preliminary study of the distribution of Cu2+ and Cu2+/Pb2+ on a Bt horizon surfaces.

    PubMed

    Cerqueira, B; Vega, F A; Serra, C; Silva, L F O; Andrade, M L

    2011-11-15

    Relatively new techniques can help in determining the occurrence of mineral species and the distribution of contaminants on soil surfaces such as natural minerals and organic matter. The Bt horizon from an Endoleptic Luvisol was chosen because of its well-known sorption capability. The samples were contaminated with Cu(2+) and/or Pb(2+) and both sorption and desorption experiments were performed. The preferential distribution of the contaminant species ((63)Cu and (208)Pb) to the main soil components and their associations were studied together with the effectiveness of the surface sorption and desorption processes. The results obtained were compared with non-contaminated samples as well as with previous results obtained by different analytical techniques and advanced statistical analysis. Pb(2+) competes favorably for the sorption sites in this soil, mainly in oxides and the clay fraction. Cu(2+) and Pb(2+) were mainly associated with hematite, gibbsite, vermiculite and chlorite. This study will serve as a basis for further scientific research on the soil retention of heavy metals. New techniques such as spectroscopic imaging and transmission electron microscopy make it possible to check which soil components retain heavy metals, thereby contributing to propose effective measures for the remediation of contaminated soil. PMID:21920666

  3. High resolution electron attachment to CO₂ clusters.

    PubMed

    Denifl, Stephan; Vizcaino, Violaine; Märk, Tilmann D; Illenberger, Eugen; Scheier, Paul

    2010-01-01

    Electron attachment to CO₂ clusters performed at high energy resolution (0.1 eV) is studied for the first time in the extended electron energy range from threshold (0 eV) to about 10 eV. Dissociative electron attachment (DEA) to single molecules yields O(-) as the only fragment ion arising from the well known (2)Π(u) shape resonance (ion yield centered at 4.4 eV) and a core excited resonance (at 8.2 eV). On proceeding to CO₂ clusters, non-dissociated complexes of the form (CO₂)(n)(-) including the monomer CO₂(-) are generated as well as solvated fragment ions of the form (CO₂)(n)O(-). The non-decomposed complexes appear already within a resonant feature near threshold (0 eV) and also within a broad contribution between 1 and 4 eV which is composed of two resonances observed for example for (CO₂)(4)(-) at 2.2 eV and 3.1 eV (peak maxima). While the complexes observed around 3.1 eV are generated via the (2)Π(u) resonance as precursor with subsequent intracluster relaxation, the contribution around 2.2 eV can be associated with a resonant scattering feature, recently discovered in single CO₂ in the selective excitation of the higher energy member of the well known Fermi dyad [M. Allan, Phys. Rev. Lett., 2001, 87, 0332012]. Formation of (CO₂)(n)(-) in the threshold region involves vibrational Feshbach resonances (VFRs) as previously discovered via an ultrahigh resolution (1 meV) laser photoelectron attachment method [E. Leber, S. Barsotti, I. I. Fabrikant, J. M. Weber, M.-W. Ruf and H. Hotop, Eur. Phys. J. D, 2000, 12, 125]. The complexes (CO₂)(n)O(-) clearly arise from DEA at an individual molecule within the cluster involving both the (2)Π(u) and the core excited resonance. PMID:21491691

  4. High cycle fatigue in the transmission electron microscope

    DOE PAGESBeta

    Bufford, Daniel C.; Stauffer, Douglas; Mook, William M.; Syed Asif, S. A.; Boyce, Brad L.; Hattar, Khalid

    2016-06-28

    One of the most common causes of structural failure in metals is fatigue induced by cyclic loading. Historically, microstructure-level analysis of fatigue cracks has primarily been performed post mortem. However, such investigations do not directly reveal the internal structural processes at work near micro- and nanoscale fatigue cracks and thus do not provide direct evidence of active microstructural mechanisms. In this paper, the tension–tension fatigue behavior of nanocrystalline Cu was monitored in real time at the nanoscale by utilizing a new capability for quantitative cyclic mechanical loading performed in situ in a transmission electron microscope (TEM). Controllable loads were appliedmore » at frequencies from one to several hundred hertz, enabling accumulations of 106 cycles within 1 h. The nanometer-scale spatial resolution of the TEM allows quantitative fatigue crack growth studies at very slow crack growth rates, measured here at ~10–12 m·cycle–1. This represents an incipient threshold regime that is well below the tensile yield stress and near the minimum conditions for fatigue crack growth. Evidence of localized deformation and grain growth within 150 nm of the crack tip was observed by both standard imaging and precession electron diffraction orientation mapping. Finally, these observations begin to reveal with unprecedented detail the local microstructural processes that govern damage accumulation, crack nucleation, and crack propagation during fatigue loading in nanocrystalline Cu.« less

  5. Amyloid Structure and Assembly: Insights from Scanning Transmission Electron Microscopy

    SciTech Connect

    Goldsbury, C.; Wall, J.; Baxa, U.; Simon, M. N.; Steven, A. C.; Engel, A.; Aebi, U.; Muller, S. A.

    2011-01-01

    Amyloid fibrils are filamentous protein aggregates implicated in several common diseases such as Alzheimer's disease and type II diabetes. Similar structures are also the molecular principle of the infectious spongiform encephalopathies such as Creutzfeldt-Jakob disease in humans, scrapie in sheep, and of the so-called yeast prions, inherited non-chromosomal elements found in yeast and fungi. Scanning transmission electron microscopy (STEM) is often used to delineate the assembly mechanism and structural properties of amyloid aggregates. In this review we consider specifically contributions and limitations of STEM for the investigation of amyloid assembly pathways, fibril polymorphisms and structural models of amyloid fibrils. This type of microscopy provides the only method to directly measure the mass-per-length (MPL) of individual filaments. Made on both in vitro assembled and ex vivo samples, STEM mass measurements have illuminated the hierarchical relationships between amyloid fibrils and revealed that polymorphic fibrils and various globular oligomers can assemble simultaneously from a single polypeptide. The MPLs also impose strong constraints on possible packing schemes, assisting in molecular model building when combined with high-resolution methods like solid-state nuclear magnetic resonance (NMR) and electron paramagnetic resonance (EPR).

  6. High Cycle Fatigue in the Transmission Electron Microscope.

    PubMed

    Bufford, Daniel C; Stauffer, Douglas; Mook, William M; Syed Asif, S A; Boyce, Brad L; Hattar, Khalid

    2016-08-10

    One of the most common causes of structural failure in metals is fatigue induced by cyclic loading. Historically, microstructure-level analysis of fatigue cracks has primarily been performed post mortem. However, such investigations do not directly reveal the internal structural processes at work near micro- and nanoscale fatigue cracks and thus do not provide direct evidence of active microstructural mechanisms. In this study, the tension-tension fatigue behavior of nanocrystalline Cu was monitored in real time at the nanoscale by utilizing a new capability for quantitative cyclic mechanical loading performed in situ in a transmission electron microscope (TEM). Controllable loads were applied at frequencies from one to several hundred hertz, enabling accumulations of 10(6) cycles within 1 h. The nanometer-scale spatial resolution of the TEM allows quantitative fatigue crack growth studies at very slow crack growth rates, measured here at ∼10(-12) m·cycle(-1). This represents an incipient threshold regime that is well below the tensile yield stress and near the minimum conditions for fatigue crack growth. Evidence of localized deformation and grain growth within 150 nm of the crack tip was observed by both standard imaging and precession electron diffraction orientation mapping. These observations begin to reveal with unprecedented detail the local microstructural processes that govern damage accumulation, crack nucleation, and crack propagation during fatigue loading in nanocrystalline Cu. PMID:27351706

  7. Quantitative Energy-filtering Transmission Electron Microscopy in Materials Science.

    PubMed

    Grogger; Hofer; Warbichler; Kothleitner

    2000-03-01

    Energy-filtered transmission electron microscopy (EFTEM) can be used to acquire elemental distribution images at high lateral resolution within short acquisition times. In this article, we present an overview of typical problems from materials science which can be preferentially solved by means of EFTEM. In the first example, we show how secondary phases in a steel specimen can be easily detected by recording jump ratio images of the matrix element under rocking beam illumination. Secondly, we describe how elemental maps can be converted into concentration maps. A Ba-Nd-titanate ceramics serves as a typical materials science example exhibiting three different compounds with varying composition. In order to reduce diffraction and/or thickness variation effects which may be a problem for quantification of crystalline specimens, we calculated atomic ratio maps by dividing two elemental maps and subsequent normalizing by the partial ionization cross-sections (or k-factors). Additionally, the atomic ratio maps are correlated using the scatter diagram technique thus leading to quantitative chemical phase maps. Finally, we show how the near-edge structures (electron energy-loss near edge fine structures, or ELNES) can be used for mapping chemical bonding states thus differentiating between various modifications of an element. In order to distinguish between diamond and non-diamond carbon in diamond coated materials, we have investigated a diamond layer on a substrate with the help of ELNES mapping utilizing the pi*-peak of the C-K ionization edge. PMID:10742404

  8. Microstructural studies of dental amalgams using analytical transmission electron microscopy

    NASA Astrophysics Data System (ADS)

    Hooghan, Tejpal Kaur

    Dental amalgams have been used for centuries as major restorative materials for decaying teeth. Amalgams are prepared by mixing alloy particles which contain Ag, Sn, and Cu as the major constituent elements with liquid Hg. The study of microstructure is essential in understanding the setting reactions and improving the properties of amalgams. Until the work reported in this dissertation, optical microscopy (OM), scanning electron microscopy (SEM), and x-ray diffractometry (XRD) were used commonly to analyze amalgam microstructures. No previous systematic transmission electron microscopy (TEM) study has been performed due to sample preparation difficulties and composite structure of dental amalgams. The goal of this research was to carry out detailed microstructural and compositional studies of dental amalgams. This was accomplished using the enhanced spatial resolution of the TEM and its associated microanalytical techniques, namely, scanning transmission electron microscopy (STEM), x-ray energy dispersive spectroscopy (XEDS) and micro-microdiffraction (mumuD). A new method was developed for thinning amalgam samples to electron transparency using the "wedge technique." Velvalloy, a low-Cu amalgam, and Tytin, a high-Cu amalgam, were the two amalgams characterized. Velvalloy is composed of a Agsb2Hgsb3\\ (gammasb1)/HgSnsb{7-9}\\ (gammasb2) matrix surrounding unreacted Agsb3Sn (gamma) particles. In addition, hitherto uncharacterized reaction layers between Agsb3Sn(gamma)/Agsb2Hgsb3\\ (gammasb2)\\ and\\ Agsb2Hgsb3\\ (gammasb1)/HgSnsb{7-9}\\ (gammasb2) were observed and analyzed. An Ag-Hg-Sn (betasb1) phase was clearly identified for the first time. In Tytin, the matrix consists of Agsb2Hgsb3\\ (gammasb1) grains. Fine precipitates of Cusb6Snsb5\\ (etasp') are embedded inside the gammasb1 and at the grain boundaries. These precipitates are responsible for the improved creep resistance of Tytin compared to Velvalloy. The additional Cu has completely eliminated the gammasb

  9. Angularly-selective transmission imaging in a scanning electron microscope.

    PubMed

    Holm, Jason; Keller, Robert R

    2016-08-01

    This work presents recent advances in transmission scanning electron microscopy (t-SEM) imaging control capabilities. A modular aperture system and a cantilever-style sample holder that enable comprehensive angular selectivity of forward-scattered electrons are described. When combined with a commercially available solid-state transmission detector having only basic bright-field and dark-field imaging capabilities, the advances described here enable numerous transmission imaging modes. Several examples are provided that demonstrate how contrast arising from diffraction to mass-thickness can be obtained. Unanticipated image contrast at some imaging conditions is also observed and addressed. PMID:27179301

  10. Electron transmission through a class of anthracene aldehyde molecules

    NASA Astrophysics Data System (ADS)

    Petreska, Irina; Ohanesjan, Vladimir; Pejov, Ljupco; Kocarev, Ljupco

    2016-03-01

    Transmission of electrons via metal-molecule-metal junctions, involving rotor-stator anthracene aldehyde molecules is investigated. Two model barriers having input parameters evaluated from accurate ab initio calculations are proposed and the transmission coefficients are obtained by using the quasiclassical approximation. Transmission coefficients further enter in the integral for the net current, utilizing Simmons' method. Conformational dependence of the tunneling processes is evident and the presence of the side groups enhances the functionality of the future single-molecule based electronic devices.

  11. Elastic and inelastic transmission of electrons through tapered glass capillaries

    NASA Astrophysics Data System (ADS)

    Wickramarachchi, S. J.; Keerthisinghe, D.; Dassanayake, B. S.; Tanis, J. A.; Ikeda, T.

    2013-05-01

    The transmission of electrons through tapered borosilicate glass capillaries has been studied for 500 and 1000 eV incident electrons. The energy and angular dependence of the transmitted electrons as well as the temporal charge deposition has been investigated. The capillaries had inlet/outlet diameters of 800 μm/100 μm and 700 μm/20 μm and lengths of 35 mm. Transmission was observed for tilt angles up to 9.5o, and 1.5o, respectively, for the two capillaries. The transmitted electrons were found to have both elastic and inelastic behavior as was observed for electrons through PET and single straight glass capillaries. The charge deposition with time consisted of stable transmission, fluctuations, blocking, and self discharging for both capillaries depending on the sample tilt angle.

  12. Visualizing Macromolecular Complexes with In Situ Liquid Scanning Transmission Electron Microscopy

    SciTech Connect

    Evans, James E.; Jungjohann, K. L.; Wong, Peony C. K.; Chiu, Po-Lin; Dutrow, Gavin H.; Arslan, Ilke; Browning, Nigel D.

    2012-11-01

    A central focus of biological research is understanding the structure/function relationship of macromolecular protein complexes. Yet conventional transmission electron microscopy techniques are limited to static observations. Here we present the first direct images of purified macromolecular protein complexes using in situ liquid scanning transmission electron microscopy. Our results establish the capability of this technique for visualizing the interface between biology and nanotechnology with high fidelity while also probing the interactions of biomolecules within solution. This method represents an important advancement towards allowing future high-resolution observations of biological processes and conformational dynamics in real-time.

  13. Possibilities and limitations of advanced transmission electron microscopy for carbon-based nanomaterials

    PubMed Central

    Bittencourt, Carla; Van Tendeloo, Gustaaf

    2015-01-01

    Summary A major revolution for electron microscopy in the past decade is the introduction of aberration correction, which enables one to increase both the spatial resolution and the energy resolution to the optical limit. Aberration correction has contributed significantly to the imaging at low operating voltages. This is crucial for carbon-based nanomaterials which are sensitive to electron irradiation. The research of carbon nanomaterials and nanohybrids, in particular the fundamental understanding of defects and interfaces, can now be carried out in unprecedented detail by aberration-corrected transmission electron microscopy (AC-TEM). This review discusses new possibilities and limits of AC-TEM at low voltage, including the structural imaging at atomic resolution, in three dimensions and spectroscopic investigation of chemistry and bonding. In situ TEM of carbon-based nanomaterials is discussed and illustrated through recent reports with particular emphasis on the underlying physics of interactions between electrons and carbon atoms. PMID:26425406

  14. Microstructural evaluation of ? bilayer film by transmission electron microscopy

    NASA Astrophysics Data System (ADS)

    Wu, Yuan; Liu, Wei; Wang, Ruilan; Xuan, Yi; Li, Lin; Li, Hongchen; Xi, Xiao Xing

    1998-07-01

    The microstructure of 0022-3727/31/14/005/img11Cu0022-3727/31/14/005/img12 bilayer film grown on 0022-3727/31/14/005/img13 substrate was studied by high-resolution transmission electron microscopy (HREM). The results showed that the 0022-3727/31/14/005/img14 film is epitaxially grown on the 0022-3727/31/14/005/img13 substrate with c axis orientation. Planar defects, grain boundaries, moiré patterns, a axis oriented 0022-3727/31/14/005/img14 and impurity particulates are found in the 0022-3727/31/14/005/img14 film. The 0022-3727/31/14/005/img18 film was grown on the 0022-3727/31/14/005/img14 film with a columnar structure. However, some region of the 0022-3727/31/14/005/img18 film is single crystalline, but with strain bands. The development of strain bands in the 0022-3727/31/14/005/img18 film could be a result of lattice mismatch between 0022-3727/31/14/005/img14 and 0022-3727/31/14/005/img18 films and the surface roughness of the 0022-3727/31/14/005/img14 film. In consequence, the dielectric properties of the strained STO film are greatly decreased compared to the bulk single crystalline STO.

  15. Electron tomography of HEK293T cells using scanning electron microscope-based scanning transmission electron microscopy.

    PubMed

    You, Yun-Wen; Chang, Hsun-Yun; Liao, Hua-Yang; Kao, Wei-Lun; Yen, Guo-Ji; Chang, Chi-Jen; Tsai, Meng-Hung; Shyue, Jing-Jong

    2012-10-01

    Based on a scanning electron microscope operated at 30 kV with a homemade specimen holder and a multiangle solid-state detector behind the sample, low-kV scanning transmission electron microscopy (STEM) is presented with subsequent electron tomography for three-dimensional (3D) volume structure. Because of the low acceleration voltage, the stronger electron-atom scattering leads to a stronger contrast in the resulting image than standard TEM, especially for light elements. Furthermore, the low-kV STEM yields less radiation damage to the specimen, hence the structure can be preserved. In this work, two-dimensional STEM images of a 1-μm-thick cell section with projection angles between ±50° were collected, and the 3D volume structure was reconstructed using the simultaneous iterative reconstructive technique algorithm with the TomoJ plugin for ImageJ, which are both public domain software. Furthermore, the cross-sectional structure was obtained with the Volume Viewer plugin in ImageJ. Although the tilting angle is constrained and limits the resulting structural resolution, slicing the reconstructed volume generated the depth profile of the thick specimen with sufficient resolution to examine cellular uptake of Au nanoparticles, and the final position of these nanoparticles inside the cell was imaged. PMID:23026379

  16. High-Resolution Analytical Electron Microscopy Characterization of Corrosion and Cracking at Buried Interfaces

    SciTech Connect

    Bruemmer, Stephen M.; Thomas, Larry E.

    2001-07-01

    Recent results are presented demonstrating the application of cross-sectional analytical transmission electron microscopy (ATEM) to corrosion and cracking in high-temperature water environments. Microstructural, chemical and crystallographic characterization of buried interfaces at near-atomic resolutions is shown to reveal evidence for unexpected local environments, corrosion reactions and material transformations. Information obtained by a wide variety of high-resolution imaging and analysis methods indicates the processes occurring during crack advance and provides insights into the mechanisms controlling environmental degradation.

  17. Transmission Electron Microscopy Characterization of Helium Bubbles in Aged Plutonium

    SciTech Connect

    Schwartz, A J; Wall, M A; Zocco, T G; Blobaum, K M

    2004-11-02

    The self-irradiation damage generated by alpha decay of plutonium results in the formation of lattice defects, helium, and uranium atoms. Over time, microstructural evolution resulting from the self-irradiation may influence the physical and mechanical properties of the material. In order to assess microstructural changes, we have developed and applied procedures for the specimen preparation, handling, and transmission electron microscopy characterization of Pu alloys. These transmission electron microscopy investigations of Pu-Ga alloys ranging in age up to 42-years old reveal the presence of nanometer-sized helium bubbles. The number density of bubbles and the average size have been determined for eight different aged materials.

  18. A compact, light weight, high resolution electron monochromator

    NASA Astrophysics Data System (ADS)

    Goembel, L.; Doering, J. P.

    1995-06-01

    A high resolution electron monochromator that incorporates Vespel polyimide plastic in its construction is described. A great saving in bulk can be realized by mounting the electron optical elements in Vespel tubes rather than mounting them by traditional means.

  19. Cell effects on high-resolution transmission spectrophotometry

    NASA Astrophysics Data System (ADS)

    Soares, Oliverio D.

    1998-12-01

    Liquids molecular transmission spectrophotometry has a broad area of applications including spectrophotometry. The measurement of the spectral transmission factor could require levels of accuracy in the order of 10-3 to 10-4. This implies the need for detailed analysis of the corrections to compensate measuring cell unpairing, differences in refractive index between reference liquid (water or solvent) and corresponding spectral non-flatness as well as the multiple inter-reflection at the various dielectric interfaces. Procedures for self-correction of optical measuring cells unpairing and compensation of further effects are presented.

  20. Scanning image detection (SID) system for conventional transmission electron microscope (CTEM) images.

    PubMed

    Tanji, T; Tomita, M; Kobayashi, H

    1990-08-01

    A new image detection system has been developed to display transmission electron microscope (TEM) images on a CRT without a video camera system. Deflection coils placed in both the upper space of an objective lens and in the lower space of the first intermediate lens scan a small electron probe simultaneously. The electrical signal acquired through an improved scintillator and a photomultiplier is synchronized with the scanning signal and displayed in a similar fashion to a conventional scanning TEM (STEM) instrument. A preliminary system using a 100 kV conventional TEM (CTEM) equipped with a hairpin-type electron gun, produced an image with a spatial resolution of 1 nm. PMID:2391565

  1. Surface sensitivity in scanning transmission x-ray microspectroscopy using secondary electron detection.

    PubMed

    Hub, C; Wenzel, S; Raabe, J; Ade, H; Fink, R H

    2010-03-01

    The successful integration of electron detection into an existing scanning transmission x-ray microspectroscope (STXM) at the Swiss Light Source is demonstrated. In conventional x-ray detection using a photomultiplier, STXM offers mainly bulk sensitivity combined with high lateral resolution. However, by implementation of a channeltron electron multiplier, the surface sensitivity can be established by the detection of secondary electrons emitted from the sample upon resonant excitation. We describe the experimental setup and discuss several relevant aspects, in particular the schemes to correct for self-absorption in the specimen due to back illumination in case of thicker films. PMID:20370182

  2. Efficient linear phase contrast in scanning transmission electron microscopy with matched illumination and detector interferometry

    NASA Astrophysics Data System (ADS)

    Ophus, Colin; Ciston, Jim; Pierce, Jordan; Harvey, Tyler R.; Chess, Jordan; McMorran, Benjamin J.; Czarnik, Cory; Rose, Harald H.; Ercius, Peter

    2016-02-01

    The ability to image light elements in soft matter at atomic resolution enables unprecedented insight into the structure and properties of molecular heterostructures and beam-sensitive nanomaterials. In this study, we introduce a scanning transmission electron microscopy technique combining a pre-specimen phase plate designed to produce a probe with structured phase with a high-speed direct electron detector to generate nearly linear contrast images with high efficiency. We demonstrate this method by using both experiment and simulation to simultaneously image the atomic-scale structure of weakly scattering amorphous carbon and strongly scattering gold nanoparticles. Our method demonstrates strong contrast for both materials, making it a promising candidate for structural determination of heterogeneous soft/hard matter samples even at low electron doses comparable to traditional phase-contrast transmission electron microscopy. Simulated images demonstrate the extension of this technique to the challenging problem of structural determination of biological material at the surface of inorganic crystals.

  3. Efficient linear phase contrast in scanning transmission electron microscopy with matched illumination and detector interferometry

    PubMed Central

    Ophus, Colin; Ciston, Jim; Pierce, Jordan; Harvey, Tyler R.; Chess, Jordan; McMorran, Benjamin J.; Czarnik, Cory; Rose, Harald H.; Ercius, Peter

    2016-01-01

    The ability to image light elements in soft matter at atomic resolution enables unprecedented insight into the structure and properties of molecular heterostructures and beam-sensitive nanomaterials. In this study, we introduce a scanning transmission electron microscopy technique combining a pre-specimen phase plate designed to produce a probe with structured phase with a high-speed direct electron detector to generate nearly linear contrast images with high efficiency. We demonstrate this method by using both experiment and simulation to simultaneously image the atomic-scale structure of weakly scattering amorphous carbon and strongly scattering gold nanoparticles. Our method demonstrates strong contrast for both materials, making it a promising candidate for structural determination of heterogeneous soft/hard matter samples even at low electron doses comparable to traditional phase-contrast transmission electron microscopy. Simulated images demonstrate the extension of this technique to the challenging problem of structural determination of biological material at the surface of inorganic crystals. PMID:26923483

  4. Efficient linear phase contrast in scanning transmission electron microscopy with matched illumination and detector interferometry.

    PubMed

    Ophus, Colin; Ciston, Jim; Pierce, Jordan; Harvey, Tyler R; Chess, Jordan; McMorran, Benjamin J; Czarnik, Cory; Rose, Harald H; Ercius, Peter

    2016-01-01

    The ability to image light elements in soft matter at atomic resolution enables unprecedented insight into the structure and properties of molecular heterostructures and beam-sensitive nanomaterials. In this study, we introduce a scanning transmission electron microscopy technique combining a pre-specimen phase plate designed to produce a probe with structured phase with a high-speed direct electron detector to generate nearly linear contrast images with high efficiency. We demonstrate this method by using both experiment and simulation to simultaneously image the atomic-scale structure of weakly scattering amorphous carbon and strongly scattering gold nanoparticles. Our method demonstrates strong contrast for both materials, making it a promising candidate for structural determination of heterogeneous soft/hard matter samples even at low electron doses comparable to traditional phase-contrast transmission electron microscopy. Simulated images demonstrate the extension of this technique to the challenging problem of structural determination of biological material at the surface of inorganic crystals. PMID:26923483

  5. Unveiling nanometric plasmons optical properties with advanced electron spectroscopy in the Scanning Transmission Electron Microscope

    NASA Astrophysics Data System (ADS)

    Kociak, Mathieu

    Since the pioneering work of Yamamoto, the use of electron spectroscopy such as Cathodoluminescence (CL) and Electron Energy Loss Spectroscopy (EELS) in a Scanning (Transmission) Electron Microscope (STEM) has considerably helped improving our understanding of the optical properties of metallic nanoparticles. The resemblance of spectroscopic signals from electron and pure optical techniques leads to the intuition that both types of techniques are very close, an idea theoretically discussed by F.J. Garcia de Abajo and coworkers. However, it is also quite intuitive that CL and EELS should be different. For example, EELS helps detecting any sort of modes while CL can only detect radiative ones. On the other hand, even between optical spectroscopy techniques, clear differences such as energy shifts or spectral shapes changes are expected in the case of plasmons. The lack of adapted instrumentation capable of performing combined EELS and CL, as well as theoretical developments allowing to account for the generic difference between EELS and CL and their optical counterparts impeached a comprehensive understanding of plasmons physics with the otherwise amazing electron spectroscopies. In this talk, I will present recent experimental results showing combined EELS and CL spectral mapping of plasmonic properties for nanoparticles with several shapes (triangles, cubes, stars...) and composition (gold, silver, aluminum...). Helped with different theoretical tools, I will try to show how these results can be related to their optical counterparts (extinction, scattering), and what type of physical insights can be gained from these combined measurements. Finally, if time allows, pointing the weaknesses of state-of-the-art CL and EELS (in terms of spectral range and/or spectral resolution), I will present EELS results obtained on highly monochromated electron beams that could cope with these limitations

  6. Molecular interactions on single-walled carbon nanotubes revealed by high-resolution transmission microscopy

    PubMed Central

    Umeyama, Tomokazu; Baek, Jinseok; Sato, Yuta; Suenaga, Kazu; Abou-Chahine, Fawzi; Tkachenko, Nikolai V.; Lemmetyinen, Helge; Imahori, Hiroshi

    2015-01-01

    The close solid-state structure–property relationships of organic π−aromatic molecules have attracted interest due to their implications for the design of organic functional materials. In particular, a dimeric structure, that is, a unit consisting of two molecules, is required for precisely evaluating intermolecular interactions. Here, we show that the sidewall of a single-walled carbon nanotube (SWNT) represents a unique molecular dimer platform that can be directly visualized using high-resolution transmission electron microscopy. Pyrene is chosen as the π−aromatic molecule; its dimer is covalently linked to the SWNT sidewalls by aryl addition. Reflecting the orientation and separation of the two molecules, the pyrene dimer on the SWNT exhibits characteristic optical and photophysical properties. The methodology discussed here—form and probe molecular dimers—is highly promising for the creation of unique models and provides indispensable and fundamental information regarding molecular interactions. PMID:26173983

  7. Molecular interactions on single-walled carbon nanotubes revealed by high-resolution transmission microscopy

    NASA Astrophysics Data System (ADS)

    Umeyama, Tomokazu; Baek, Jinseok; Sato, Yuta; Suenaga, Kazu; Abou-Chahine, Fawzi; Tkachenko, Nikolai V.; Lemmetyinen, Helge; Imahori, Hiroshi

    2015-07-01

    The close solid-state structure-property relationships of organic π-aromatic molecules have attracted interest due to their implications for the design of organic functional materials. In particular, a dimeric structure, that is, a unit consisting of two molecules, is required for precisely evaluating intermolecular interactions. Here, we show that the sidewall of a single-walled carbon nanotube (SWNT) represents a unique molecular dimer platform that can be directly visualized using high-resolution transmission electron microscopy. Pyrene is chosen as the π-aromatic molecule; its dimer is covalently linked to the SWNT sidewalls by aryl addition. Reflecting the orientation and separation of the two molecules, the pyrene dimer on the SWNT exhibits characteristic optical and photophysical properties. The methodology discussed here--form and probe molecular dimers--is highly promising for the creation of unique models and provides indispensable and fundamental information regarding molecular interactions.

  8. Characterisation of nanoparticles by means of high-resolution SEM/EDS in transmission mode

    NASA Astrophysics Data System (ADS)

    Hodoroaba, V.-D.; Rades, S.; Salge, T.; Mielke, J.; Ortel, E.; Schmidt, R.

    2016-02-01

    Advances in scanning electron microscopy (SEM) enable the high-resolution imaging of single nanoparticles (NPs) with sizes well below 10 nm. The SEM analysis in transmission mode (T-SEM) of NPs on thin film supports has many benefits when compared to the analysis of NPs on bulk substrates. The enhanced material (mass - thickness) contrast of the T-SEM imaging mode is well suited for in-depth and, particularly valuable, to very accurate, traceable, lateral dimensional measurements of NPs. Compared to samples prepared on bulk substrates, T-SEM with energy dispersive X-ray spectroscopy (EDS) achieves a drastically improved spatial resolution of the emitted X-rays. The poor signal-to-noise ratio of the X-ray spectra emitted by a single nanoparticle (NP) can be improved by the use of high-sensitivity (high collection solid angle) silicon drift (SDD), energy-dispersive X-ray spectrometers (EDS). The EDS spectral imaging of a single NP with a spatial resolution below 10 nm has become possible. This is demonstrated by means of various examples of nanostructures. Advanced data processing of T-SEM/EDS results sets the stage for the automated classification of NPs by feature analysis. This method combines the detection of morphological structures of interest by image processing of T-SEM micrographs with the chemical classification by EDS.

  9. Dose-dependent high-resolution electron ptychography

    NASA Astrophysics Data System (ADS)

    D'Alfonso, A. J.; Allen, L. J.; Sawada, H.; Kirkland, A. I.

    2016-02-01

    Recent reports of electron ptychography at atomic resolution have ushered in a new era of coherent diffractive imaging in the context of electron microscopy. We report and discuss electron ptychography under variable electron dose conditions, exploring the prospects of an approach which has considerable potential for imaging where low dose is needed.

  10. Highlighting material structure with transmission electron diffraction correlation coefficient maps.

    PubMed

    Kiss, Ákos K; Rauch, Edgar F; Lábár, János L

    2016-04-01

    Correlation coefficient maps are constructed by computing the differences between neighboring diffraction patterns collected in a transmission electron microscope in scanning mode. The maps are shown to highlight material structural features like grain boundaries, second phase particles or dislocations. The inclination of the inner crystal interfaces are directly deduced from the resulting contrast. PMID:26866276

  11. Nanowire growth kinetics in aberration corrected environmental transmission electron microscopy.

    PubMed

    Chou, Yi-Chia; Panciera, Federico; Reuter, Mark C; Stach, Eric A; Ross, Frances M

    2016-04-14

    We visualize atomic level dynamics during Si nanowire growth using aberration corrected environmental transmission electron microscopy, and compare with lower pressure results from ultra-high vacuum microscopy. We discuss the importance of higher pressure observations for understanding growth mechanisms and describe protocols to minimize effects of the higher pressure background gas. PMID:27041654

  12. In situ nanoindentation in a transmission electron microscope

    SciTech Connect

    Minor, Andrew M.

    2002-12-02

    This dissertation presents the development of the novel mechanical testing technique of in situ nanoindentation in a transmission electron microscope (TEM). This technique makes it possible to simultaneously observe and quantify the mechanical behavior of nano-scale volumes of solids.

  13. Nanoscale Energy-Filtered Scanning Confocal Electron Microscopy Using a Double-Aberration-Corrected Transmission Electron Microscope

    SciTech Connect

    Wang Peng; Behan, Gavin; Kirkland, Angus I.; Nellist, Peter D.; Takeguchi, Masaki; Hashimoto, Ayako; Mitsuishi, Kazutaka; Shimojo, Masayuki

    2010-05-21

    We demonstrate that a transmission electron microscope fitted with two spherical-aberration correctors can be operated as an energy-filtered scanning confocal electron microscope. A method for establishing this mode is described and initial results showing 3D chemical mapping with nanoscale sensitivity to height and thickness changes in a carbon film are presented. Importantly, uncorrected chromatic aberration does not limit the depth resolution of this technique and moreover performs an energy-filtering role, which is explained in terms of a combined depth and energy-loss response function.

  14. Transmission mode time-reversal super-resolution imaging.

    PubMed

    Lehman, Sean K; Devaney, Anthony J

    2003-05-01

    The theory of time-reversal super-resolution imaging of point targets embedded in a reciprocal background medium [A. J. Devaney, "Super-resolution imaging using time-reversal and MUSIC," J. Acoust. Soc. Am. (to be published)] is generalized to the case where the transmitter and receiver sensor arrays need not be coincident and for cases where the background medium can be nonreciprocal. The new theory developed herein is based on the singular value decomposition of the generalized multistatic data matrix of the sensor system rather than the standard eigenvector/eigenvalue decomposition of the time-reversal matrix as was employed in the above-mentioned work and other treatments of time-reversal imaging [Prada, Thomas, and Fink, "The iterative time reversal process: Analysis of the convergence," J. Acoust. Soc. Am. 97, 62 (1995); Prada et al., "Decomposition of the time reversal operator: Detection and selective focusing on two scatterers," J. Acoust. Soc. Am. 99, 2067 (1996)]. A generalized multiple signal classification (MUSIC) algorithm is derived that allows super-resolution imaging of both well-resolved and non-well-resolved point targets from arbitrary sensor array geometries. MUSIC exploits the orthogonal nature of the scatterer and noise subspaces defined by the singular vectors of the multistatic data matrix to form scatterer images. The time-reversal/MUSIC algorithm is tested and validated in two computer simulations of offset vertical seismic profiling where the sensor sources are aligned along the earth's surface and the receiver array is aligned along a subsurface borehole. All results demonstrate the high contrast, high resolution imaging capabilities of this new algorithm combination when compared with "classical" backpropagation or field focusing. Above and beyond the application of seismo-acoustic imaging, the time-reversal super-resolution theory has applications in ocean acoustics for target location, and ultrasonic nondestructive evaluation of

  15. Liquid scanning transmission electron microscopy: Nanoscale imaging in micrometers-thick liquids

    NASA Astrophysics Data System (ADS)

    Schuh, Tobias; de Jonge, Niels

    2014-02-01

    Scanning transmission electron microscopy (STEM) of specimens in liquid is possible using a microfluidic chamber with thin silicon nitride windows. This paper includes an analytic equation of the resolution as a function of the sample thickness and the vertical position of an object in the liquid. The equipment for STEM of liquid specimen is briefly described. STEM provides nanometer resolution in micrometer-thick liquid layers with relevance for both biological research and materials science. Using this technique, we investigated tagged proteins in whole eukaryotic cells, and gold nanoparticles in liquid with time-lapse image series. Possibly future applications are discussed.

  16. High resolution electron microscopy and spectroscopy of ferritin in thin window liquid cells

    NASA Astrophysics Data System (ADS)

    Wang, Canhui; Qiao, Qiao; Shokuhfar, Tolou; Klie, Robert

    2014-03-01

    In-situ transmission electron microscopy (TEM) has seen a dramatic increase in interest in recent years with the commercial development of liquid and gas stages. High-resolution TEM characterization of samples in a liquid environment remains limited by radiation damage and loss of resolution due to the thick window-layers required by the in-situ stages. We introduce thin-window static-liquid cells that enable sample imaging with atomic resolution and electron energy-loss (EEL) spectroscopy with 1.3 nm resolution. Using this approach, atomic and electronic structures of biological samples such as ferritin is studied via in-situ transmission electron microscopy experiments. Ferritin in solution is encapsulated using the static liquid cells with reduced window thickness. The integrity of the thin window liquid cell is maintained by controlling the electron dose rate. Radiation damage of samples, such as liquid water and protein, is quantitatively studied to allow precision control of radiation damage level within the liquid cells. Biochemical reactions, such as valence change of the iron in a functioning ferritin, is observed and will be quantified. Relevant biochemical activity: the release and uptake of Fe atoms through the channels of ferritin protein shell is also imaged at atomic resolution. This work is funded by Michigan Technological University. The UIC JEOL JEM-ARM200CF is supported by an MRI-R2 grant from the National Science Foundation (Grant No. DMR-0959470).

  17. Foucault imaging by using non-dedicated transmission electron microscope

    NASA Astrophysics Data System (ADS)

    Taniguchi, Yoshifumi; Matsumoto, Hiroaki; Harada, Ken

    2012-08-01

    An electron optical system for observing Foucault images was constructed using a conventional transmission electron microscope without any special equipment for Lorentz microscopy. The objective lens was switched off and an electron beam was converged by a condenser optical system to the crossover on the selected area aperture plane. The selected area aperture was used as an objective aperture to select the deflected beam for Foucault mode, and the successive image-forming lenses were controlled for observation of the specimen images. The irradiation area on the specimen was controlled by selecting the appropriate diameter of the condenser aperture.

  18. Transmission of electrons inside the cryogenic pumps of ITER injector.

    PubMed

    Veltri, P; Sartori, E

    2016-02-01

    Large cryogenic pumps are installed in the vessel of large neutral beam injectors (NBIs) used to heat the plasma in nuclear fusion experiments. The operation of such pumps can be compromised by the presence of stray secondary electrons that are generated along the beam path. In this paper, we present a numerical model to analyze the propagation of the electrons inside the pump. The aim of the study is to quantify the power load on the active pump elements, via evaluation of the transmission probabilities across the domain of the pump. These are obtained starting from large datasets of particle trajectories, obtained by numerical means. The transmission probability of the electrons across the domain is calculated for the NBI of the ITER and for its prototype Megavolt ITer Injector and Concept Advancement (MITICA) and the results are discussed. PMID:26932041

  19. Transmission of electrons inside the cryogenic pumps of ITER injector

    NASA Astrophysics Data System (ADS)

    Veltri, P.; Sartori, E.

    2016-02-01

    Large cryogenic pumps are installed in the vessel of large neutral beam injectors (NBIs) used to heat the plasma in nuclear fusion experiments. The operation of such pumps can be compromised by the presence of stray secondary electrons that are generated along the beam path. In this paper, we present a numerical model to analyze the propagation of the electrons inside the pump. The aim of the study is to quantify the power load on the active pump elements, via evaluation of the transmission probabilities across the domain of the pump. These are obtained starting from large datasets of particle trajectories, obtained by numerical means. The transmission probability of the electrons across the domain is calculated for the NBI of the ITER and for its prototype Megavolt ITer Injector and Concept Advancement (MITICA) and the results are discussed.

  20. Achieving atomic resolution magnetic dichroism by controlling the phase symmetry of an electron probe

    SciTech Connect

    Rusz, Jan; Idrobo, Juan -Carlos; Bhowmick, Somnath

    2014-09-30

    The calculations presented here reveal that an electron probe carrying orbital angular momentum is just a particular case of a wider class of electron beams that can be used to measure electron magnetic circular dichroism (EMCD) with atomic resolution. It is possible to obtain an EMCD signal with atomic resolution by simply breaking the symmetry of the electron probe phase front using the aberration-corrected optics of a scanning transmission electron microscope. The probe’s required phase distribution depends on the sample’s magnetic symmetry and crystal structure. The calculations indicate that EMCD signals that use the electron probe’s phase are as strong as those obtained by nanodiffraction methods.

  1. Achieving atomic resolution magnetic dichroism by controlling the phase symmetry of an electron probe

    DOE PAGESBeta

    Rusz, Jan; Idrobo, Juan -Carlos; Bhowmick, Somnath

    2014-09-30

    The calculations presented here reveal that an electron probe carrying orbital angular momentum is just a particular case of a wider class of electron beams that can be used to measure electron magnetic circular dichroism (EMCD) with atomic resolution. It is possible to obtain an EMCD signal with atomic resolution by simply breaking the symmetry of the electron probe phase front using the aberration-corrected optics of a scanning transmission electron microscope. The probe’s required phase distribution depends on the sample’s magnetic symmetry and crystal structure. The calculations indicate that EMCD signals that use the electron probe’s phase are as strongmore » as those obtained by nanodiffraction methods.« less

  2. In-situ high-pressure transmission electron microscopy of minerals

    NASA Astrophysics Data System (ADS)

    Wu, J.; Buseck, P. R.

    2010-12-01

    We show that high-resolution studies are possible at high pressure and temperature within a transmission electron microscope (TEM). To achieve this goal, which avoids the crystallographic and chemical changes that can occur upon quenching, we use the unusual structural properties of carbon nanotubes (CNTs) and fullerenes. These carbon materials, which are used as sample containers, contract under radiation by energetic electrons at elevated temperatures in a TEM. The result is compression of materials that have been encapsulated within these containers. We estimated pressures greater than 20 GPa from the Fourier transforms of high-resolution images of oxide particles such as ZnO and Sm2O3 under compression within CNTs. Using an arc-discharge technique, we recently also loaded olivine into fullerenes. Such ability to compress and then examine minerals in situ at high resolution opens up new possibilities for the high-pressure research of minerals.

  3. Transmission of electrons through tapered glass capillaries: Temporal dependence

    NASA Astrophysics Data System (ADS)

    Wickramarachchi, S.; Keerthisinghe, D.; Tanis, J. A.; Ikeda, T.; Dassanayake, B. S.

    2014-05-01

    Electron transmission through a funnel-shaped borosilicate glass capillary as a function of the time evolution of the charge deposition has been studied for 500 and 1000 eV incident electrons. These measurements were done at Western Michigan University. The capillary had inlet/outlet diameters of 800 μm/100 μm and a length of 35 mm. The time dependence was studied for deposited charge in the range 0 - 1000 nC for each angle investigated, except for 5° at 1000 eV for which the measurements extended to 7000 nC. Measurements were obtained for the direct region near zero degree tilt angle where there are no collisions with the capillary walls, and for the indirect region for larger tilt angles (up to 5°) where electrons are deflected by the deposited charge or they collide with the capillary walls. In the direct region, the transmission showed no stable behavior with erratic fluctuations occurring for all deposited charges. In the indirect region, the transmission showed some fluctuations with rapid self-discharging but the transmission slowly increased with deposited charge. Total blocking was observed for 1000 eV at the tilt angle of 5° when the incident charge was higher than 6500 nC.

  4. Transmission electron microscopy investigation of auto catalyst and cobalt germanide

    NASA Astrophysics Data System (ADS)

    Sun, Haiping

    The modern ceria-zirconia based catalysts are used in automobiles to reduce exhaust pollutants. Cobalt germanides have potential applications as electrical contacts in the future Ge-based semiconductor devices. In this thesis, transmission electron microscopy (TEM) techniques were used to study the atomic scale interactions between metallic nanostructures and crystalline substrates in the two material systems mentioned above. The model catalyst samples consisted of precious metal nano-particles (Pd, Rh) supported on the surface of (Ce,Zr)O2 thin films. The response of the microstructure of the metal-oxide interface to the reduction and oxidation treatments was investigated by cross-sectional high resolution TEM. Atomic detail of the metal-oxide interface was obtained. It was found that Pd and Rh showed different sintering and interaction behaviors on the oxide surface. The preferred orientation of Pd particles in this study was Pd(111)//CZO(111). Partial encapsulation of Pd particles by reduced (Ce,Zr)O 2 surface was observed and possible mechanisms of the encapsulation were discussed. The characteristics of the metal-oxide interaction depend on the properties of the oxide, as well as their relative orientation. The results provide experimental evidence for understanding the thermodynamics of the equilibrium morphology of a solid particle supported on a solid surface that is not considered as inert. The reaction of Co with Ge to form epitaxial Co5Ge7 was studied by in situ ultra-high vacuum (UHV) TEM using two methods. One was reactive deposition of Co on Ge, in which the Ge substrate was maintained at 350°C during deposition. The other method was solid state reaction, in which the deposition of Co on Ge was carried out at room temperature followed by annealing to higher temperatures. During reactive deposition, the deposited Co reacted with Ge to form nanosized 3D Co 5Ge7 islands. During solid state reaction, a continuous epitaxial Co5Ge7 film on the (001) Ge

  5. High Speed, Radiation Hard CMOS Pixel Sensors for Transmission Electron Microscopy

    NASA Astrophysics Data System (ADS)

    Contarato, Devis; Denes, Peter; Doering, Dionisio; Joseph, John; Krieger, Brad

    CMOS monolithic active pixel sensors are currently being established as the technology of choice for new generation digital imaging systems in Transmission Electron Microscopy (TEM). A careful sensor design that couples μm-level pixel pitches with high frame rate readout and radiation hardness to very high electron doses enables the fabrication of direct electron detectors that are quickly revolutionizing high-resolution TEM imaging in material science and molecular biology. This paper will review the principal characteristics of this novel technology and its advantages over conventional, optically-coupled cameras, and retrace the sensor development driven by the Transmission Electron Aberration corrected Microscope (TEAM) project at the LBNL National Center for Electron Microscopy (NCEM), illustrating in particular the imaging capabilities enabled by single electron detection at high frame rate. Further, the presentation will report on the translation of the TEAM technology to a finer feature size process, resulting in a sensor with higher spatial resolution and superior radiation tolerance currently serving as the baseline for a commercial camera system.

  6. Prospects for Electron Imaging with Ultrafast Time Resolution

    SciTech Connect

    Armstrong, M R; Reed, B W; Torralva, B R; Browning, N D

    2007-01-26

    Many pivotal aspects of material science, biomechanics, and chemistry would benefit from nanometer imaging with ultrafast time resolution. Here we demonstrate the feasibility of short-pulse electron imaging with t10 nanometer/10 picosecond spatio-temporal resolution, sufficient to characterize phenomena that propagate at the speed of sound in materials (1-10 kilometer/second) without smearing. We outline resolution-degrading effects that occur at high current density followed by strategies to mitigate these effects. Finally, we present a model electron imaging system that achieves 10 nanometer/10 picosecond spatio-temporal resolution.

  7. Concurrent in situ ion irradiation transmission electron microscope

    SciTech Connect

    Hattar, K.; Bufford, D. C.; Buller, D. L.

    2014-08-29

    An in situ ion irradiation transmission electron microscope has been developed and is operational at Sandia National Laboratories. This facility permits high spatial resolution, real time observation of electron transparent samples under ion irradiation, implantation, mechanical loading, corrosive environments, and combinations thereof. This includes the simultaneous implantation of low-energy gas ions (0.8–30 keV) during high-energy heavy ion irradiation (0.8–48 MeV). In addition, initial results in polycrystalline gold foils are provided to demonstrate the range of capabilities.

  8. Reliable strain measurement in transistor arrays by robust scanning transmission electron microscopy

    SciTech Connect

    Kim, Suhyun; Kim, Joong Jung; Jung, Younheum; Lee, Kyungwoo; Byun, Gwangsun; Hwang, KyoungHwan; Lee, Sunyoung; Lee, Kyupil

    2013-09-15

    Accurate measurement of the strain field in the channels of transistor arrays is critical for strain engineering in modern electronic devices. We applied atomic-resolution high-angle annular dark-field scanning transmission electron microscopy to quantitative measurement of the strain field in transistor arrays. The quantitative strain profile over 20 transistors was obtained with high reliability and a precision of 0.1%. The strain field was found to form homogeneously in the channels of the transistor arrays. Furthermore, strain relaxation due to the thin foil effect was quantitatively investigated for thicknesses of 35 to 275 nm.

  9. In situ probing electrical response on bending of ZnO nanowires inside transmission electron microscope

    NASA Astrophysics Data System (ADS)

    Liu, K. H.; Gao, P.; Xu, Z.; Bai, X. D.; Wang, E. G.

    2008-05-01

    In situ electrical transport measurements on individual bent ZnO nanowires have been performed inside a high-resolution transmission electron microscope, where the crystal structures of ZnO nanowires were simultaneously imaged. A series of consecutively recorded current-voltage (I-V) curves along with an increase in nanowire bending show the striking effect of bending on their electrical behavior. The bending-induced changes of resistivity, electron concentration, and carrier mobility of ZnO nanowires have been retrieved based on the experimental I-V data, which suggests the applications of ZnO nanowires as nanoelectromechanical sensors.

  10. Secondary electron imaging of monolayer materials inside a transmission electron microscope

    SciTech Connect

    Cretu, Ovidiu Lin, Yung-Chang; Suenaga, Kazutomo

    2015-08-10

    A scanning transmission electron microscope equipped with a backscattered and secondary electron detector is shown capable to image graphene and hexagonal boron nitride monolayers. Secondary electron contrasts of the two lightest monolayer materials are clearly distinguished from the vacuum level. A signal difference between these two materials is attributed to electronic structure differences, which will influence the escape probabilities of the secondary electrons. Our results show that the secondary electron signal can be used to distinguish between the electronic structures of materials with atomic layer sensitivity, enhancing its applicability as a complementary signal in the analytical microscope.

  11. Transmission of High-Power Electron Beams Through Small Apertures

    SciTech Connect

    Tschalaer, Christoph; Alarcon, Ricardo O.; Balascuta, S.; Benson, Stephen V.; Bertozzi, William; Boyce, James R.; Cowan, Ray Franklin; Douglas, David R.; Evtushenko, Pavel; Fisher, Peter H.; Ihloff, Ernest E.; Kalantarians, Narbe; Kelleher, Aidan Michael; Legg, Robert A.; Milner, Richard; Neil, George R.; Ou, Longwu; Schmookler, Barak Abraham; Tennant, Christopher D.; Williams, Gwyn P.; Zhang, Shukui

    2013-11-01

    Tests were performed to pass a 100 MeV, 430 kWatt c.w. electron beam from the energy-recovery linac at the Jefferson Laboratory's FEL facility through a set of small apertures in a 127 mm long aluminum block. Beam transmission losses of 3 p.p.m. through a 2 mm diameter aperture were maintained during a 7 hour continuous run.

  12. High Brightness and high polarization electron source using transmission photocathode

    SciTech Connect

    Yamamoto, Naoto; Jin Xiuguang; Ujihara, Toru; Takeda, Yoshikazu; Mano, Atsushi; Nakagawa, Yasuhide; Nakanishi, Tsutomu; Okumi, Shoji; Yamamoto, Masahiro; Konomi, Taro; Ohshima, Takashi; Saka, Takashi; Kato, Toshihiro; Horinaka, Hiromichi; Yasue, Tsuneo; Koshikawa, Takanori

    2009-08-04

    A transmission photocathode was fabricated based on GaAs-GaAsP strained superlattice layers on a GaP substrate and a 20 kV-gun was built to generate the polarized electron beams with the diameter of a few micro-meter. As the results, the reduced brightness of 1.3x10{sup 7} A/cm{sup 2}/sr and the polarization of 90% were achieved.

  13. Practical aspects of monochromators developed for transmission electron microscopy

    PubMed Central

    Kimoto, Koji

    2014-01-01

    A few practical aspects of monochromators recently developed for transmission electron microscopy are briefly reviewed. The basic structures and properties of four monochromators, a single Wien filter monochromator, a double Wien filter monochromator, an omega-shaped electrostatic monochromator and an alpha-shaped magnetic monochromator, are outlined. The advantages and side effects of these monochromators in spectroscopy and imaging are pointed out. A few properties of the monochromators in imaging, such as spatial or angular chromaticity, are also discussed. PMID:25125333

  14. Studying localized corrosion using liquid cell transmission electron microscopy

    SciTech Connect

    Chee, See Wee; Pratt, Sarah H.; Hattar, Khalid; Duquette, David; Ross, Frances M.; Hull, Robert

    2014-11-07

    Using liquid cell transmission electron microscopy (LCTEM), localized corrosion of Cu and Al thin films immersed in aqueous NaCl solutions was studied. We demonstrate that potentiostatic control can be used to initiate pitting and that local compositional changes, due to focused ion beam implantation of Au+ ions, can modify the corrosion susceptibility of Al films. Likewise, a discussion on strategies to control the onset of pitting is also presented.

  15. 8 CFR 217.7 - Electronic data transmission requirement.

    Code of Federal Regulations, 2011 CFR

    2011-01-01

    ... manifest data relative to that alien passenger in accordance with 19 CFR 4.7b or 19 CFR 122.49a. Upon... relative to that alien passenger in accordance with 19 CFR 4.64 and 19 CFR 122.75a. (b) If a carrier fails... 8 Aliens and Nationality 1 2011-01-01 2011-01-01 false Electronic data transmission...

  16. 8 CFR 217.7 - Electronic data transmission requirement.

    Code of Federal Regulations, 2013 CFR

    2013-01-01

    ... manifest data relative to that alien passenger in accordance with 19 CFR 4.7b or 19 CFR 122.49a. Upon... relative to that alien passenger in accordance with 19 CFR 4.64 and 19 CFR 122.75a. (b) If a carrier fails... 8 Aliens and Nationality 1 2013-01-01 2013-01-01 false Electronic data transmission...

  17. 8 CFR 217.7 - Electronic data transmission requirement.

    Code of Federal Regulations, 2014 CFR

    2014-01-01

    ... manifest data relative to that alien passenger in accordance with 19 CFR 4.7b or 19 CFR 122.49a. Upon... relative to that alien passenger in accordance with 19 CFR 4.64 and 19 CFR 122.75a. (b) If a carrier fails... 8 Aliens and Nationality 1 2014-01-01 2014-01-01 false Electronic data transmission...

  18. 8 CFR 217.7 - Electronic data transmission requirement.

    Code of Federal Regulations, 2012 CFR

    2012-01-01

    ... manifest data relative to that alien passenger in accordance with 19 CFR 4.7b or 19 CFR 122.49a. Upon... relative to that alien passenger in accordance with 19 CFR 4.64 and 19 CFR 122.75a. (b) If a carrier fails... 8 Aliens and Nationality 1 2012-01-01 2012-01-01 false Electronic data transmission...

  19. 8 CFR 217.7 - Electronic data transmission requirement.

    Code of Federal Regulations, 2010 CFR

    2010-01-01

    ... manifest data relative to that alien passenger in accordance with 19 CFR 4.7b or 19 CFR 122.49a. Upon... relative to that alien passenger in accordance with 19 CFR 4.64 and 19 CFR 122.75a. (b) If a carrier fails... 8 Aliens and Nationality 1 2010-01-01 2010-01-01 false Electronic data transmission...

  20. Studying localized corrosion using liquid cell transmission electron microscopy

    DOE PAGESBeta

    Chee, See Wee; Pratt, Sarah H.; Hattar, Khalid; Duquette, David; Ross, Frances M.; Hull, Robert

    2014-11-07

    Using liquid cell transmission electron microscopy (LCTEM), localized corrosion of Cu and Al thin films immersed in aqueous NaCl solutions was studied. We demonstrate that potentiostatic control can be used to initiate pitting and that local compositional changes, due to focused ion beam implantation of Au+ ions, can modify the corrosion susceptibility of Al films. Likewise, a discussion on strategies to control the onset of pitting is also presented.

  1. Field mapping with nanometer-scale resolution for the next generation of electronic devices.

    PubMed

    Cooper, David; de la Peña, Francisco; Béché, Armand; Rouvière, Jean-Luc; Servanton, Germain; Pantel, Roland; Morin, Pierre

    2011-11-01

    In order to improve the performance of today's nanoscaled semiconductor devices, characterization techniques that can provide information about the position and activity of dopant atoms and the strain fields are essential. Here we demonstrate that by using a modern transmission electron microscope it is possible to apply multiple techniques to advanced materials systems in order to provide information about the structure, fields, and composition with nanometer-scale resolution. Off-axis electron holography has been used to map the active dopant potentials in state-of-the-art semiconductor devices with 1 nm resolution. These dopant maps have been compared to electron energy loss spectroscopy maps that show the positions of the dopant atoms. The strain fields in the devices have been measured by both dark field electron holography and nanobeam electron diffraction. PMID:21972919

  2. Transmission electron microscopy of a model crystalline organic, theophylline

    NASA Astrophysics Data System (ADS)

    Cattle, J.; S'ari, M.; Hondow, N.; Abellán, P.; Brown, A. P.; Brydson, R. M. D.

    2015-10-01

    We report on the use of transmission electron microscopy (TEM) to analyse the diffraction patterns of the model crystalline organic theophylline to investigate beam damage in relation to changing accelerating voltage, sample temperature and TEM grid support films. We find that samples deposited on graphene film grids have the longest lifetimes when also held at -190 °C and imaged at 200 kV accelerating voltage. Finally, atomic lattice images are obtained in bright field STEM by working close to the estimated critical electron dose for theophylline.

  3. Transmission Electron Microscopy Study of InN Nanorods

    SciTech Connect

    Liliental-Weber, Z.; Li, X.; Kryliouk, Olga; Park, H.J.; Mangum,J.; Anderson, T.

    2006-07-13

    InN nanorods were grown on a, c-, and r-plane of sapphire and also on Si (111) and GaN (0001) by non-catalytic, template-free hydride metal-organic vapor phase epitaxy and studied by transmission electron microscopy, electron energy loss (EELS) and photoluminescence (PL) at room temperature. These nanocrystals have different shapes and different faceting depending on the substrate used and their crystallographic orientation. EELS measurements have confirmed the high purity of these crystals. The observed PL peak was in the range of 0.9-0.95 eV. The strongest PL intensity was observed for the nanocrystals with the larger diameters.

  4. High resolution transmission spectroscopy as a diagnostic for Jovian exoplanet atmospheres: constraints from theoretical models

    SciTech Connect

    Kempton, Eliza M.-R.; Perna, Rosalba; Heng, Kevin

    2014-11-01

    We present high resolution transmission spectra of giant planet atmospheres from a coupled three-dimensional (3D) atmospheric dynamics and transmission spectrum model that includes Doppler shifts which arise from winds and planetary motion. We model Jovian planets covering more than two orders of magnitude in incident flux, corresponding to planets with 0.9-55 day orbital periods around solar-type stars. The results of our 3D dynamical models reveal certain aspects of high resolution transmission spectra that are not present in simple one-dimensional (1D) models. We find that the hottest planets experience strong substellar to anti-stellar (SSAS) winds, resulting in transmission spectra with net blueshifts of up to 3 km s{sup –1}, whereas less irradiated planets show almost no net Doppler shifts. We find only minor differences between transmission spectra for atmospheres with temperature inversions and those without. Compared to 1D models, peak line strengths are significantly reduced for the hottest atmospheres owing to Doppler broadening from a combination of rotation (which is faster for close-in planets under the assumption of tidal locking) and atmospheric winds. Finally, high resolution transmission spectra may be useful in studying the atmospheres of exoplanets with optically thick clouds since line cores for very strong transitions should remain optically thick to very high altitude. High resolution transmission spectra are an excellent observational test for the validity of 3D atmospheric dynamics models, because they provide a direct probe of wind structures and heat circulation. Ground-based exoplanet spectroscopy is currently on the verge of being able to verify some of our modeling predictions, most notably the dependence of SSAS winds on insolation. We caution that interpretation of high resolution transmission spectra based on 1D atmospheric models may be inadequate, as 3D atmospheric motions can produce a noticeable effect on the absorption

  5. High Resolution Transmission Spectroscopy as a Diagnostic for Jovian Exoplanet Atmospheres: Constraints from Theoretical Models

    NASA Astrophysics Data System (ADS)

    Kempton, Eliza M.-R.; Perna, Rosalba; Heng, Kevin

    2014-11-01

    We present high resolution transmission spectra of giant planet atmospheres from a coupled three-dimensional (3D) atmospheric dynamics and transmission spectrum model that includes Doppler shifts which arise from winds and planetary motion. We model Jovian planets covering more than two orders of magnitude in incident flux, corresponding to planets with 0.9-55 day orbital periods around solar-type stars. The results of our 3D dynamical models reveal certain aspects of high resolution transmission spectra that are not present in simple one-dimensional (1D) models. We find that the hottest planets experience strong substellar to anti-stellar (SSAS) winds, resulting in transmission spectra with net blueshifts of up to 3 km s-1, whereas less irradiated planets show almost no net Doppler shifts. We find only minor differences between transmission spectra for atmospheres with temperature inversions and those without. Compared to 1D models, peak line strengths are significantly reduced for the hottest atmospheres owing to Doppler broadening from a combination of rotation (which is faster for close-in planets under the assumption of tidal locking) and atmospheric winds. Finally, high resolution transmission spectra may be useful in studying the atmospheres of exoplanets with optically thick clouds since line cores for very strong transitions should remain optically thick to very high altitude. High resolution transmission spectra are an excellent observational test for the validity of 3D atmospheric dynamics models, because they provide a direct probe of wind structures and heat circulation. Ground-based exoplanet spectroscopy is currently on the verge of being able to verify some of our modeling predictions, most notably the dependence of SSAS winds on insolation. We caution that interpretation of high resolution transmission spectra based on 1D atmospheric models may be inadequate, as 3D atmospheric motions can produce a noticeable effect on the absorption signatures.

  6. Dielectric metasurfaces for complete control of phase and polarization with subwavelength spatial resolution and high transmission.

    PubMed

    Arbabi, Amir; Horie, Yu; Bagheri, Mahmood; Faraon, Andrei

    2015-11-01

    Metasurfaces are planar structures that locally modify the polarization, phase and amplitude of light in reflection or transmission, thus enabling lithographically patterned flat optical components with functionalities controlled by design. Transmissive metasurfaces are especially important, as most optical systems used in practice operate in transmission. Several types of transmissive metasurface have been realized, but with either low transmission efficiencies or limited control over polarization and phase. Here, we show a metasurface platform based on high-contrast dielectric elliptical nanoposts that provides complete control of polarization and phase with subwavelength spatial resolution and an experimentally measured efficiency ranging from 72% to 97%, depending on the exact design. Such complete control enables the realization of most free-space transmissive optical elements such as lenses, phase plates, wave plates, polarizers, beamsplitters, as well as polarization-switchable phase holograms and arbitrary vector beam generators using the same metamaterial platform. PMID:26322944

  7. Sub-Angstrom Low Voltage Performance of a Monochromated, Aberration-Corrected Transmission Electron Microscope

    PubMed Central

    Bell, David C.; Russo, Christopher J.; Benner, Gerd

    2011-01-01

    Lowering the electron energy in the transmission electron microscope allows for a significant improvement in contrast of light elements, and reduces knock-on damage for most materials. If low-voltage electron microscopes are defined as those with accelerating voltages below 100 kV, the introduction of aberration correctors and monochromators to the electron microscope column enables Ångstrom-level resolution, which was previously reserved for higher voltage instruments. Decreasing electron energy has three important advantages: 1) knock-on damage is lower, which is critically important for sensitive materials such as graphene and carbon nanotubes; 2) cross sections for electron-energy-loss spectroscopy increase, improving signal-to-noise for chemical analysis; 3) elastic scattering cross sections increase, improving contrast in high-resolution, zero-loss images. The results presented indicate that decreasing the acceleration voltage from 200 kV to 80 kV in a monochromated, aberration-corrected microscope enhances the contrast while retaining sub-angstrom resolution. These improvements in low-voltage performance are expected to produce many new results and enable a wealth of new experiments in materials science. PMID:20598206

  8. Tailoring of electron flow current in magnetically insulated transmission lines

    NASA Astrophysics Data System (ADS)

    Martin, J. P.; Savage, M. E.; Pointon, T. D.; Gilmore, M. A.

    2009-03-01

    It is desirable to optimize (minimizing both the inductance and electron flow) the magnetically insulated vacuum sections of low impedance pulsed-power drivers. The goal of low inductance is understandable from basic efficiency arguments. The goal of low electron flow results from two observations: (1) flowing electrons generally do not deliver energy to (or even reach) most loads, and thus constitute a loss mechanism; (2) energetic electrons deposited in a small area can cause anode damage and anode plasma formation. Low inductance and low electron flow are competing goals; an optimized system requires a balance of the two. While magnetically insulated systems are generally forgiving, there are times when optimization is crucial. For example, in large pulsed-power drivers used to energize high energy density physics loads, the electron flow as a fraction of total current is small, but that flow often reaches the anode in relatively small regions. If the anode temperature becomes high enough to desorb gas, the resulting plasma initiates a gap closure process that can impact system performance. Magnetic-pressure driven (z pinches and material equation of state) loads behave like a fixed inductor for much of the drive pulse. It is clear that neither fixed gap nor constant-impedance transmission lines are optimal for driving inductive loads. This work shows a technique for developing the optimal impedance profile for the magnetically insulated section of a high-current driver. Particle-in-cell calculations are used to validate the impedance profiles developed in a radial disk magnetically insulated transmission line geometry. The input parameters are the spacing and location of the minimum gap, the effective load inductance, and the desired electron flow profile. The radial electron flow profiles from these simulations are in good agreement with theoretical predictions when driven at relatively high voltage (i.e., V≥2MV).

  9. Precision electron flow measurements in a disk transmission line.

    SciTech Connect

    Clark, Waylon T.; Pelock, Michael D.; Martin, Jeremy Paul; Jackson, Daniel Peter Jr.; Savage, Mark Edward; Stoltzfus, Brian Scott; Mendel, Clifford Will, Jr.; Pointon, Timothy David

    2008-01-01

    An analytic model for electron flow in a system driving a fixed inductive load is described and evaluated with particle in cell simulations. The simple model allows determining the impedance profile for a magnetically insulated transmission line given the minimum gap desired, and the lumped inductance inside the transition to the minimum gap. The model allows specifying the relative electron flow along the power flow direction, including cases where the fractional electron flow decreases in the power flow direction. The electrons are able to return to the cathode because they gain energy from the temporally rising magnetic field. The simulations were done with small cell size to reduce numerical heating. An experiment to compare electron flow to the simulations was done. The measured electron flow is {approx}33% of the value from the simulations. The discrepancy is assumed to be due to a reversed electric field at the cathode because of the inductive load and falling electron drift velocity in the power flow direction. The simulations constrain the cathode electric field to zero, which gives the highest possible electron flow.

  10. Analysis of Electron Beam Damage of Crystalline Pharmaceutical Materials by Transmission Electron Microscopy

    NASA Astrophysics Data System (ADS)

    S'ari, M.; Cattle, J.; Hondow, N.; Blade, H.; Cosgrove, S.; Brydson, R. M.; Brown, A. P.

    2015-10-01

    We have studied the impact of transmission electron microscopy (TEM) and low dose electron diffraction on ten different crystalline pharmaceutical compounds, covering a diverse chemical space and with differing physical properties. The aim was to establish if particular chemical moieties were more susceptible to damage within the electron beam. We have measured crystalline diffraction patterns for each and indexed nine out of ten of them. Characteristic electron dosages are reported for each material, with no apparent correlation between chemical structure and stability within the electron beam. Such low dose electron diffraction protocols are suitable for the study of pharmaceutical compounds.

  11. Recent developments of the in situ wet cell technology for transmission electron microscopies

    NASA Astrophysics Data System (ADS)

    Chen, Xin; Li, Chang; Cao, Hongling

    2015-03-01

    In situ wet cells for transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM) allow studying structures and processes in a liquid environment with high temporal and spatial resolutions, and have been attracting increasing research interests in many fields. In this review, we highlight the structural and functional developments of the wet cells for TEM and STEM. One of the key features of the wet cells is the sealing technique used to isolate the liquid sample from the TEM/STEM vacuum environments, thus the existing in situ wet cells are grouped by different sealing methods. In this study, the advantages and shortcomings of each type of in situ wet cells are discussed, the functional developments of different wet cells are presented, and the future trends of the wet cell technology are addressed. It is suggested that in the future the in situ wet cell TEM/STEM technology will have an increasing impact on frontier nanoscale research.

  12. The vacuum geometry effect on neutron transmission and spatial resolution of neutron transmission.

    PubMed

    Khanouchi, A; Sabir, A; Boulkheir, M; Ichaoui, R; Ghassoun, J; Jehouani, A

    1997-01-01

    Frequently, shields used against radiation contain some vacuum channels. We have therefore considered an infinite slab with a fixed thickness (thickness 20 lambda with lambda the mean free path of the neutron in the slab) and an infinite plane source of neutrons which arrived on the left side of the slab; transmitted neutrons through the slab to its right side are detected by finite detectors having windows equal to 2 lambda. This slab contains a vacuum channel. This channel has many legs with several horizontal parts. We used the Monte Carlo method for sampling the neutron history in the slab with a spatial biasing technique in order to accelerate the calculation convergence (Levitt, L. B. (1968) Nuclear Science and Engineering 31, 500-504; Jehouani, A., Ghassoun, J. and Aboubker, A. (1994) In Proceedings of 6th International Symposium on Radiation Physics, Rabat, Morocco). We studied the effects of the angle position and the number of horizontal parts of the channel on the neutron transmission. We have studied the effect of the vacuum channel opening (Artigas, R. and Hungerford, H. E. (1969) Nuclear Science and Engineering 36, 295-303) on the neutron transmission; for several values of this opening we have calculated the neutron transmission probability for each detector position. This study allowed us to determine the optimal conditions of vacuum geometries to improve protection against neutrons. In the second part we considered a shield which consists of a slab and a two-legged vacuum channel with two horizontal parts. The spatial distribution of neutrons transmitted through the protection screen was determined. This distribution shows two peaks. The study was made for different distances between the two horizontal parts. We have determined the smallest distance between the two horizontal parts for which the two peaks can be resolved. PMID:9463882

  13. Conventional transmission electron microscopy imaging beyond the diffraction and information limits.

    PubMed

    Rosenauer, Andreas; Krause, Florian F; Müller, Knut; Schowalter, Marco; Mehrtens, Thorsten

    2014-08-29

    There are mainly two complementary imaging modes in transmission electron microscopy (TEM): Conventional TEM (CTEM) and scanning TEM (STEM). In the CTEM mode the specimen is illuminated with a plane electron wave, and the direct image formed by the objective lens is recorded in the image plane. STEM is based on scanning the specimen surface with a focused electron beam and collecting scattered electrons with an extended disk or ring-shaped detector. Here we show that combination of CTEM imaging with STEM illumination generally allows extending the point resolution of CTEM imaging beyond the diffraction limit. This new imaging mode improves imaging characteristics, is more robust against chromatic aberration, exhibits direct structural imaging with superior precision, visualizes light elements with excellent contrast, and even allows us to overcome the conventional information limit of a microscope. PMID:25215995

  14. Few-layer graphene as a support film for transmission electron microscopy imaging of nanoparticles.

    PubMed

    McBride, James R; Lupini, Andrew R; Schreuder, Michael A; Smith, Nathanael J; Pennycook, Stephen J; Rosenthal, Sandra J

    2009-12-01

    One consistent limitation for high-resolution imaging of small nanoparticles is the high background signal from the amorphous carbon support film. With interest growing for smaller and smaller nanostructures, state of the art electron microscopes are becoming necessary for rudimentary tasks, such as nanoparticle sizing. As a monolayer of carbon, free-standing graphene represents the ultimate support film for nanoparticle imaging. In this work, conventional high-resolution transmission electron microscopy (HRTEM) and aberration-corrected scanning transmission electron microscopy (STEM) were used to assess the benefits and feasibility of few-layer graphene support films. Suspensions of few-layer graphene to produce the support films were prepared by simple sonication of exfoliated graphite. The greatest benefit was observed for conventional HRTEM, where lattice resolved imaging of sub 2 nm CdSe nanocrystals was achieved. The few-layer graphene films were also used as a support film for C(s)-corrected STEM and electron energy loss spectroscopy of CuInSe(2) nanocrystals. PMID:20356171

  15. In-situ electrochemical transmission electron microscopy for battery research.

    PubMed

    Mehdi, B Layla; Gu, Meng; Parent, Lucas R; Xu, Wu; Nasybulin, Eduard N; Chen, Xilin; Unocic, Raymond R; Xu, Pinghong; Welch, David A; Abellan, Patricia; Zhang, Ji-Guang; Liu, Jun; Wang, Chong-Min; Arslan, Ilke; Evans, James; Browning, Nigel D

    2014-04-01

    The recent development of in-situ liquid stages for (scanning) transmission electron microscopes now makes it possible for us to study the details of electrochemical processes under operando conditions. As electrochemical processes are complex, care must be taken to calibrate the system before any in-situ/operando observations. In addition, as the electron beam can cause effects that look similar to electrochemical processes at the electrolyte/electrode interface, an understanding of the role of the electron beam in modifying the operando observations must also be understood. In this paper we describe the design, assembly, and operation of an in-situ electrochemical cell, paying particular attention to the method for controlling and quantifying the experimental parameters. The use of this system is then demonstrated for the lithiation/delithiation of silicon nanowires. PMID:24755142

  16. Effects of instrument imperfections on quantitative scanning transmission electron microscopy.

    PubMed

    Krause, Florian F; Schowalter, Marco; Grieb, Tim; Müller-Caspary, Knut; Mehrtens, Thorsten; Rosenauer, Andreas

    2016-02-01

    Several instrumental imperfections of transmission electron microscopes are characterized and their effects on the results of quantitative scanning electron microscopy (STEM) are investigated and quantified using simulations. Methods to either avoid influences of these imperfections during acquisition or to include them in reference calculations are proposed. Particularly, distortions inflicted on the diffraction pattern by an image-aberration corrector can cause severe errors of more than 20% if not accounted for. A procedure for their measurement is proposed here. Furthermore, afterglow phenomena and nonlinear behavior of the detector itself can lead to incorrect normalization of measured intensities. Single electrons accidentally impinging on the detector are another source of error but can also be exploited for threshold-less calibration of STEM images to absolute dose, incident beam current determination and measurement of the detector sensitivity. PMID:26686661

  17. Transmission electron microscopic examination of phosphoric acid fuel cell components

    NASA Technical Reports Server (NTRS)

    Pebler, A.

    1986-01-01

    Transmission electron microscopy (TEM) was used to physically characterize tested and untested phosphoric acid fuel cell (PAFC) components. Those examined included carbon-supported platinum catalysts, carbon backing paper, and Teflon-bonded catalyst layers at various stages of fabrication and after testing in pressurized PAFC's. Applicability of electron diffraction and electron energy loss spectroscopy for identifying the various phases was explored. The discussion focuses on the morphology and size distribution of platinum, the morphology and structural aspects of Teflon in catalyst layers, and the structural evidence of carbon corrosion. Reference is made to other physical characterization techniques where appropriate. A qualitative model of the catalyst layer that emerged from the TEM studies is presented.

  18. In-Situ Electrochemical Transmission Electron Microscopy for Battery Research

    SciTech Connect

    Mehdi, Beata L; Gu, Meng; Parent, Lucas; Xu, WU; Nasybulin, Eduard; Chen, Xilin; Unocic, Raymond R; Xu, Pinghong; Welch, David; Abellan, Patricia; Zhang, Ji-Guang; Liu, Jun; Wang, Chongmin; Arslan, Ilke; Evans, James E; Browning, Nigel

    2014-01-01

    The recent development of in-situ liquid stages for (scanning) transmission electron microscopes now makes it possible for us to study the details of electrochemical processes under operando conditions. As electrochemical processes are complex, care must be taken to calibrate the system before any in-situ/operando observations. In addition, as the electron beam can cause effects that look similar to electrochemical processes at the electrolyte/electrode interface, an understanding of the role of the electron beam in modifying the operando observations must also be understood. In this paper we describe the design, assembly, and operation of an in-situ electrochemical cell, paying particular attention to the method for controlling and quantifying the experimental parameters. The use of this system is then demonstrated for the lithiation/delithiation of silicon nanowires.

  19. In Situ Electrochemical Transmission Electron Microscopy for Battery Research

    SciTech Connect

    Mehdi, Beata L.; Gu, Meng; Parent, Lucas R.; Xu, Wu; Nasybulin, Eduard N.; Chen, Xilin; Unocic, Raymond R.; Xu, Pinghong; Welch, David A.; Abellan, Patricia; Zhang, Jiguang; Liu, Jun; Wang, Chong M.; Arslan, Ilke; Evans, James E.; Browning, Nigel D.

    2014-04-01

    The recent development of in situ liquid stages for (scanning) transmission electron microscopes now makes it possible for us to study the details of electrochemical processes under operando conditions. As electrochemical processes are complex, care must be taken to calibrate the system before any in situ/operando observations. In addition, as the electron beam can cause effects that look similar to electrochemical processes at the electrolyte/electrode interface, an understanding of the role of the electron beam in modifying the operando observations must also be understood. In this paper we describe the design, assembly, and operation of an in situ electrochemical cell, paying particular attention to the method for controlling and quantifying the experimental parameters. The use of this system is then demonstrated for the lithiation/delithiation of silicon nanowires.

  20. Accurate Nanoscale Crystallography in Real-Space Using Scanning Transmission Electron Microscopy.

    PubMed

    Dycus, J Houston; Harris, Joshua S; Sang, Xiahan; Fancher, Chris M; Findlay, Scott D; Oni, Adedapo A; Chan, Tsung-Ta E; Koch, Carl C; Jones, Jacob L; Allen, Leslie J; Irving, Douglas L; LeBeau, James M

    2015-08-01

    Here, we report reproducible and accurate measurement of crystallographic parameters using scanning transmission electron microscopy. This is made possible by removing drift and residual scan distortion. We demonstrate real-space lattice parameter measurements with <0.1% error for complex-layered chalcogenides Bi2Te3, Bi2Se3, and a Bi2Te2.7Se0.3 nanostructured alloy. Pairing the technique with atomic resolution spectroscopy, we connect local structure with chemistry and bonding. Combining these results with density functional theory, we show that the incorporation of Se into Bi2Te3 causes charge redistribution that anomalously increases the van der Waals gap between building blocks of the layered structure. The results show that atomic resolution imaging with electrons can accurately and robustly quantify crystallography at the nanoscale. PMID:26169835

  1. Transfer-printing of single DNA molecule arrays on graphene for high resolution electron imaging and analysis

    PubMed Central

    Cerf, Aline; Alava, Thomas; Barton, Robert A.; Craighead, Harold G.

    2011-01-01

    Graphene represents the ultimate substrate for high-resolution transmission electron microscopy, but the deposition of biological samples on this highly hydrophobic material has until now been a challenge. We present a reliable method for depositing ordered arrays of individual elongated DNA molecules on single-layer graphene substrates for high resolution electron beam imaging and electron energy loss spectroscopy analysis. This method is a necessary step towards the observation of single elongated DNA molecules with single base spatial resolution to directly read genetic and epigenetic information. PMID:21919532

  2. Formation of bimetallic clusters in superfluid helium nanodroplets analysed by atomic resolution electron tomography

    PubMed Central

    Haberfehlner, Georg; Thaler, Philipp; Knez, Daniel; Volk, Alexander; Hofer, Ferdinand; Ernst, Wolfgang E.; Kothleitner, Gerald

    2015-01-01

    Structure, shape and composition are the basic parameters responsible for properties of nanoscale materials, distinguishing them from their bulk counterparts. To reveal these in three dimensions at the nanoscale, electron tomography is a powerful tool. Advancing electron tomography to atomic resolution in an aberration-corrected transmission electron microscope remains challenging and has been demonstrated only a few times using strong constraints or extensive filtering. Here we demonstrate atomic resolution electron tomography on silver/gold core/shell nanoclusters grown in superfluid helium nanodroplets. We reveal morphology and composition of a cluster identifying gold- and silver-rich regions in three dimensions and we estimate atomic positions without using any prior information and with minimal filtering. The ability to get full three-dimensional information down to the atomic scale allows understanding the growth and deposition process of the nanoclusters and demonstrates an approach that may be generally applicable to all types of nanoscale materials. PMID:26508471

  3. Problem Resolution through Electronic Mail: A Five-Step Model.

    ERIC Educational Resources Information Center

    Grandgenett, Neal; Grandgenett, Don

    2001-01-01

    Discusses the use of electronic mail within the general resolution and management of administrative problems and emphasizes the need for careful attention to problem definition and clarity of language. Presents a research-based five-step model for the effective use of electronic mail based on experiences at the University of Nebraska at Omaha.…

  4. Addressing preservation of elastic contrast in energy-filtered transmission electron microscopy.

    PubMed

    Brown, H G; D'Alfonso, A J; Forbes, B D; Allen, L J

    2016-01-01

    Energy-filtered transmission electron microscopy (EFTEM) images with resolutions of the order of an Ångström can be obtained using modern microscopes corrected for chromatic aberration. However, the delocalized nature of the transition potentials for atomic ionization often confounds direct interpretation of EFTEM images, leading to what is known as "preservation of elastic contrast". In this paper we demonstrate how more interpretable images might be obtained by scanning with a focused coherent probe and incoherently averaging the energy-filtered images over probe position. We dub this new imaging technique energy-filtered imaging scanning transmission electron microscopy (EFISTEM). We develop a theoretical framework for EFISTEM and show that it is in fact equivalent to precession EFTEM, where the plane wave illumination is precessed through a range of tilts spanning the same range of angles as the probe forming aperture in EFISTEM. It is demonstrated that EFISTEM delivers similar results to scanning transmission electron microscopy with an electron energy-loss spectrometer but has the advantage that it is immune to coherent aberrations and spatial incoherence of the probe and is also more resilient to scan distortions. PMID:26476801

  5. A scanning transmission electron microscopy study of two dental amalgams.

    PubMed

    Williams, K R

    1983-10-01

    Two fully aged amalgam alloys were examined using a scanning transmission electron microscope both in the transmission and scanning mode. The dispersed type amalgam containing a distribution of silver-copper spheres in addition to the Ag3Sn powder showed a markedly reduced gamma 1 grain size compared to a conventional Ag3Sn type amalgam. It is suggested that the increased compressive creep strength of the dispersed type material is a direct result of the reduced gamma 1 grain size and not due to a dispersion hardening effect from the cores of the remaining Ag-Cu spheres. Similarly, the formation of complex Cu-Sn intermediate phases at the Ag-Cu sphere surfaces are unlikely to lead to a dispersion strengthening effect. It is postulated that the reduced grain size in high copper amalgams is a consequence of the enhanced nucleating effect of a copper based phase on gamma 1. PMID:6640049

  6. Nanocrystal size distribution analysis from transmission electron microscopy images

    NASA Astrophysics Data System (ADS)

    van Sebille, Martijn; van der Maaten, Laurens J. P.; Xie, Ling; Jarolimek, Karol; Santbergen, Rudi; van Swaaij, René A. C. M. M.; Leifer, Klaus; Zeman, Miro

    2015-12-01

    We propose a method, with minimal bias caused by user input, to quickly detect and measure the nanocrystal size distribution from transmission electron microscopy (TEM) images using a combination of Laplacian of Gaussian filters and non-maximum suppression. We demonstrate the proposed method on bright-field TEM images of an a-SiC:H sample containing embedded silicon nanocrystals with varying magnifications and we compare the accuracy and speed with size distributions obtained by manual measurements, a thresholding method and PEBBLES. Finally, we analytically consider the error induced by slicing nanocrystals during TEM sample preparation on the measured nanocrystal size distribution and formulate an equation to correct this effect.We propose a method, with minimal bias caused by user input, to quickly detect and measure the nanocrystal size distribution from transmission electron microscopy (TEM) images using a combination of Laplacian of Gaussian filters and non-maximum suppression. We demonstrate the proposed method on bright-field TEM images of an a-SiC:H sample containing embedded silicon nanocrystals with varying magnifications and we compare the accuracy and speed with size distributions obtained by manual measurements, a thresholding method and PEBBLES. Finally, we analytically consider the error induced by slicing nanocrystals during TEM sample preparation on the measured nanocrystal size distribution and formulate an equation to correct this effect. Electronic supplementary information (ESI) available. See DOI: 10.1039/c5nr06292f

  7. How Ubiquitous is Total Electron Transmission through Nanostructures (Quantum Dragons)?

    NASA Astrophysics Data System (ADS)

    Novotny, Mark

    2015-03-01

    In transport through nanostructures connected to two semi-infinite leads, the transmission probability calT (E) as a function of the energy E of the incoming electron plays a central role in the Landauer calculation of the electrical conductance G. A quantum dragon nanostructure is one which when connected to appropriate leads has total electron transmission for all energies, calT (E) =1. In two-lead measurements of single-channel quantum dragons, the quantum of conductance, G0 = 2e2 / h , should be observed. A quantum dragon may have strong scattering. In the disorder was along the axis of electron propagation, the z axis. We show that quantum dragon nanostructures can be found for strong disorder perpendicular to the z axis. In select types of nanostructures, we find the ratio of the dimension of the parameter space where quantum dragons exist to that of the complete parameter space. The results use the single-band tight-binding model, and are for the case with only one open channel and homogeneous leads. One type of nanostructure with calT (E) =1 has completely disordered slices perpendicular to the z axis, but identical slices along the z direction. Supported in part by NSF Grant DMR-1206233.

  8. 45 CFR Appendix C to Part 1355 - Electronic Data Transmission Format

    Code of Federal Regulations, 2013 CFR

    2013-10-01

    ... 45 Public Welfare 4 2013-10-01 2013-10-01 false Electronic Data Transmission Format C Appendix C.... 1355, App. C Appendix C to Part 1355—Electronic Data Transmission Format All AFCARS data to be sent... be four semi-annual electronic data transmissions from the title IV-E agency to the...

  9. Breaking resolution limits in ultrafast electron diffraction and microscopy

    PubMed Central

    Baum, Peter; Zewail, Ahmed H.

    2006-01-01

    Ultrafast electron microscopy and diffraction are powerful techniques for the study of the time-resolved structures of molecules, materials, and biological systems. Central to these approaches is the use of ultrafast coherent electron packets. The electron pulses typically have an energy of 30 keV for diffraction and 100–200 keV for microscopy, corresponding to speeds of 33–70% of the speed of light. Although the spatial resolution can reach the atomic scale, the temporal resolution is limited by the pulse width and by the difference in group velocities of electrons and the light used to initiate the dynamical change. In this contribution, we introduce the concept of tilted optical pulses into diffraction and imaging techniques and demonstrate the methodology experimentally. These advances allow us to reach limits of time resolution down to regimes of a few femtoseconds and, possibly, attoseconds. With tilted pulses, every part of the sample is excited at precisely the same time as when the electrons arrive at the specimen. Here, this approach is demonstrated for the most unfavorable case of ultrafast crystallography. We also present a method for measuring the duration of electron packets by autocorrelating electron pulses in free space and without streaking, and we discuss the potential of tilting the electron pulses themselves for applications in domains involving nuclear and electron motions. PMID:17056711

  10. Transmission electron microscope evidence of telocytes in canine dura mater.

    PubMed

    Xu, Ting; Lu, Shanshan; Zhang, Hongqi

    2016-01-01

    Telocytes (TCs) are a novel type of interstitial cells present in a wide variety of organs and tissues (www.telocytes.com). Telocytes are identified morphologically by a small cell body and specific long prolongations (telopodes) alternating thin segments (podomers) with dilations (podoms). The presence of TCs in rat meninges has been identified in previous research. We here present further evidence that TCs existed in canine dura mater, closed to capillary and surrounded by a great deal of collagen fibres under transmission electron microscope. PMID:26781033