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Sample records for situ transmission electron

  1. Progress and applications of in situ transmission electron microscopy

    International Nuclear Information System (INIS)

    Wang Rongming; Liu Jialong; Song Yuanjun

    2015-01-01

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

  2. In situ Transmission Electron Microscopy of catalyst sintering

    DEFF Research Database (Denmark)

    DeLaRiva, Andrew T.; Hansen, Thomas Willum; Challa, Sivakumar R.

    2013-01-01

    Recent advancements in the field of electron microscopy, such as aberration correctors, have now been integrated into Environmental Transmission Electron Microscopes (TEMs), making it possible to study the behavior of supported metal catalysts under operating conditions at atomic resolution. Here......, we focus on in situ electron microscopy studies of catalysts that shed light on the mechanistic aspects of catalyst sintering. Catalyst sintering is an important mechanism for activity loss, especially for catalysts that operate at elevated temperatures. Literature from the past decade is reviewed...... along with our recent in situ TEM studies on the sintering of Ni/MgAl2O4 catalysts. These results suggest that the rapid loss of catalyst activity in the earliest stages of catalyst sintering could result from Ostwald ripening rather than through particle migration and coalescence. The smallest...

  3. In situ transmission electron microscopy for magnetic nanostructures

    DEFF Research Database (Denmark)

    Ngo, Duc-The; Kuhn, Luise Theil

    2016-01-01

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

  4. In SITU Transmission Electron Microscopy on Operating Electrochemical CELLS

    DEFF Research Database (Denmark)

    Gualandris, Fabrizio; Simonsen, Søren Bredmose; Mogensen, Mogens Bjerg

    2016-01-01

    Solid oxide cells (SOC) have the potential of playing a significant role in the future efficient energy system scenario. In order to become widely commercially available, an improved performance and durability of the cells has to be achieved [1]. Conventional scanning and transmission SEM and TEM...... have been often used for ex-situ post mortem characterization of SOFCs and SOECs [2,3]. However, in order to get fundamental insight of the microstructural development of SOFC/SOEC during operation conditions in situ studies are necessary [4]....

  5. In situ Electrical measurements in Transmission Electron Microscopy

    NARCIS (Netherlands)

    Rudneva, M.

    2013-01-01

    In the present thesis the combination of real-time electricalmeasurements on nano-sampleswith simultaneous examination by transmission electron microscope (TEM) is discussed. Application of an electrical current may lead to changes in the samples thus the possibility to correlate such changes with

  6. In situ and operando transmission electron microscopy of catalytic materials

    DEFF Research Database (Denmark)

    Crozier, Peter A.; Hansen, Thomas Willum

    2015-01-01

    measurements of gas-phase catalytic products. To overcome this deficiency, operando TEM techniques are being developed that combine atomic characterization with the simultaneous measurement of catalytic products. This article provides a short review of the current status and major developments......) is a powerful technique for revealing the atomic structures of materials at elevated temperatures in the presence of reactive gases. This approach can allow the structure-reactivity relations underlying catalyst functionality to be investigated. Thus far, ETEM has been limited by the absence of in situ...... in the application of ETEM to gas-phase catalysis over the past 10 years....

  7. Current status and future directions for in situ transmission electron microscopy

    DEFF Research Database (Denmark)

    Taheri, Mitra L.; Stach, Eric A.; Arslan, Ilke

    2016-01-01

    This review article discusses the current and future possibilities for the application of in situ transmission electron microscopy to reveal synthesis pathways and functional mechanisms in complex and nanoscale materials. The findings of a group of scientists, representing academia, government labs...

  8. In-Situ Transmission Electron Microscopy on Operating Electrochemical Cells

    DEFF Research Database (Denmark)

    Gualandris, Fabrizio; Simonsen, Søren Bredmose; Mogensen, Mogens Bjerg

    have been often used for ex-situpost mortem characterization of SOFCs and SOECs [2,3]. However, in order to get fundamental insight of themicrostructural development of SOFC/SOEC during operation conditions in-situ studies are necessary [4]. Thedevelopment of advanced TEM chips and holders makes...... it possible to undertake analysis during exposure to theSOFC/SOEC sample of reactive gas flow, elevated temperatures and electrical biasing in combination. Thisallows the study of nanostructure development under temperature and electrode polarisation conditions similarto operation conditions.In this work, we...... with animage corrector and a differential pumping system.A symmetric cell was prepared by depositing a cell consisting of three thin films on a strontium titanate (STO)single crystal substrate by pulsed laser deposition (PLD). Lanthanum strontium cobaltite La0.6Sr0.4CoO3-δ (LSC)was chosen as electrode...

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

    International Nuclear Information System (INIS)

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

    2014-01-01

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

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

    NARCIS (Netherlands)

    De Hosson, Jeff Th. M.

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

  11. Current status and future directions for in situ transmission electron microscopy

    International Nuclear Information System (INIS)

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

    2016-01-01

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

  12. Current status and future directions for in situ transmission electron microscopy

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-11-15

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

  13. Irradiation-related amorphization and crystallization: In situ transmission electron microscope studies

    International Nuclear Information System (INIS)

    Allen, C.W.

    1994-01-01

    Interfacing an ion accelerator to a transmission electron microscope (TEM) allows the analytical functions of TEM imaging and diffraction to be employed during ion-irradiation effects studies. At present there are twelve such installations in Japan, one in France and one in the US. This paper treats several aspects of in situ studies involving electron and ion beam induced and enhanced phase transformations and presents results of several in situ experiments to illustrate the dynamics of this approach in the materials science of irradiation effects. The paper describes the ion- and electron-induced amorphization of CuTi; the ion-irradiation-enhanced transformation of TiCr 2 ; and the ion- and electron-irradiation-enhanced crystallization of CoSi 2

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

    International Nuclear Information System (INIS)

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

    2008-01-01

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

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

    KAUST Repository

    McDowell, Matthew T.

    2012-09-04

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

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

    KAUST Repository

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

    2012-01-01

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

  17. A transmission electron microscopy procedure for in-situ straining of miniature

    Czech Academy of Sciences Publication Activity Database

    Olbricht, J.; Wagner, M. F- X.; Condó, A.; Dlouhý, Antonín; Grossman, Ch.; Kröger, A.; Somsen, Ch.; Eggeler, G.

    2008-01-01

    Roč. 99, č. 10 (2008), s. 1150-1156 ISSN 1862-5282 R&D Projects: GA ČR(CZ) GA106/05/0918 Institutional research plan: CEZ:AV0Z20410507 Keywords : transmission electron microscopy * in-situ straining * nano-crystalline NiTi Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 0.819, year: 2008

  18. In-situ transmission electron microscopy growth of nanoparticles under extreme conditions

    International Nuclear Information System (INIS)

    Luce, F. P.; Azevedo, G. de M.; Baptista, D. L.; Zawislak, F. C.; Oliviero, E.; Fichtner, P. F. P.

    2016-01-01

    The formation and time resolved behavior of individual Pb nanoparticles embedded in silica have been studied by in-situ transmission electron microscopy observations at high temperatures (400–1100 °C) and under 200 keV electron irradiation. It is shown that under such extreme conditions, nanoparticles can migrate at long distances presenting a Brownian-like behavior and eventually coalesce. The particle migration phenomenon is discussed considering the influence of the thermal energy and the electron irradiation effects on the atomic diffusion process which is shown to control particle migration. These results and comparison with ex-situ experiments tackle the stability and the microstructure evolution of nanoparticles systems under extreme conditions. It elucidates on the effects of energetic particle irradiation-annealing treatments either as a tool or as a detrimental issue that could hamper their long-term applications in radiation-harsh environments such as in space or nuclear sectors

  19. Transmission electron microscopic method for gene mapping on polytene chromosomes by in situ hybridization

    OpenAIRE

    Wu, Madeline; Davidson, Norman

    1981-01-01

    A transmission electron microscope method for gene mapping by in situ hybridization to Drosophila polytene chromosomes has been developed. As electron-opaque labels, we use colloidal gold spheres having a diameter of 25 nm. The spheres are coated with a layer of protein to which Escherichia coli single-stranded DNA is photochemically crosslinked. Poly(dT) tails are added to the 3' OH ends of these DNA strands, and poly(dA) tails are added to the 3' OH ends of a fragmented cloned Drosophila DN...

  20. In situ investigation of bismuth nanoparticles formation by transmission electron microscope.

    Science.gov (United States)

    Liu, Liming; Wang, Honghang; Yi, Zichuan; Deng, Quanrong; Lin, Zhidong; Zhang, Xiaowen

    2018-02-01

    Bismuth (Bi) nanoparticles are prepared by using NaBi(MoO 4 ) 2 nanosheets in the beam of electrons emitted by transmission electron microscope. The formation and growth of Bi nanoparticles are investigated in situ. The sizes of Bi nanoparticles are confined within the range of 6-10nm by controlling irradiation time. It is also observed that once the diameter of nanoparticles is larger than 10nm, the Bi particles are stable as a result of the immobility of large nanoparticles. In addition, some nanoparticles on the edges form nanorods, which are explained as the result of a coalescence process, if the irradiation period is longer than 10min. The in situ research on Bi nanoparticles facilitates in-depth investigations of the physicochemical behavior and provides more potential applications in various fields such as sensors, catalysts and optical devices. Copyright © 2017 Elsevier Ltd. All rights reserved.

  1. Investigating the use of in situ liquid cell scanning transmission electron microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Nguy, Amanda [Iowa State Univ., Ames, IA (United States)

    2016-02-19

    Engineering nanoparticles with desired shape-dependent properties is the key to many applications in nanotechnology. Although many synthetic procedures exist to produce anisotropic gold nanoparticles, the dynamics of growth are typically unknown or hypothetical. In the case of seed-mediated growth in the presence of DNA into anisotropic nanoparticles, it is not known exactly how DNA directs growth into specific morphologies. A series of preliminary experiments were carried out to contribute to the investigation of the possible mechanism of DNA-mediated growth of gold nanoprisms into gold nanostars using liquid cell scanning transmission electron microscopy (STEM). Imaging in the liquid phase was achieved through the use of a liquid cell platform and liquid cell holder that allow the sample to be contained within a “chip sandwich” between two electron transparent windows. Ex situ growth experiments were performed using Au-T30 NPrisms (30-base thymine oligonucleotide-coated gold nanoprisms) that are expected to grow into gold nanostars. Growth to form these nanostars were imaged using TEM (transmission electron microscopy) and liquid cell STEM (scanning transmission electron microscopy). An attempt to perform in situ growth experiments with the same Au-T30 nanoprisms revealed challenges in obtaining desired morphology results due to the environmental differences within the liquid cell compared to the ex situ environment. Different parameters in the experimental method were explored including fluid line set up, simultaneous and alternating reagent addition, and the effect of different liquid cell volumes to ensure adequate flow of reagents into the liquid cell. Lastly, the binding affinities were compared for T30 and A30 DNA incubated with gold nanoparticles using zeta potential measurements, absorption spectroscopy, and isothermal titration calorimetry (ITC). It was previously reported thymine bases have a lower binding affinity to gold surfaces than adenine

  2. In situ transmission electron microscope observation of the formation of fuzzy structures on tungsten

    International Nuclear Information System (INIS)

    Miyamoto, M; Watanabe, T; Nagashima, H; Nishijima, D; Doerner, R P; Krasheninnikov, S I; Sagara, A; Yoshida, N

    2014-01-01

    To investigate the formation processes of tungsten nano-structures, so called fuzz, in situ transmission electron microscope observations during helium ion irradiation and high temperature annealing have been performed. The irradiation with 3 keV He + from room temperature to 1273 K is found to cause high-density helium bubbles in tungsten with no significant change in the surface structure. At higher temperatures, surface morphology changes were observed even without helium irradiation due probably to surface diffusion of tungsten atoms driven by surface tension. It is clearly shown that this morphology change is enhanced with helium irradiation, i.e. the formation of helium bubbles. (paper)

  3. In-situ environmental (scanning) transmission electron microscopy of catalysts at the atomic level

    International Nuclear Information System (INIS)

    Gai, P L; Boyes, E D

    2014-01-01

    Observing reacting single atoms on the solid catalyst surfaces under controlled reaction conditions is a key goal in understanding and controlling heterogeneous catalytic reactions. In-situ real time aberration corrected environmental (scanning) transmission electron microscopy (E(S)TEM permit the direct imaging of dynamic surface and sub-surface structures of reacting catalysts. In this paper in-situ AC ETEM and AC ESTEM studies under controlled reaction environments of oxide catalysts and supported metal nanocatalysts important in chemical industry are presented. They provide the direct evidence of dynamic processes at the oxide catalyst surface at the atomic scale and single atom dynamics in catalytic reactions. The ESTEM studies of single atom dynamics in controlled reaction environments show that nanoparticles act as reservoirs of ad-atoms. The results have important implications in catalysis and nanoparticle studies

  4. In-situ straining and time-resolved electron tomography data acquisition in a transmission electron microscope.

    Science.gov (United States)

    Hata, S; Miyazaki, S; Gondo, T; Kawamoto, K; Horii, N; Sato, K; Furukawa, H; Kudo, H; Miyazaki, H; Murayama, M

    2017-04-01

    This paper reports the preliminary results of a new in-situ three-dimensional (3D) imaging system for observing plastic deformation behavior in a transmission electron microscope (TEM) as a directly relevant development of the recently reported straining-and-tomography holder [Sato K et al. (2015) Development of a novel straining holder for transmission electron microscopy compatible with single tilt-axis electron tomography. Microsc. 64: 369-375]. We designed an integrated system using the holder and newly developed straining and image-acquisition software and then developed an experimental procedure for in-situ straining and time-resolved electron tomography (ET) data acquisition. The software for image acquisition and 3D visualization was developed based on the commercially available ET software TEMographyTM. We achieved time-resolved 3D visualization of nanometer-scale plastic deformation behavior in a Pb-Sn alloy sample, thus demonstrating the capability of this system for potential applications in materials science. © The Author 2016. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

  5. In Situ Transmission Electron Microscopy Observation of Nanostructural Changes in Phase-Change Memory

    KAUST Repository

    Meister, Stefan

    2011-04-26

    Phase-change memory (PCM) has been researched extensively as a promising alternative to flash memory. Important studies have focused on its scalability, switching speed, endurance, and new materials. Still, reliability issues and inconsistent switching in PCM devices motivate the need to further study its fundamental properties. However, many investigations treat PCM cells as black boxes; nanostructural changes inside the devices remain hidden. Here, using in situ transmission electron microscopy, we observe real-time nanostructural changes in lateral Ge2Sb2Te5 (GST) PCM bridges during switching. We find that PCM devices with similar resistances can exhibit distinct threshold switching behaviors due to the different initial distribution of nanocrystalline and amorphous domains, explaining variability of switching behaviors of PCM cells in the literature. Our findings show a direct correlation between nanostructure and switching behavior, providing important guidelines in the design and operation of future PCM devices with improved endurance and lower variability. © 2011 American Chemical Society.

  6. In Situ Room Temperature Electron-Beam Driven Graphene Growth from Hydrocarbon Contamination in a Transmission Electron Microscope

    Directory of Open Access Journals (Sweden)

    Mark H Rummeli

    2018-05-01

    Full Text Available The excitement of graphene (as well as 2D materials in general has generated numerous procedures for the fabrication of graphene. Here we present a mini-review on a rather less known, but attractive, in situ means to fabricate graphene inside a transmission electron microscope (TEM. This is achieved in a conventional TEM (viz. no sophisticated specimen holders or microscopes are required and takes advantage of inherent hydrocarbon contamination as a carbon source. Both catalyst free and single atom catalyst approaches are reviewed. An advantage of this technique is that not only can the growth process be imaged in situ, but this can also be achieved with atomic resolution. Moreover, in the future, one can anticipate such approaches enabling the growth of nano-materials with atomic precision.

  7. In situ oxidation and reduction of triangular nickel nanoplates via environmental transmission electron microscopy

    KAUST Repository

    LAGROW, A.P.; AlYami, Noktan; LLOYD, D.C.; Bakr, Osman; BOYES, E.D.; GAI, P.L.

    2017-01-01

    Understanding the oxidation and reduction mechanisms of transition metals, such as nickel (Ni), is important for their use in industrial applications of catalysis. A powerful technique for investigating the redox reactive species is in situ environmental transmission electron microscopy (ETEM), where oxidation and reduction can be tracked in real time. One particular difficulty in understanding the underlying reactions is understanding the underlying morphology of the starting structure in a reaction, in particular the defects contained in the material, and the exposed surface facets. Here-in, we use a colloidal nanoparticle synthesis in a continuous flow reactor to form nanoplates of nickel coated with oleylamine as a capping agent. We utilise an in situ heating procedure at 300 °C in vacuum to remove the oleylamine ligands, and then oxidise the Ni nanoparticles at 25 °C with 2 Pa oxygen, and follow the nanoparticles initial oxidation. After that, the nanoparticles are oxidised at 200 and 300 °C, making the size of the oxide shell increase to ∼4 nm. The oxide shell could be reduced under 2 Pa hydrogen at 500 °C to its initial size of ∼1 nm. High temperature oxidation encouraged the nanoparticles to form pure NiO nanoparticles, which occurred via the Kirkendall effect leading to hollowing and void formation.

  8. In situ oxidation and reduction of triangular nickel nanoplates via environmental transmission electron microscopy

    KAUST Repository

    LAGROW, A.P.

    2017-08-29

    Understanding the oxidation and reduction mechanisms of transition metals, such as nickel (Ni), is important for their use in industrial applications of catalysis. A powerful technique for investigating the redox reactive species is in situ environmental transmission electron microscopy (ETEM), where oxidation and reduction can be tracked in real time. One particular difficulty in understanding the underlying reactions is understanding the underlying morphology of the starting structure in a reaction, in particular the defects contained in the material, and the exposed surface facets. Here-in, we use a colloidal nanoparticle synthesis in a continuous flow reactor to form nanoplates of nickel coated with oleylamine as a capping agent. We utilise an in situ heating procedure at 300 °C in vacuum to remove the oleylamine ligands, and then oxidise the Ni nanoparticles at 25 °C with 2 Pa oxygen, and follow the nanoparticles initial oxidation. After that, the nanoparticles are oxidised at 200 and 300 °C, making the size of the oxide shell increase to ∼4 nm. The oxide shell could be reduced under 2 Pa hydrogen at 500 °C to its initial size of ∼1 nm. High temperature oxidation encouraged the nanoparticles to form pure NiO nanoparticles, which occurred via the Kirkendall effect leading to hollowing and void formation.

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

    International Nuclear Information System (INIS)

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

    2014-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-03-10

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

  11. A review of transmission electron microscopes with in situ ion irradiation

    Science.gov (United States)

    Hinks, J. A.

    2009-12-01

    Transmission electron microscopy (TEM) with in situ ion irradiation is unique amongst experimental techniques in allowing the direct observation of the internal microstructure of materials on the nanoscale whilst they are being subjected to bombardment with energetic particles. Invaluable insights into the underlying atomistic processes at work can be gained through direct investigation of radiation induced and enhanced effects such as: phase changes and segregation; mechanical and structural changes; atomic/layer mixing and chemical disorder; compositional changes; chemical reactions; grain growth and shrinkage; precipitation and dissolution; defect/bubble formation, growth, motion, coalescence, removal and destruction; ionisation; diffusion; and collision cascades. The experimental results obtained can be used to validate the predictions of computational models which in turn can elucidate the mechanisms behind the phenomena seen in the microscope. It is 50 years since the first TEM observations of in situ ion irradiation were made by D.W. Pashley, A.E.B. Presland and J.W. Menter at the Tube Investment Laboratories in Cambridge, United Kingdom and 40 years since the first interfacing of an ion beam system with a TEM by P.A. Thackery, R.S. Nelson and H.C. Sansom at the Atomic Energy Research Establishment at Harwell, United Kingdom. In that time the field has grown with references in the literature to around thirty examples of such facilities. This paper gives an overview of the importance of the technique, especially with regard to the current challenges faced in understanding radiation damage in nuclear environments; a description of some of the important construction elements and design considerations of TEMs with in situ ion irradiation; a brief history of the development of this type of instrument; a summary of the facilities built around the world over the last half century; and finally a focus on the instruments in operation today.

  12. The nanoaquarium: A nanofluidic platform for in situ transmission electron microscopy in liquid media

    Science.gov (United States)

    Grogan, Joseph M.

    There are many scientifically interesting and technologically relevant nanoscale phenomena that take place in liquid media. Examples include aggregation and assembly of nanoparticles; colloidal crystal formation; liquid phase growth of structures such as nanowires; electrochemical deposition and etching for fabrication processes and battery applications; interfacial phenomena; boiling and cavitation; and biological interactions. Understanding of these fields would benefit greatly from real-time, in situ transmission electron microscope (TEM) imaging with nanoscale resolution. Most liquids cannot be imaged by traditional TEM due to evaporation in the high vacuum environment and the requirement that samples be very thin. Liquid-cell in situ TEM has emerged as an exciting new experimental technique that hermetically seals a thin slice of liquid between two electron transparent membranes to enable TEM imaging of liquid-based processes. This work presents details of the fabrication of a custom-made liquid-cell in situ TEM device, dubbed the nanoaquarium. The nanoaquarium's highlights include an exceptionally thin sample cross section (10s to 100s of nm); wafer scale processing that enables high-yield mass production; robust hermetic sealing that provides leak-free operation without use of glue, epoxy, or any polymers; compatibility with lab-on-chip technology; and on-chip integrated electrodes for sensing and actuation. The fabrication process is described, with an emphasis on direct wafer bonding. Experimental results involving direct observation of colloid aggregation using an aqueous solution of gold nanoparticles are presented. Quantitative analysis of the growth process agrees with prior results and theory, indicating that the experimental technique does not radically alter the observed phenomenon. For the first time, in situ observations of nanoparticles at a contact line and in an evaporating thin film of liquid are reported, with applications for techniques such

  13. Growth Termination and Multiple Nucleation of Single-Wall Carbon Nanotubes Evidenced by in Situ Transmission Electron Microscopy

    DEFF Research Database (Denmark)

    Zhang, Lili; He, Maoshuai; Hansen, Thomas Willum

    2017-01-01

    and successive growth of additional SWCNTs on Co catalyst particles supported on MgO by means of environmental transmission electron microscopy. Such in situ observations reveal the plethora of solid carbon formations at the local scale while it is happening and thereby elucidate the multitude of configurations...

  14. In situ Reduction and Oxidation of Nickel from Solid Oxide Fuel Cells in a Transmission Electron Microscope

    DEFF Research Database (Denmark)

    Faes, Antonin; Jeangros, Quentin; Wagner, Jakob Birkedal

    2009-01-01

    Environmental transmission electron microscopy was used to characterize in situ the reduction and oxidation of nickel from a Ni/YSZ solid oxide fuel cell anode support between 300-500{degree sign}C. The reduction is done under low hydrogen pressure. The reduction initiates at the NiO/YSZ interface...

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

    International Nuclear Information System (INIS)

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

    2013-01-01

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

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

    Science.gov (United States)

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

    2013-02-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2017-05-15

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

  18. Impact of Membrane-Induced Particle Immobilization on Seeded Growth Monitored by In Situ Liquid Scanning Transmission Electron Microscopy.

    Science.gov (United States)

    Weiner, Rebecca G; Chen, Dennis P; Unocic, Raymond R; Skrabalak, Sara E

    2016-05-01

    In situ liquid cell scanning transmission electron microscopy probes seeded growth in real time. The growth of Pd on Au nanocubes is monitored as a model system to compare growth within a liquid cell and traditional colloidal synthesis. Different growth patterns are observed due to seed immobilization and the highly reducing environment within the liquid cell. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. In-situ reduction of promoted cobalt oxide supported on alumina by environmental transmission electron microscopy

    DEFF Research Database (Denmark)

    Dehghan, Roya; Hansen, Thomas Willum; Wagner, Jakob Birkedal

    2011-01-01

    the reactivity of the nanoparticles and the importance of controlling the gas composition and specimen temperature during this type of experiment. Similar behaviour was observed for a non-promoted catalyst. Imaging and analysis of the promoted sample before and after reduction indicated a uniform distribution...... resolution transmission electron microscopy and scanning transmission electron microscopy imaging. The cobalt particles were mainly face centred cubic while some hexagonal close packed particles were also found. Reoxidation of the sample upon cooling to room temperature, still under flowing H2, underlines...

  20. Facilities for in situ ion beam studies in transmission electron microscopes

    International Nuclear Information System (INIS)

    Allen, C.W.; Ohnuki, S.; Takahashi, H.

    1993-08-01

    Interfacing an ion accelerator to a transmission electron microscope (TEM) allows the analytical functions of TEM imaging and electron diffraction from very small regions to be employed during ion-irradiation effects studies. At present there are ten such installations in Japan, one in France and one in the USA. General specifications of facilities which are operational in 1993 are summarized, and additional facilities which are planned or being proposed are briefly described

  1. An in-situ analytical scanning and transmission electron microscopy investigation of structure-property relationships in electronic materials

    Science.gov (United States)

    Wagner, Andrew James

    As electronic and mechanical devices are scaled downward in size and upward in complexity, macroscopic principles no longer apply. Synthesis of three-dimensionally confined structures exhibit quantum confinement effects allowing, for example, silicon nanoparticles to luminesce. The reduction in size of classically brittle materials reveals a ductile-to-brittle transition. Such a transition, attributed to a reduction in defects, increases elasticity. In the case of silicon, elastic deformation can improve electronic carrier mobility by over 50%, a vital attribute of modern integrated circuits. The scalability of such principles and the changing atomistic processes which contribute to them presents a vitally important field of research. Beginning with the direct observation of dislocations and lattice planes in the 1950s, the transmission electron microscope has been a powerful tool in materials science. More recently, as nanoscale technologies have proliferated modern life, their unique ability to spatially resolve nano- and atomic-scale structures has become a critical component of materials research and characterization. Signals produced by an incident beam of high-energy electrons enables researchers to both image and chemically analyze materials at the atomic scale. Coherently and elastically-scattered electrons can be collected to produce atomic-scale images of a crystalline sample. New specimen stages have enabled routine investigation of samples heated up to 1000 °C and cooled to liquid nitrogen temperatures. MEMS-based transducers allow for sub-nm scale mechanical testing and ultrathin membranes allow study of liquids and gases. Investigation of a myriad of previously "unseeable" processes can now be observed within the TEM, and sometimes something new is found within the old. High-temperature annealing of pure a Si:H films leads to crystallization of the film. Such films provide higher carrier mobility compared to amorphous films, offering improved

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

    Science.gov (United States)

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

    2016-12-01

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

  3. Nanosecond time-resolved investigations using the in situ of dynamic transmission electron microscope (DTEM)

    International Nuclear Information System (INIS)

    LaGrange, Thomas; Campbell, Geoffrey H.; Reed, B.W.; Taheri, Mitra; Pesavento, J. Bradley; Kim, Judy S.; Browning, Nigel D.

    2008-01-01

    Most biological processes, chemical reactions and materials dynamics occur at rates much faster than can be captured with standard video rate acquisition methods in transmission electron microscopes (TEM). Thus, there is a need to increase the temporal resolution in order to capture and understand salient features of these rapid materials processes. This paper details the development of a high-time resolution dynamic transmission electron microscope (DTEM) that captures dynamics in materials with nanosecond time resolution. The current DTEM performance, having a spatial resolution <10 nm for single-shot imaging using 15 ns electron pulses, will be discussed in the context of experimental investigations in solid state reactions of NiAl reactive multilayer films, the study of martensitic transformations in nanocrystalline Ti and the catalytic growth of Si nanowires. In addition, this paper will address the technical issues involved with high current, electron pulse operation and the near-term improvements to the electron optics, which will greatly improve the signal and spatial resolutions, and to the laser system, which will allow tailored specimen and photocathode drive conditions

  4. Nanosecond time-resolved investigations using the in situ of dynamic transmission electron microscope (DTEM)

    Energy Technology Data Exchange (ETDEWEB)

    LaGrange, Thomas [Lawrence Livermore National Laboratory, 7000 East Avenue, Livermore, CA 94550 (United States)], E-mail: lagrange@llnl.gov; Campbell, Geoffrey H.; Reed, B.W.; Taheri, Mitra; Pesavento, J. Bradley [Lawrence Livermore National Laboratory, 7000 East Avenue, Livermore, CA 94550 (United States); Kim, Judy S.; Browning, Nigel D. [Lawrence Livermore National Laboratory, 7000 East Avenue, Livermore, CA 94550 (United States); Department of Chemical Engineering and Materials Science, University of California, One Shields Avenue, Davis, CA 95616 (United States)

    2008-10-15

    Most biological processes, chemical reactions and materials dynamics occur at rates much faster than can be captured with standard video rate acquisition methods in transmission electron microscopes (TEM). Thus, there is a need to increase the temporal resolution in order to capture and understand salient features of these rapid materials processes. This paper details the development of a high-time resolution dynamic transmission electron microscope (DTEM) that captures dynamics in materials with nanosecond time resolution. The current DTEM performance, having a spatial resolution <10 nm for single-shot imaging using 15 ns electron pulses, will be discussed in the context of experimental investigations in solid state reactions of NiAl reactive multilayer films, the study of martensitic transformations in nanocrystalline Ti and the catalytic growth of Si nanowires. In addition, this paper will address the technical issues involved with high current, electron pulse operation and the near-term improvements to the electron optics, which will greatly improve the signal and spatial resolutions, and to the laser system, which will allow tailored specimen and photocathode drive conditions.

  5. In situ transmission electron microscope studies of ion irradiation-induced and irradiation-enhanced phase changes

    International Nuclear Information System (INIS)

    Allen, C.W.

    1992-01-01

    Motivated at least initially by materials needs for nuclear reactor development, extensive irradiation effects studies employing transmission electron microscopes (TEM) have been performed for several decades, involving irradiation-induced and irradiation-enhanced microstructural changes, including phase transformations such as precipitation, dissolution, crystallization, amorphization, and order-disorder phenomena. From the introduction of commercial high voltage electron microscopes (HVEM) in the mid-1960s, studies of electron irradiation effects have constituted a major aspect of HVEM application in materials science. For irradiation effects studies two additional developments have had particularly significant impact; the development of TEM specimen holder sin which specimen temperature can be controlled in the range 10-2200 K and the interfacing of ion accelerators which allows in situ TEM studies of irradiation effects and the ion beam modification of materials within this broad temperature range. This paper treats several aspects of in situ studies of electron and ion beam-induced and enhanced phase changes and presents two case studies involving in situ experiments performed in an HVEM to illustrate the strategies of such an approach of the materials research of irradiation effects

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

    International Nuclear Information System (INIS)

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

    2010-01-01

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

  7. Quantitative analysis for in situ sintering of 3% yttria-stablized zirconia in the transmission electron microscope

    International Nuclear Information System (INIS)

    Majidi, Hasti; Holland, Troy B.; Benthem, Klaus van

    2015-01-01

    Studying particle-agglomerate systems compared to two-particle systems elucidates different stages of sintering by monitoring both pores and particles. We report on in situ sintering of 3% yttria-stablized zirconia particle agglomerates in the transmission electron microscope (TEM). Real-time TEM observations indicate neck formation and growth, particle coalescence and pore closure. A MATLAB-based image processing tool was developed to calculate the projected area of the agglomerate with and without internal pores during in situ sintering. We demonstrate the first densification curves generated from sequentially acquired TEM images. The in situ sintering onset temperature was then determined to be at 960 °C. Densification curves illustrated that the agglomerate projected area which excludes the internal observed pores also shrinks during in situ sintering. To overcome the common projection problem for TEM analyses, agglomerate mass-thickness maps were obtained from low energy-loss analysis combined with STEM imaging. The decrease in the projected area was directly related to the increase in mass-thickness of the agglomerate, likely caused by hidden pores existing in the direction of the beam. Access to shrinkage curves through in situ TEM analysis provides a new avenue to investigate fundamental mechanisms of sintering through directly correlating microstructural changes during consolidation with mesoscale densification behavior

  8. Quantitative analysis for in situ sintering of 3% yttria-stablized zirconia in the transmission electron microscope

    Energy Technology Data Exchange (ETDEWEB)

    Majidi, Hasti [Department of Chemical Engineering and Materials Science, University of California, Davis, CA 95616 (United States); Holland, Troy B. [Department of Mechanical Engineering, Colorado State University, Fort Collins, CO 80523 (United States); Benthem, Klaus van, E-mail: benthem@ucdavis.edu [Department of Chemical Engineering and Materials Science, University of California, Davis, CA 95616 (United States)

    2015-05-15

    Studying particle-agglomerate systems compared to two-particle systems elucidates different stages of sintering by monitoring both pores and particles. We report on in situ sintering of 3% yttria-stablized zirconia particle agglomerates in the transmission electron microscope (TEM). Real-time TEM observations indicate neck formation and growth, particle coalescence and pore closure. A MATLAB-based image processing tool was developed to calculate the projected area of the agglomerate with and without internal pores during in situ sintering. We demonstrate the first densification curves generated from sequentially acquired TEM images. The in situ sintering onset temperature was then determined to be at 960 °C. Densification curves illustrated that the agglomerate projected area which excludes the internal observed pores also shrinks during in situ sintering. To overcome the common projection problem for TEM analyses, agglomerate mass-thickness maps were obtained from low energy-loss analysis combined with STEM imaging. The decrease in the projected area was directly related to the increase in mass-thickness of the agglomerate, likely caused by hidden pores existing in the direction of the beam. Access to shrinkage curves through in situ TEM analysis provides a new avenue to investigate fundamental mechanisms of sintering through directly correlating microstructural changes during consolidation with mesoscale densification behavior.

  9. Quantitative analysis for in situ sintering of 3% yttria-stablized zirconia in the transmission electron microscope.

    Science.gov (United States)

    Majidi, Hasti; Holland, Troy B; van Benthem, Klaus

    2015-05-01

    Studying particle-agglomerate systems compared to two-particle systems elucidates different stages of sintering by monitoring both pores and particles. We report on in situ sintering of 3% yttria-stablized zirconia particle agglomerates in the transmission electron microscope (TEM). Real-time TEM observations indicate neck formation and growth, particle coalescence and pore closure. A MATLAB-based image processing tool was developed to calculate the projected area of the agglomerate with and without internal pores during in situ sintering. We demonstrate the first densification curves generated from sequentially acquired TEM images. The in situ sintering onset temperature was then determined to be at 960 °C. Densification curves illustrated that the agglomerate projected area which excludes the internal observed pores also shrinks during in situ sintering. To overcome the common projection problem for TEM analyses, agglomerate mass-thickness maps were obtained from low energy-loss analysis combined with STEM imaging. The decrease in the projected area was directly related to the increase in mass-thickness of the agglomerate, likely caused by hidden pores existing in the direction of the beam. Access to shrinkage curves through in situ TEM analysis provides a new avenue to investigate fundamental mechanisms of sintering through directly correlating microstructural changes during consolidation with mesoscale densification behavior. Copyright © 2014 Elsevier B.V. All rights reserved.

  10. In situ transmission electron microscopy of individual carbon nanotetrahedron/ribbon structures in bending

    Energy Technology Data Exchange (ETDEWEB)

    Kohno, Hideo, E-mail: kohno.hideo@kochi-tech.ac.jp [School of Environmental Science and Engineering, Kochi University of Technology, Kami, Kochi 782-8502 (Japan); Masuda, Yusuke [Graduate School of Science, Osaka University, Toyonaka, Osaka 560-0043 (Japan)

    2015-05-11

    When the direction of flattening of a carbon nanotube changes during growth mediated by a metal nanoparticle, a carbon nanotetrahedron is formed in the middle of the carbon nanoribbon. We report the bending properties of the carbon nanotetrahedron/nanoribbon structure using a micro-manipulator system in a transmission electron microscope. In many cases, bending occurs at an edge of the carbon nanotetrahedron. No significant change is observed in the tetrahedron's shape during bending, and the bending is reversible and repeatable. Our results show that the carbon nanotetrahedron/nanoribbon structure has good durability against mechanical bending.

  11. Combining nanocalorimetry and dynamic transmission electron microscopy for in situ characterization of materials processes under rapid heating and cooling

    Energy Technology Data Exchange (ETDEWEB)

    Grapes, Michael D., E-mail: mgrapes1@jhu.edu [Department of Materials Science and Engineering, Johns Hopkins University, Baltimore, Maryland 21218 (United States); Materials Measurement Science Division, Material Measurement Laboratory, National Institute of Standards and Technology, Gaithersburg, Maryland 20899 (United States); LaGrange, Thomas; Reed, Bryan W.; Campbell, Geoffrey H. [Condensed Matter and Materials Division, Lawrence Livermore National Laboratory, Livermore, California 94550 (United States); Friedman, Lawrence H.; LaVan, David A., E-mail: david.lavan@nist.gov [Materials Measurement Science Division, Material Measurement Laboratory, National Institute of Standards and Technology, Gaithersburg, Maryland 20899 (United States); Weihs, Timothy P., E-mail: weihs@jhu.edu [Department of Materials Science and Engineering, Johns Hopkins University, Baltimore, Maryland 21218 (United States)

    2014-08-15

    Nanocalorimetry is a chip-based thermal analysis technique capable of analyzing endothermic and exothermic reactions at very high heating and cooling rates. Here, we couple a nanocalorimeter with an extremely fast in situ microstructural characterization tool to identify the physical origin of rapid enthalpic signals. More specifically, we describe the development of a system to enable in situ nanocalorimetry experiments in the dynamic transmission electron microscope (DTEM), a time-resolved TEM capable of generating images and electron diffraction patterns with exposure times of 30 ns–500 ns. The full experimental system consists of a modified nanocalorimeter sensor, a custom-built in situ nanocalorimetry holder, a data acquisition system, and the DTEM itself, and is capable of thermodynamic and microstructural characterization of reactions over a range of heating rates (10{sup 2} K/s–10{sup 5} K/s) accessible by conventional (DC) nanocalorimetry. To establish its ability to capture synchronized calorimetric and microstructural data during rapid transformations, this work describes measurements on the melting of an aluminum thin film. We were able to identify the phase transformation in both the nanocalorimetry traces and in electron diffraction patterns taken by the DTEM. Potential applications for the newly developed system are described and future system improvements are discussed.

  12. Switching behaviour of individual Ag-TCNQ nanowires: an in situ transmission electron microscopy study

    Science.gov (United States)

    Ran, Ke; Rösner, Benedikt; Butz, Benjamin; Fink, Rainer H.; Spiecker, Erdmann

    2016-10-01

    The organic semiconductor silver-tetracyanoquinodimethane (Ag-TCNQ) exhibits electrical switching and memory characteristics. Employing a scanning tunnelling microscopy setup inside a transmission electron microscope, the switching behaviour of individual Ag-TCNQ nanowires (NWs) is investigated in detail. For a large number of NWs, the switching between a high (OFF) and a low (ON) resistance state was successfully stimulated by negative bias sweeps. Fitting the experimental I-V curves with a Schottky emission function makes the switching features prominent and thus enables a direct evaluation of the switching process. A memory cycle including writing, reading and erasing features is demonstrated at an individual NW. Moreover, electronic failure mechanisms due to Joule heating are discussed. These findings have a significant impact on our understanding of the switching behaviour of Ag-TCNQ.

  13. In situ light spectroscopy in the environmental transmission electron microscope (ETEM)

    DEFF Research Database (Denmark)

    Cavalca, Filippo; Langhammer, C.; Pedersen, Thomas

    2012-01-01

    the LSPR signal coming from the whole specimen, providing information complementary to the TEM analysis. During any ETEM experiment the electron beam effect on the sample is a difficult issue to address and rule out. In addition, if a reaction has to be followed in situ in the ETEM, the information...... is often recorded on a limited portion of the sample. Being able to probe the sample with INPS and ETEM at the same time allows parallel investigation at the local and macro scale, as well as aids the assessment of beam effects. A dedicated custom TEM specimen holder containing two optical fibers, five...... electrical contacts, a fixed miniaturized optical bench for light handling and a heating element (Fig. 1) has been designed. A system of pre-aligned mirrors and a MEMS heater are implemented in the holder. The system is primarily designed for use in combination with LSPR spectroscopy, but it is flexible...

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

    International Nuclear Information System (INIS)

    Berlin, Katja; Trampert, Achim

    2017-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2017-07-15

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

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

    Science.gov (United States)

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

    2017-09-07

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

  17. Real time nanoscale structural evaluation of gold structures on Si (100) surface using in-situ transmission electron microscopy

    International Nuclear Information System (INIS)

    Rath, A.; Juluri, R. R.; Satyam, P. V.

    2014-01-01

    Transport behavior of gold nanostructures on Si(100) substrate during annealing under high vacuum has been investigated using in-situ real time transmission electron microscopy (TEM). A comparative study has been done on the morphological changes due to annealing under different vacuum environments. Au thin films of thickness ∼2.0 nm were deposited on native oxide covered silicon substrate by using thermal evaporation system. In-situ real time TEM measurements at 850 °C showed the isotropic growth of rectangular/square shaped gold-silicon alloy structures. During the growth, it is observed that the alloying occurs in liquid phase followed by transformation into the rectangular shapes. For similar system, ex-situ annealing in low vacuum (10 −2 millibars) at 850 °C showed the spherical gold nanostructures with no Au-Si alloy formation. Under low vacuum annealing conditions, the rate of formation of the oxide layer dominates the oxide desorption rate, resulting in the creation of a barrier layer between Au and Si, which restricts the inter diffusion of Au in to Si. This work demonstrates the important role of interfacial oxide layer on the growth of nanoscale Au-Si alloy structures during the initial growth. The time dependent TEM images are presented to offer a direct insight into the fundamental dynamics of the sintering process at the nanoscale

  18. Mechanical characterization of diesel soot nanoparticles: in situ compression in a transmission electron microscope and simulations

    Science.gov (United States)

    Jenei, Istvan Zoltan; Dassenoy, Fabrice; Epicier, Thierry; Khajeh, Arash; Martini, Ashlie; Uy, Dairene; Ghaednia, Hamed; Gangopadhyay, Arup

    2018-02-01

    Incomplete fuel burning inside an internal combustion engine results in the creation of soot in the form of nanoparticles. Some of these soot nanoparticles (SNP) become adsorbed into the lubricating oil film present on the cylinder walls, which adversely affects the tribological performance of the lubricant. In order to better understand the mechanisms underlying the wear caused by SNPs, it is important to understand the behavior of SNPs and to characterize potential changes in their mechanical properties (e.g. hardness) caused by (or during) mechanical stress. In this study, the behavior of individual SNPs originating from diesel engines was studied under compression. The experiments were performed in a transmission electron microscope using a nanoindentation device. The nanoparticles exhibited elasto-plastic behavior in response to consecutive compression cycles. From the experimental data, the Young’s modulus and hardness of the SNPs were calculated. The Young’s modulus and hardness of the nanoparticles increased with the number of compression cycles. Using an electron energy loss spectroscopy technique, it was shown that the sp2/sp3 ratio within the compressed nanoparticle decreases, which is suggested to be the cause of the increase in elasticity and hardness. In order to corroborate the experimental findings, molecular dynamics simulations of a model SNP were performed. The SNP model was constructed using carbon and hydrogen atoms with morphology and composition comparable to those observed in the experiment. The model SNP was subjected to repeated compressions between two virtual rigid walls. During the simulation, the nanoparticle exhibited elasto-plastic behavior like that in the experiments. The results of the simulations confirm that the increase in the elastic modulus and hardness is associated with a decrease in the sp2/sp3 ratio.

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

    International Nuclear Information System (INIS)

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

    2012-01-01

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

  20. In situ high-resolution transmission electron microscopy synthesis observation of nanostructured carbon coated LiFePO 4

    Science.gov (United States)

    Trudeau, M. L.; Laul, D.; Veillette, R.; Serventi, A. M.; Mauger, A.; Julien, C. M.; Zaghib, K.

    In situ high-resolution transmission electron microscopy (HRTEM) studies of the structural transformations that occur during the synthesis of carbon-coated LiFePO 4 (C-LiFePO 4) and heat treatment to elevated temperatures were conducted in two different electron microscopes. Both microscopes have sample holders that are capable of heating up to 1500 °C, with one working under high vacuum and the other capable of operating with the sample surrounded by a low gaseous environment. The C-LiFePO 4 samples were prepared using three different compositions of precursor materials with Fe(0), Fe(II) or Fe(III), a Li-containing salt and a polyethylene- block-poly(ethylene glycol)-50% ethylene oxide or lactose. The in situ TEM studies suggest that low-cost Fe(0) and a low-cost carbon-containing compound such as lactose are very attractive precursors for mass production of C-LiFePO 4, and that 700 °C is the optimum synthesis temperature. At temperatures higher than 800 °C, LiFePO 4 has a tendency to decompose. The same in situ measurements have been made on particles without carbon coat. The results show that the homogeneous deposit of the carbon deposit at 700 °C is the result of the annealing that cures the disorder of the surface layer of bare LiFePO 4. Electrochemical tests supported the conclusion that the C-LiFePO 4 derived from Fe(0) is the most attractive for mass production.

  1. In-situ Study of Dynamic Phenomena at Metal Nanosolder Interfaces Using Aberration Corrected Scanning Transmission Electron Microcopy.

    Energy Technology Data Exchange (ETDEWEB)

    Lu, Ping

    2014-10-01

    Controlling metallic nanoparticle (NP) interactions plays a vital role in the development of new joining techniques (nanosolder) that bond at lower processing temperatures but remain viable at higher temperatures. The pr imary objective of this project is t o develop a fundamental understanding of the actual reaction processes, associated atomic mechanisms, and the resulting microstructure that occur during thermally - driven bond formation concerning metal - metal nano - scale (%3C50nm) interfaces. In this LDRD pr oject, we have studied metallic NPs interaction at the elevated temperatures by combining in - situ transmission electron microscopy (TEM ) using an aberration - corrected scanning transmission electron microscope (AC - STEM) and atomic - scale modeling such as m olecular dynamic (MD) simulations. Various metallic NPs such as Ag, Cu and Au are synthesized by chemical routines. Numerous in - situ e xperiments were carried out with focus of the research on study of Ag - Cu system. For the first time, using in - situ STEM he ating experiments , we directly observed t he formation of a 3 - dimensional (3 - D) epitaxial Cu - Ag core - shell nanoparticle during the thermal interaction of Cu and Ag NPs at elevated temperatures (150 - 300 o C). The reaction takes place at temperatures as low as 150 o C and was only observed when care was taken to circumvent the effects of electron beam irradiation during STEM imaging. Atomic - scale modeling verified that the Cu - Ag core - shell structure is energetically favored, and indicated that this phenomenon is a nano - scale effect related to the large surface - to - volume ratio of the NPs. The observation potentially can be used for developing new nanosolder technology that uses Ag shell as the "glue" that stic ks the particles of Cu together. The LDRD has led to several journal publications and numerous conference presentations, and a TA. In addition, we have developed new TEM characterization techniques and phase

  2. Size effect on compression properties of GaN nanocones examined using in situ transmission electron microscopy

    International Nuclear Information System (INIS)

    Kang, Shao-Hui; Fang, Te-Hua

    2014-01-01

    Highlights: • Strain-induced structural variations of GaN nanocones are estimated using in situ TEM. • Young’s modulus of GaN nanocones with a diameter of 100–350 nm are 190–290 GPa. • The E 2 peak was red-shifted, indicated increased compressive stress. - Abstract: Mechanical property measurements of single nanocones are challenging because the small scale of the nanostructures. In this study, critical-stress- and strain-induced structural variations of GaN nanocones are estimated using in situ transmission electron microscopy (TEM) compression experiments. For single GaN nanocones with a diameter of 100–350 nm, the Young’s modulus, plastic deformation energy (W p ), and elastic deformation energy (W e ) values were 190–290 GPa, 0.02–1.65 × 10 −11 J, and 0.04–3.85 × 10 −11 J, respectively. Raman spectra were used to measure GaN indentation. The E 2 peak was red-shifted, indicated increased compressive stress in the indented area

  3. In Situ Transmission Electron Microscopy Study of Electron Beam-Induced Transformations in Colloidal Cesium Lead Halide Perovskite Nanocrystals

    Science.gov (United States)

    2017-01-01

    An increasing number of studies have recently reported the rapid degradation of hybrid and all-inorganic lead halide perovskite nanocrystals under electron beam irradiation in the transmission electron microscope, with the formation of nanometer size, high contrast particles. The nature of these nanoparticles and the involved transformations in the perovskite nanocrystals are still a matter of debate. Herein, we have studied the effects of high energy (80/200 keV) electron irradiation on colloidal cesium lead bromide (CsPbBr3) nanocrystals with different shapes and sizes, especially 3 nm thick nanosheets, a morphology that facilitated the analysis of the various ongoing processes. Our results show that the CsPbBr3 nanocrystals undergo a radiolysis process, with electron stimulated desorption of a fraction of bromine atoms and the reduction of a fraction of Pb2+ ions to Pb0. Subsequently Pb0 atoms diffuse and aggregate, giving rise to the high contrast particles, as previously reported by various groups. The diffusion is facilitated by both high temperature and electron beam irradiation. The early stage Pb nanoparticles are epitaxially bound to the parent CsPbBr3 lattice, and evolve into nonepitaxially bound Pb crystals upon further irradiation, leading to local amorphization and consequent dismantling of the CsPbBr3 lattice. The comparison among CsPbBr3 nanocrystals with various shapes and sizes evidences that the damage is particularly pronounced at the corners and edges of the surface, due to a lower diffusion barrier for Pb0 on the surface than inside the crystal and the presence of a larger fraction of under-coordinated atoms. PMID:28122188

  4. In situ environmental transmission electron microscope investigation of NiGa nanoparticle synthesis

    DEFF Research Database (Denmark)

    Damsgaard, Christian Danvad; Duchstein, Linus Daniel Leonhard; Elkjær, Christian Fink

    2011-01-01

    . Both Ni and Ga edges are observed in the spectra. Quantification of Ni:Ga ratio is hampered by the presence of the Ni L1 edge. The ETEM experiments have been supported by complementary in situ X-Ray Diffraction (XRD) measurements on synthesis of Ni5Ga3 catalyst on a high surface area silica support...... prepared by wet impregnation [2]. Although the in situ XRD was performed at significantly higher H2 flow (40 Nml/min) and pressure (100 kPa) the complimentary data correlates with the main temperature dependence of phase and structure and shows formation of the Ni5Ga3 phase for temperatures higher than 300...

  5. Local stress modification during in situ transmission electron microscopy straining experiments

    Czech Academy of Sciences Publication Activity Database

    Zárubová, Niva; Gemperle, Antonín; Gemperlová, Juliana

    2007-01-01

    Roč. 462, - (2007), s. 407-411 ISSN 0921-5093 R&D Projects: GA ČR GA202/04/2016 Institutional research plan: CEZ:AV0Z10100520 Keywords : in situ TEM straining, Local stress in a strained foil * local stress in a strained foil Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.457, year: 2007

  6. In-situ transmission electron microscopy observation of slip propagation in ä3 bicrystals

    Czech Academy of Sciences Publication Activity Database

    Gemperlová, Juliana; Jacques, A.; Gemperle, Antonín; Vystavěl, Tomáš; Zárubová, Niva; Janecek, M.

    2002-01-01

    Roč. 324, - (2002), s. 183-189 ISSN 0921-5093 R&D Projects: GA ČR GA202/98/1281 Institutional research plan: CEZ:AV0Z1010914 Keywords : in- situ TEM deformation * propagation of slip * plastic deformation * grain boundary * symmetrical ä3 bicrystal Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.107, year: 2002

  7. In situ Transmission Electron Microscopy He{sup +} implantation and thermal aging of nanocrystalline iron

    Energy Technology Data Exchange (ETDEWEB)

    Muntifering, Brittany, E-mail: brmunti@sandia.gov [Sandia National Laboratories, Albuquerque, NM, 87185 (United States); Department of Civil and Environmental Engineering, Northwestern University, Evanston, IL, 60208 (United States); Fang, Youwu [Department of Civil and Environmental Engineering, Northwestern University, Evanston, IL, 60208 (United States); Leff, Asher C. [Department of Materials Science & Engineering, Drexel University, Philadelphia, PA, 19104 (United States); Dunn, Aaron [Sandia National Laboratories, Albuquerque, NM, 87185 (United States); George W. Woodruff School of Mechanical Engineering, Georgia Institute of Technology, UMI 2958 Georgia Tech CNRS, 57070, Metz (France); Qu, Jianmin [Department of Civil and Environmental Engineering, Northwestern University, Evanston, IL, 60208 (United States); School of Engineering, Tufts University, Medford, MA, 02155 (United States); Taheri, Mitra L. [Department of Materials Science & Engineering, Drexel University, Philadelphia, PA, 19104 (United States); Dingreville, Remi; Hattar, Khalid [Sandia National Laboratories, Albuquerque, NM, 87185 (United States)

    2016-12-15

    The high density of interfaces in nanostructured materials are hypothesized to improve radiation tolerance compared to coarse-grained materials. In order to investigate the roles of vacancies, self-interstitials, and helium, both room temperature in situ TEM He{sup +} implantation and annealing, as well as high temperature He{sup +} implantation was performed on nanocrystalline iron. Dislocation loops are formed by the accumulation of mobile point defects rather than by displacement cascades at intermediate temperatures. Around 600 °C, loops disappeared through gradual shrinking, which is hypothesized to correspond to the annihilation of self-interstitial atoms by mobile vacancies that also resulted in cavity formation. The room temperature implantation resulted in cavities evenly distributed throughout the grain after annealing, whereas cavities were predominately observed at grain boundaries for the elevated temperature implantation. This difference is associated with the formation of stable helium-vacancy complexes in the grains during room temperature implantation, which is not present during high temperature implantation. - Highlights: • In situ TEM He{sup +} implantation and annealing was performed on nanocrystalline iron. • Small grains limited loop size and resulted in complete disappearance of loops by 600 °C. • Implantation followed by annealing resulted in cavities evenly distributed through grain. • Cavities predominately observed at grain boundaries after He{sup +} implantation at 600 °C.

  8. Transmission electron microscopy in situ investigation of dislocation mobility in semiconductors

    CERN Document Server

    Vanderschaeve, G; Insa, P D T; Caillard, D

    2000-01-01

    TEM in situ straining experiments provide a unique way to investigate in real time the behaviour of individual dislocations under applied stress. The results obtained on a variety of semiconductors are presented: numerous dislocation sources are observed which makes it possible to measure the dislocation velocity as a function of different physical parameters (local shear stress, temperature, dislocation character, length of the moving dislocation, ...). The experimental results are consistent with a dislocation glide governed by the Peierls mechanism, even for II-VI compounds which have a significant degree of ionic character. For compounds, a linear dependence of the dislocation velocity on the length of the moving segment is noticed, whereas for elemental semiconductors a transition between a length-dependent and a length-independent velocity regime is observed. Analysed in the framework of the kink diffusion model (Hirth and Lothe theory), these results allow an estimation of the kink formation and migrat...

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

    International Nuclear Information System (INIS)

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

    2011-01-01

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

  10. In situ transmission electron microscopy study of the microstructural origins for the electric field-induced phenomena in ferroelectric perovskites

    Energy Technology Data Exchange (ETDEWEB)

    Guo, Hanzheng [Iowa State Univ., Ames, IA (United States)

    2014-12-15

    Ferroelectrics are important materials due to their extensive technological applications, such as non-volatile memories, field-effect transistors, ferroelectric tunneling junctions, dielectric capacitors, piezoelectric transducers, sensors and actuators. As is well known, the outstanding dielectric, piezoelectric, and ferroelectric properties of these functional oxides originate from their ferroelectric domain arrangements and the corresponding evolution under external stimuli (e.g. electric field, stress, and temperature). Electric field has been known as the most efficient stimulus to manipulate the ferroelectric domains through polarization switching and alignment. Therefore, direct observation of the dynamic process of electric field-induced domain evolution and crystal structure transformation is of significant importance to understand the microstructural mechanisms for the functional properties of ferroelectrics. In this dissertation, electric field in situ transmission electron microscopy (TEM) technique was employed to monitor the real-time evolution of the domain morphology and crystal structure during various electrical processes: (1) the initial poling process, (2) the electric field reversal process, and (3) the electrical cycling process. Two types of perovskite-structured ceramics, normal ferroelectrics and relaxor ferroelectrics, were used for this investigation. In addition to providing the microscopic insight for some wellaccepted phase transformation rules, discoveries of some new or even unexpected physical phenomena were also demonstrated.

  11. In situ transmission electron microscopy analyses of thermally annealed self catalyzed GaAs nanowires grown by molecular beam epitaxy

    DEFF Research Database (Denmark)

    Ambrosini, S.; Wagner, Jakob Birkedal; Booth, Tim

    2011-01-01

    Self catalyzed GaAs nanowires grown on Si-treated GaAs substrates were studied with a transmission electron microscope before and after annealing at 600◦C. At room temperature the nanowires have a zincblende structure and are locally characterized by a high density of rotational twins and stacking...... faults. Selected area diffraction patterns and high-resolution transmission electron microscopy images show that nanowires undergo structural modifications upon annealing, suggesting a decrease of defect density following the thermal treatment....

  12. InAlN high electron mobility transistor Ti/Al/Ni/Au Ohmic contact optimisation assisted by in-situ high temperature transmission electron microscopy

    International Nuclear Information System (INIS)

    Smith, M. D.; Parbrook, P. J.; O'Mahony, D.; Conroy, M.; Schmidt, M.

    2015-01-01

    This paper correlates the micro-structural and electrical characteristics associated with annealing of metallic multi-layers typically used in the formation of Ohmic contacts to InAlN high electron mobility transistors. The multi-layers comprised Ti/Al/Ni/Au and were annealed via rapid thermal processing at temperatures up to 925 °C with electrical current-voltage analysis establishing the onset of Ohmic (linear IV) behaviour at 750–800 °C. In-situ temperature dependent transmission electron microscopy established that metallic diffusion and inter-mixing were initiated near a temperature of 500 °C. Around 800 °C, inter-diffusion of the metal and semiconductor (nitride) was observed, correlating with the onset of Ohmic electrical behaviour. The sheet resistance associated with the InAlN/AlN/GaN interface is highly sensitive to the anneal temperature, with the range depending on the Ti layer thickness. The relationship between contact resistivity and measurement temperature follow that predicted by thermionic field emission for contacts annealed below 850 °C, but deviated above this due to excessive metal-semiconductor inter-diffusion

  13. A MEMS-based heating holder for the direct imaging of simultaneous in-situ heating and biasing experiments in scanning/transmission electron microscopes.

    Science.gov (United States)

    Mele, Luigi; Konings, Stan; Dona, Pleun; Evertz, Francis; Mitterbauer, Christoph; Faber, Pybe; Schampers, Ruud; Jinschek, Joerg R

    2016-04-01

    The introduction of scanning/transmission electron microscopes (S/TEM) with sub-Angstrom resolution as well as fast and sensitive detection solutions support direct observation of dynamic phenomena in-situ at the atomic scale. Thereby, in-situ specimen holders play a crucial role: accurate control of the applied in-situ stimulus on the nanostructure combined with the overall system stability to assure atomic resolution are paramount for a successful in-situ S/TEM experiment. For those reasons, MEMS-based TEM sample holders are becoming one of the preferred choices, also enabling a high precision in measurements of the in-situ parameter for more reproducible data. A newly developed MEMS-based microheater is presented in combination with the new NanoEx™-i/v TEM sample holder. The concept is built on a four-point probe temperature measurement approach allowing active, accurate local temperature control as well as calorimetry. In this paper, it is shown that it provides high temperature stability up to 1,300°C with a peak temperature of 1,500°C (also working accurately in gaseous environments), high temperature measurement accuracy (in-situ S/TEM imaging experiments, but also elemental mapping at elevated temperatures using energy-dispersive X-ray spectroscopy (EDS). Moreover, it has the unique capability to enable simultaneous heating and biasing experiments. © 2016 Wiley Periodicals, Inc.

  14. In-situ transmission electron microscopy of the solid-phase epitaxial growth of GaAs: sample preparation and artifact characterization

    International Nuclear Information System (INIS)

    Llewellyn, D.J.; Llewellyn, D.J.; Belay, K.B.; Ridgway, M.C.

    1998-01-01

    In-situ transmission electron microscopy (TEM) has been used to characterize the solid phase epitaxial growth of amorphized GaAs at a temperature of 260 deg C. To maximize heat transfer from the heated holder to the sample and minimize electron-irradiation induced artifacts, non-conventional methodologies were utilized for the preparation of cross-sectional samples. GaAs 3x1 mm rectangular wafers were cleaved then glued face-to-face to form a wafer stack size of 3x3 mm while maintaining the TEM region at the center. This stack was subsequently polished on the cross-section to a thickness of ∼ 200 μm. A 3 mm disc was then cut perpendicular to the cross-section using a Gatan ultrasonic cutter. The disc was polished then dimpled on both sides to a thickness of ∼ 15 μm. This was ion-beam milled at liquid nitrogen temperature to an electron-transparent layer. From a comparison of in-situ and ex-situ measurements of the recrystallization rate, the actual sample temperature during in-situ characterization was estimated to deviate by ≤ 20 deg C from that of the heated holder. The influence of electron-irradiation was found to be negligible by comparing the recrystallization rate and microstructure of irradiated and unirradiated regions of comparable thickness. Similarly, the influence of the 'thin-foil effect' was found to be negligible by comparing the recrystallization rate and microstructure of thick and thin regions, the former determined after the removal of the sample from the microscope and further ion-beam milling of tens of microns of material. In conclusion, the potential influence of artifacts during in-situ TEM can be minimized by the appropriate choice of sample preparation procedures. (authors)

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

    Science.gov (United States)

    Heinemann, K.

    1987-01-01

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

  16. Direct in situ transmission electron microscopy observation of Al push up during early stages of the Al-induced layer exchange

    International Nuclear Information System (INIS)

    Birajdar, B.I.; Antesberger, T.; Butz, B.; Stutzmann, M.; Spiecker, E.

    2012-01-01

    The mechanism of Al transport during Al-induced layer exchange and crystallization of amorphous Si (a-Si) has been investigated by in situ and analytical transmission electron microscopy. Significant grain boundary realignment and coarsening of Al grains close to the Si crystallization growth front as well as push up of excess Al into the a-Si layer at distances even a few micrometers away from the crystallization front were observed. Stress-mediated diffusion of Al is postulated to explain the experimental observations.

  17. In-situ realtime monitoring of nanoscale gold electroplating using micro-electro-mechanical systems liquid cell operating in transmission electron microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Egawa, Minoru; Fujita, Hiroyuki [Institute of Industrial Science, University of Tokyo, Meguro, Tokyo 153-8505 (Japan); Ishida, Tadashi, E-mail: ishida.t.ai@m.titech.ac.jp [Institute of Industrial Science, University of Tokyo, Meguro, Tokyo 153-8505 (Japan); Graduate School of Science and Technology, Tokyo Institute of Technology, Yokohama, Kanagawa 225-8503 (Japan); Jalabert, Laurent [LIMMS/CNRS-IIS (UMI 2820), Institute of Industrial Science, University of Tokyo, Meguro, Tokyo 153-8505 (Japan); CNRS, LAAS, 7 Avenue du Colonel Roche, F-31400 Toulouse, France and University of Toulouse, LAAS, F-31400 Toulouse (France)

    2016-01-11

    The dynamics of nanoscale electroplating between gold electrodes was investigated using a microfabricated liquid cell mounted on a scanning transmission electron microscope. The electroplating was recorded in-situ for 10 min with a spatial resolution higher than 6 nm. At the beginning of the electroplating, gold spike-like structures of about 50 nm in size grew from an electrode, connected gold nanoclusters around them, and form three dimensional nanoscale structures. We visualized the elementary process of the gold electroplating, and believe that the results lead to the deeper understanding of electroplating at the nanoscale.

  18. In-situ realtime monitoring of nanoscale gold electroplating using micro-electro-mechanical systems liquid cell operating in transmission electron microscopy

    International Nuclear Information System (INIS)

    Egawa, Minoru; Fujita, Hiroyuki; Ishida, Tadashi; Jalabert, Laurent

    2016-01-01

    The dynamics of nanoscale electroplating between gold electrodes was investigated using a microfabricated liquid cell mounted on a scanning transmission electron microscope. The electroplating was recorded in-situ for 10 min with a spatial resolution higher than 6 nm. At the beginning of the electroplating, gold spike-like structures of about 50 nm in size grew from an electrode, connected gold nanoclusters around them, and form three dimensional nanoscale structures. We visualized the elementary process of the gold electroplating, and believe that the results lead to the deeper understanding of electroplating at the nanoscale

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

    Science.gov (United States)

    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.

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

    DEFF Research Database (Denmark)

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

    2014-01-01

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

  1. In situ transmission electron microscopy investigation of the interfacial reaction between Ni and Al during rapid heating in a nanocalorimeter

    Energy Technology Data Exchange (ETDEWEB)

    Grapes, Michael D., E-mail: mgrapes1@jhu.edu, E-mail: david.lavan@nist.gov, E-mail: weihs@jhu.edu [Department of Materials Science and Engineering, Johns Hopkins University, Baltimore, Maryland 21218 (United States); Material Measurement Laboratory, Materials Measurement Science Division, National Institute of Standards and Technology, Gaithersburg, Maryland 20899 (United States); LaGrange, Thomas; Reed, Bryan W.; Campbell, Geoffrey H. [Lawrence Livermore National Laboratory, Materials Science and Technology Division, Livermore, California 94550 (United States); Woll, Karsten [Department of Materials Science and Engineering, Johns Hopkins University, Baltimore, Maryland 21218 (United States); Institute of Applied Materials, Karlsruhe Institute of Technology, 76344 Eggenstein-Leopoldshafen (Germany); LaVan, David A., E-mail: mgrapes1@jhu.edu, E-mail: david.lavan@nist.gov, E-mail: weihs@jhu.edu [Material Measurement Laboratory, Materials Measurement Science Division, National Institute of Standards and Technology, Gaithersburg, Maryland 20899 (United States); Weihs, Timothy P., E-mail: mgrapes1@jhu.edu, E-mail: david.lavan@nist.gov, E-mail: weihs@jhu.edu [Department of Materials Science and Engineering, Johns Hopkins University, Baltimore, Maryland 21218 (United States)

    2014-11-01

    The Al/Ni formation reaction is highly exothermic and of both scientific and technological significance. In this report, we study the evolution of intermetallic phases in this reaction at a heating rate of 830 K/s. 100-nm-thick Al/Ni bilayers were deposited onto nanocalorimeter sensors that enable the measurement of temperature and heat flow during rapid heating. Time-resolved transmission electron diffraction patterns captured simultaneously with thermal measurements allow us to identify the intermetallic phases present and reconstruct the phase transformation sequence as a function of time and temperature. The results show a mostly unaltered phase transformation sequence compared to lower heating rates.

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

    Science.gov (United States)

    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.

  3. In situ observation of the impact of surface oxidation on the crystallization mechanism of GeTe phase-change thin films by scanning transmission electron microscopy

    Science.gov (United States)

    Berthier, R.; Bernier, N.; Cooper, D.; Sabbione, C.; Hippert, F.; Noé, P.

    2017-09-01

    The crystallization mechanisms of prototypical GeTe phase-change material thin films have been investigated by in situ scanning transmission electron microscopy annealing experiments. A novel sample preparation method has been developed to improve sample quality and stability during in situ annealing, enabling quantitative analysis and live recording of phase change events. Results show that for an uncapped 100 nm thick GeTe layer, exposure to air after fabrication leads to composition changes which promote heterogeneous nucleation at the oxidized surface. We also demonstrate that protecting the GeTe layer with a 10 nm SiN capping layer prevents nucleation at the surface and allows volume nucleation at a temperature 50 °C higher than the onset of crystallization in the oxidized sample. Our results have important implications regarding the integration of these materials in confined memory cells.

  4. Manipulation and in situ transmission electron microscope characterization of sub-100 nm nanostructures using a microfabricated nanogripper

    DEFF Research Database (Denmark)

    Cagliani, Alberto; Wierzbicki, Rafal; Occhipini, Luigi

    2010-01-01

    ion beam milling and subsequently coating these with Au, the nanogripper could lift up laterally aligned single-walled carbon nanotubes from a 1 µm wide trench, while immediately making good electrical contact. One such carbon nanotube was structurally and electrically characterized real-time in TEM......We present here a polysilicon electrothermal microfabricated nanogripper capable of manipulating nanowires and nanotubes in the sub-100 nm range. The nanogripper was fabricated with a mix and match microfabrication process, combining high throughput of photolithography with 10 nm resolution...... of electron beam lithography. Vertically grown III–V nanowires with a diameter of 70 nm were picked up using the nanogripper, allowing direct transfer of the nanogripper-nanowire ensemble into a transmission electron microscope (TEM) for structural characterization. By refining the end-effectors with focused...

  5. In situ electrical probing and bias-mediated manipulation of dielectric nanotubes in a high-resolution transmission electron microscope

    International Nuclear Information System (INIS)

    Golberg, D.; Mitome, M.; Kurashima, K.; Zhi, C.Y.; Tang, C.C.; Bando, Y.; Lourie, O.

    2006-01-01

    Boron nitride nanotubes filled with magnesium oxides [MgO, MgO 2 ] and/or hydroxide [Mg(OH) 2 ] are electrically probed and delicately manipulated inside a 300 kV JEOL-3000F high-resolution transmission analytical electron microscope equipped with a side-entry 'Nanofactory Instruments' piezoholder. At a low bias the nanotubes demonstrate truly insulating behavior. At a high bias of ±30 V they show reversible breakdown current of several dozens of nA. Under 300 kV electron beam irradiation the nanotubes are positively charged that allows us to perform on-demand manipulation with them through tuning of polarity and/or value of a bias voltage on a gold counterelectrode from -140 to +140 V, owing to the prominent electrostatic nanotube-electrode interactions

  6. In-situ transmission electron microscopy imaging of formation and evolution of LixWO3 during lithiation of WO3 nanowires

    International Nuclear Information System (INIS)

    Qi, Kuo; Li, Xiaomin; Sun, Muhua; Huang, Qianming; Wei, Jiake; Xu, Zhi; Wang, Wenlong; Bai, Xuedong; Wang, Enge

    2016-01-01

    The phase transition from monoclinic WO 3 to cubic Li x WO 3 during lithiation of WO 3 is one of the key features for tungsten oxide as the most used electrochromic material. Conventionally, the lithium intercalation of WO 3 has been studied by building generic layered electrochromic device combining with structural characterization and electrochemistry measurement at macro scale. In-situ transmission electron microscopy (in-situ TEM) has been proposed as a method for revealing the detailed mechanism of structural, physical, and chemical properties. Here, we use in-situ TEM method to investigate the formation and evolution of Li x WO 3 in real-time during the electrochemical lithiation of WO 3 nanowires. The dynamic lithiation process is recorded by TEM imaging, diffraction, and electron energy loss spectroscopy. The WO 3 -Li x WO 3 phase boundary of reaction front has been observed at high resolution. The timeliness of crystallinity of Li x WO 3 and the intercalation channels for Li ions are also identified. Moreover, the co-existence of both polycrystalline Li-poor area and amorphous Li-rich phases of Li x WO 3 was found. Our results provide an insight into the basic lithiation process of WO 3 , which is significantly important for understanding the electrochromic mechanism of tungsten oxide.

  7. In situ transmission electron microscopy study of the microstructural origins for the electric field-induced phenomena in ferroelectric perovskites

    Science.gov (United States)

    Guo, Hanzheng

    Ferroelectrics are important materials due to their extensive technological applications, such as non-volatile memories, field-effect transistors, ferroelectric tunneling junctions, dielectric capacitors, piezoelectric transducers, sensors and actuators. As is well known, the outstanding dielectric, piezoelectric, and ferroelectric properties of these functional oxides originate from their ferroelectric domain arrangements and the corresponding evolution under external stimuli (e.g. electric field, stress, and temperature). Electric field has been known as the most efficient stimulus to manipulate the ferroelectric domains through polarization switching and alignment. Therefore, direct observation of the dynamic process of electric field-induced domain evolution and crystal structure transformation is of significant importance to understand the microstructural mechanisms for the functional properties of ferroelectrics. In this dissertation, electric field in situ transmission electron microscopy (TEM) technique was employed to monitor the real-time evolution of the domain morphology and crystal structure during various electrical processes: (1) the initial poling process, (2) the electric field reversal process, and (3) the electrical cycling process. Two types of perovskite-structured ceramics, normal ferroelectrics and relaxor ferroelectrics, were used for this investigation. In addition to providing the microscopic insight for some well-accepted phase transformation rules, discoveries of some new or even unexpected physical phenomena were also demonstrated. For the initial poling process, microstructural origins for the piezoelectricity development in the three most promising lead-free piezoceramic systems were investigated. For the non-ergodic relaxor ferroelectric compositions ( x = 6% - 9%) in the (1-x)(Bi1/2Na 1/2)TiO3-xBaTiO3 system, well-developed piezoelectricity was realized at poling fields far below the coercive field and phase transition field. Such

  8. In situ redox cycle of a nickel–YSZ fuel cell anode in an environmental transmission electron microscope

    DEFF Research Database (Denmark)

    Jeangros, Quentin; Faes, Antonin; Wagner, Jakob Birkedal

    2010-01-01

    triggers the reduction reaction. During Ni reoxidation, the creation of a porous structure, due to mass transport, accounts for the redox instability of the Ni-based anode. Both the expansion of NiO during a redox cycle and the presence of stress in the yttria-stabilized zirconia grains are observed......Environmental transmission electron microscopy is used in combination with density functional theory calculations to study the redox stability of a nickel/yttria-stabilized zirconia solid oxide fuel cell anode. The results reveal that the transfer of oxygen from NiO to yttria-stabilized zirconia...... directly. Besides providing an understanding of the Ni–YSZ anode redox degradation, the observations are used to propose an alternative anode design for improved redox tolerance....

  9. Manipulation and in situ transmission electron microscope characterization of sub-100 nm nanostructures using a microfabricated nanogripper

    International Nuclear Information System (INIS)

    Cagliani, Alberto; Wierzbicki, Rafal; Petersen, Dirch Hjorth; Dyvelkov, Karin Nordstrøm; Sardan Sukas, Özlem; Booth, Tim; Bøggild, Peter; Occhipinti, Luigi; Herstrøm, Berit G

    2010-01-01

    We present here a polysilicon electrothermal microfabricated nanogripper capable of manipulating nanowires and nanotubes in the sub-100 nm range. The nanogripper was fabricated with a mix and match microfabrication process, combining high throughput of photolithography with 10 nm resolution of electron beam lithography. Vertically grown III–V nanowires with a diameter of 70 nm were picked up using the nanogripper, allowing direct transfer of the nanogripper-nanowire ensemble into a transmission electron microscope (TEM) for structural characterization. By refining the end-effectors with focused ion beam milling and subsequently coating these with Au, the nanogripper could lift up laterally aligned single-walled carbon nanotubes from a 1 µm wide trench, while immediately making good electrical contact. One such carbon nanotube was structurally and electrically characterized real-time in TEM, showing a breakdown current density of approximately 0.5 × 10 12 Am −2 . The nanogripper is the smallest microfabricated gripper to date and is the first tool showing repeatable, 3D nanomanipulation of sub-100 nm structures.

  10. Microstructural changes in CdSe-coated ZnO nanowires evaluated by in situ annealing in transmission electron microscopy and x-ray diffraction

    International Nuclear Information System (INIS)

    Majidi, Hasti; Baxter, Jason B; Winkler, Christopher R; Taheri, Mitra L

    2012-01-01

    We report on the crystallite growth and phase change of electrodeposited CdSe coatings on ZnO nanowires during annealing. Both in situ transmission electron microscopy (TEM) and x-ray diffraction (XRD) reveal that the nanocrystal size increases from ∼3 to ∼10 nm upon annealing at 350 °C for 1 h and then to more than 30 nm during another 1 h at 400 °C, exhibiting two distinct growth regimes. Nanocrystal growth occurs together with a structural change from zinc blende to wurtzite. The structural transition begins at 350 °C, which results in the formation of stacking faults. Increased crystallite size, comparable to the coating thickness, can improve charge separation in extremely thin absorber solar cells. We demonstrate a nearly two-fold improvement in power conversion efficiency upon annealing. (paper)

  11. Microstructural changes in CdSe-coated ZnO nanowires evaluated by in situ annealing in transmission electron microscopy and x-ray diffraction

    Science.gov (United States)

    Majidi, Hasti; Winkler, Christopher R.; Taheri, Mitra L.; Baxter, Jason B.

    2012-07-01

    We report on the crystallite growth and phase change of electrodeposited CdSe coatings on ZnO nanowires during annealing. Both in situ transmission electron microscopy (TEM) and x-ray diffraction (XRD) reveal that the nanocrystal size increases from ˜3 to ˜10 nm upon annealing at 350 °C for 1 h and then to more than 30 nm during another 1 h at 400 °C, exhibiting two distinct growth regimes. Nanocrystal growth occurs together with a structural change from zinc blende to wurtzite. The structural transition begins at 350 °C, which results in the formation of stacking faults. Increased crystallite size, comparable to the coating thickness, can improve charge separation in extremely thin absorber solar cells. We demonstrate a nearly two-fold improvement in power conversion efficiency upon annealing.

  12. Quantitative analysis of stress-induced martensites by in situ transmission electron microscopy superelastic tests in Cu-Al-Ni shape memory alloys

    International Nuclear Information System (INIS)

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

    2010-01-01

    Stress-induced martensite nucleation and further growing, in Cu-Al-Ni shape memory alloys, have been studied during in situ superelastic tests in the transmission electron microscope. Two kinds of martensite, β 3 ' and γ 3 ' , are induced and can coexist under stress, both exhibiting in a high density of stacking faults. The interface plane and the orientation relationships between the different variants of such martensites have been determined, and the atomic configurations of the lattices across the interface have been described. Finally, in light of the results, selection rules for the stress-induced promoted martensites at the nano-scale have been established, being determined by the shear direction and the basal plane of the martensite lattice.

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

    Science.gov (United States)

    Boyes, Edward D.; Gai, Pratibha L.

    2014-02-01

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

  14. Diffusion processes in Cu-Al-Ni shape memory alloys studied by mechanical spectroscopy and in situ transmission electron microscopy at high temperatures

    International Nuclear Information System (INIS)

    No, M.L.; Ibarra, A.; Lopez-Echarri, A.; Bocanegra, E.H.; San Juan, J.

    2006-01-01

    We have studied the mobility of defects in the frozen β phase of the Cu-Al-Ni shape memory alloys by mechanical spectroscopy as a function of temperature. In parallel, we have characterized the microstructure and their evolution with over-heating treatments. Thermal treatments have been performed in situ in a transmission electron microscope by using a heating stage. Internal friction and modulus defect measurements have been correlated with the microstructural observations by transmission electron microscopy. We discuss the behavior of the internal friction spectra, corresponding to over-heating in the β-phase, and propose microscopic mechanisms responsible for the evolution when the material is not in thermal equilibrium. In particular, the dislocations became mobile in the temperature range between 750 and 800 K where the L2 1 atomic order changes to the B2 order. A relaxation peak has been observed in the equilibrium β phase domain, which has been examined in detail by isothermal measurements as a function of frequency. The activation enthalpy of the peak has been determined to be 3.05 ± 0.1 eV, and possible microscopic mechanisms responsible for the peak are discussed

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

    Energy Technology Data Exchange (ETDEWEB)

    Zweiacker, K., E-mail: Kai@zweiacker.org; Liu, C.; Wiezorek, J. M. K. [Department of Mechanical Engineering and Materials Science, University of Pittsburgh, 648 Benedum Hall, 3700 OHara Street, Pittsburgh, Pennsylvania 15261 (United States); McKeown, J. T.; LaGrange, T.; Reed, B. W.; Campbell, G. H. [Materials Science Division, Physical and Life Science Directorate, Lawrence Livermore National Laboratory, 7000 East Avenue, Livermore, California 94551 (United States)

    2016-08-07

    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{sup −1} to ∼2.5 m s{sup −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{sup −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.

  16. Pseudoelastic deformation and size effects during in situ transmission electron microscopy tensile testing of NiTi

    Czech Academy of Sciences Publication Activity Database

    Manchuraju, S.; Kroeger, A.; Somsen, C.; Dlouhý, Antonín; Eggeler, G.; Sarosi, P. M.; Anderson, P. M.; Mills, M. J.

    2012-01-01

    Roč. 60, 6-7 (2012), s. 2770-2777 ISSN 1359-6454 Institutional support: RVO:68081723 Keywords : martensitic phase transformation * In Situ TEM * Shape memory alloys * Crystallographic theory of martensite Subject RIV: JG - Metallurgy Impact factor: 3.941, year: 2012

  17. Direct transmission electron microscopy observations of martensitic transformations in Ni-rich NiTi single crystals during in situ cooling and straining

    International Nuclear Information System (INIS)

    Kroeger, A.; Dziaszyk, S.; Frenzel, J.; Somsen, Ch.; Dlouhy, A.; Eggeler, G.

    2008-01-01

    We investigate martensitic transformations using transmission electron microscopy (TEM) in compression aged Ni-rich NiTi single crystals with one family of Ni 4 Ti 3 precipitates. Small cylinders from a Ni-rich NiTi single crystal with a Ni content of 51.0 at.% were compression aged at 550 deg. C in the [1 1 1] B2 direction for different aging times. Differential scanning calorimetry (DSC) investigations show that a three-step martensitic transformation (three DSC peaks on cooling from the high temperature regime) can be observed for aging times of 4 ks. In situ cooling TEM investigations reveal that the first peak on cooling is associated with a transformation from B2 to R-phase, starting from all precipitate/matrix interfaces. On further cooling, the B19'-phase appears and grows along precipitate/matrix interfaces (second step). With further decreasing temperature, the remaining R-phase between the precipitates transforms to B19' (third peak). In situ TEM straining experiments of B2 above the martensitic start temperature reveal that first some microstructural regions directly transform in microscopic burst like events from B2 to B19'. On further straining, the B19'-phase grows along precipitate/matrix interfaces. However, no formation of R-phase precedes the formation of stress-induced B19'

  18. Direct visualization of initial SEI morphology and growth kinetics during lithium deposition by in situ electrochemical transmission electron microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Sacci, Robert L. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Materials Science adn Technology Division; Dudney, Nancy J. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Materials Science adn Technology Division; More, Karren L. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Center for Nanophase Materials Science; Parent, Lucas R. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States). Fundamental and Computational Sciences Directorate; Arslan, Ilke [Pacific Northwest National Lab. (PNNL), Richland, WA (United States). Fundamental and Computational Sciences Directorate; Browning, Nigel D. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States). Fundamental and Computational Sciences Directorate; Unocic, Raymond R. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Center for Nanophase Materials Science

    2013-12-20

    Deposition of Li is a major safety concern existing in Li-ion secondary batteries. We perform the first in situ high spatial resolution measurement coupled with real-time quantitative electrochemistry to characterize SEI formation on gold using a standard battery electrolyte. We also demonstrate that a dendritic SEI forms prior to Li deposition and that it remains on the surface after Li electrodissolution.

  19. Micromechanical and in situ shear testing of Al–SiC nanolaminate composites in a transmission electron microscope (TEM)

    Energy Technology Data Exchange (ETDEWEB)

    Mayer, C. [Materials Science and Engineering, Arizona State University, Tempe, AZ 85287-6106 (United States); Li, N.; Mara, N. [Center for Integrated Nanotechnologies, Los Alamos National Laboratory, Albuquerque, NM (United States); Chawla, N., E-mail: nchawla@asu.edu [Materials Science and Engineering, Arizona State University, Tempe, AZ 85287-6106 (United States)

    2015-01-05

    Nanolaminate composites show promise as high strength and toughness materials. However, due to the limited volume of these materials, micron scale mechanical testing methods must be used to determine the properties of these films. To this end, a novel approach combining a double notch shear testing geometry and compression with a flat punch in a nanoindenter was developed to determine the mechanical properties of these films under shear loading. To further elucidate the failure mechanisms under shear loading, in situ TEM experiments were performed using a double notch geometry cut into the TEM foil. Aluminum layer thicknesses of 50 nm and 100 nm were used to show the effect of constraint on the deformation. Higher shear strength was observed in the 50 nm sample (690±54 MPa) compared to the 100 nm sample (423±28.7 MPa). Additionally, failure occurred close to the Al–SiC interface in the 50 nm sample as opposed to failure within the Al layer in the 100 nm sample.

  20. Understanding the Thermal Stability of Palladium-Platinum Core-Shell Nanocrystals by In Situ Transmission Electron Microscopy and Density Functional Theory.

    Science.gov (United States)

    Vara, Madeline; Roling, Luke T; Wang, Xue; Elnabawy, Ahmed O; Hood, Zachary D; Chi, Miaofang; Mavrikakis, Manos; Xia, Younan

    2017-05-23

    Core-shell nanocrystals offer many advantages for heterogeneous catalysis, including precise control over both the surface structure and composition, as well as reduction in loading for rare and costly metals. Although many catalytic processes are operated at elevated temperatures, the adverse impacts of heating on the shape and structure of core-shell nanocrystals are yet to be understood. In this work, we used ex situ heating experiments to demonstrate that Pd@Pt 4L core-shell nanoscale cubes and octahedra are promising for catalytic applications at temperatures up to 400 °C. We also used in situ transmission electron microscopy to monitor the thermal stability of the core-shell nanocrystals in real time. Our results demonstrate a facet dependence for the thermal stability in terms of shape and composition. Specifically, the cubes enclosed by {100} facets readily deform shape at a temperature 300 °C lower than that of the octahedral counterparts enclosed by {111} facets. A reversed trend is observed for composition, as alloying between the Pd core and the Pt shell of an octahedron occurs at a temperature 200 °C lower than that for the cubic counterpart. Density functional theory calculations provide atomic-level explanations for the experimentally observed behaviors, demonstrating that the barriers for edge reconstruction determine the relative ease of shape deformation for cubes compared to octahedra. The opposite trend for alloying of the core-shell structure can be attributed to a higher propensity for subsurface Pt vacancy formation in octahedra than in cubes.

  1. In situ transmission electron microscopy observation of pulverization of aluminum nanowires and evolution of the thin surface Al2O3 layers during lithiation-delithiation cycles.

    Science.gov (United States)

    Liu, Yang; Hudak, Nicholas S; Huber, Dale L; Limmer, Steven J; Sullivan, John P; Huang, Jian Yu

    2011-10-12

    Lithiation-delithiation cycles of individual aluminum nanowires (NWs) with naturally oxidized Al(2)O(3) surface layers (thickness 4-5 nm) were conducted in situ in a transmission electron microscope. Surprisingly, the lithiation was always initiated from the surface Al(2)O(3) layer, forming a stable Li-Al-O glass tube with a thickness of about 6-10 nm wrapping around the NW core. After lithiation of the surface Al(2)O(3) layer, lithiation of the inner Al core took place, which converted the single crystal Al to a polycrystalline LiAl alloy, with a volume expansion of about 100%. The Li-Al-O glass tube survived the 100% volume expansion, by enlarging through elastic and plastic deformation, acting as a solid electrolyte with exceptional mechanical robustness and ion conduction. Voids were formed in the Al NWs during the initial delithiation step and grew continuously with each subsequent delithiation, leading to pulverization of the Al NWs to isolated nanoparticles confined inside the Li-Al-O tube. There was a corresponding loss of capacity with each delithiation step when arrays of NWs were galvonostatically cycled. The results provide important insight into the degradation mechanism of lithium-alloy electrodes and into recent reports about the performance improvement of lithium ion batteries by atomic layer deposition of Al(2)O(3) onto the active materials or electrodes.

  2. A method for measuring the local gas pressure within a gas-flow stage in situ in the transmission electron microscope

    International Nuclear Information System (INIS)

    Colby, R.; Alsem, D.H.; Liyu, A.; Kabius, B.

    2015-01-01

    Environmental transmission electron microscopy (TEM) has enabled in situ experiments in a gaseous environment with high resolution imaging and spectroscopy. Addressing scientific challenges in areas such as catalysis, corrosion, and geochemistry can require pressures much higher than the ∼20 mbar achievable with a differentially pumped environmental TEM. Gas flow stages, in which the environment is contained between two semi-transparent thin membrane windows, have been demonstrated at pressures of several atmospheres. However, the relationship between the pressure at the sample and the pressure drop across the system is not clear for some geometries. We demonstrate a method for measuring the gas pressure at the sample by measuring the ratio of elastic to inelastic scattering and the defocus of the pair of thin windows. This method requires two energy filtered high-resolution TEM images that can be performed during an ongoing experiment, at the region of interest. The approach is demonstrated to measure greater than atmosphere pressures of N 2 gas using a commercially available gas-flow stage. This technique provides a means to ensure reproducible sample pressures between different experiments, and even between very differently designed gas-flow stages. - Highlights: • Method developed for measuring gas pressure within a gas-flow stage in the TEM. • EFTEM and CTF-fitting used to calculate amount and volume of gas. • Requires only a pair of images without leaving region of interest. • Demonstrated for P > 1 atm with a common commercial gas-flow stage

  3. In situ investigation of explosive crystallization in a-Ge: Experimental determination of the interface response function using dynamic transmission electron microscopy

    International Nuclear Information System (INIS)

    Nikolova, Liliya; MacLeod, Jennifer M.; Ibrahim, Heide; Stern, Mark J.; Siwick, Bradley J.; Reed, Bryan W.; Campbell, Geoffrey H.; LaGrange, Thomas; Rosei, Federico

    2014-01-01

    The crystallization of amorphous semiconductors is a strongly exothermic process. Once initiated the release of latent heat can be sufficient to drive a self-sustaining crystallization front through the material in a manner that has been described as explosive. Here, we perform a quantitative in situ study of explosive crystallization in amorphous germanium using dynamic transmission electron microscopy. Direct observations of the speed of the explosive crystallization front as it evolves along a laser-imprinted temperature gradient are used to experimentally determine the complete interface response function (i.e., the temperature-dependent front propagation speed) for this process, which reaches a peak of 16 m/s. Fitting to the Frenkel-Wilson kinetic law demonstrates that the diffusivity of the material locally/immediately in advance of the explosive crystallization front is inconsistent with those of a liquid phase. This result suggests a modification to the liquid-mediated mechanism commonly used to describe this process that replaces the phase change at the leading amorphous-liquid interface with a change in bonding character (from covalent to metallic) occurring in the hot amorphous material

  4. Investigation of the growth and in situ heating transmission electron microscopy analysis of Ag2S-catalyzed ZnS nanowires

    Science.gov (United States)

    Kim, Jung Han; Kim, Jong Gu; Song, Junghyun; Bae, Tae-Sung; Kim, Kyou-Hyun; Lee, Young-Seak; Pang, Yoonsoo; Oh, Kyu Hwan; Chung, Hee-Suk

    2018-04-01

    We investigated the semiconductor-catalyzed formation of semiconductor nanowires (NWs) - silver sulfide (Ag2S)-catalyzed zinc sulfide (ZnS) NWs - based on a vapor-liquid-solid (VLS) growth mechanism through metal-organic chemical vapor deposition (MOCVD) with a Ag thin film. The Ag2S-catalyzed ZnS NWs were confirmed to have a wurtzite structure with a width and length in the range of ∼30 nm to ∼80 nm and ∼1 μm, respectively. Using extensive transmission electron microscopy (TEM) and energy-dispersive X-ray spectroscopy (EDS) analyses from plane and cross-sectional viewpoints, the ZnS NWs were determined to have a c-axis, [0001] growth direction. In addition, the catalyst at the top of the ZnS NWs was determined to consist of a Ag2S phase. To support the Ag2S-catalyzed growth of the ZnS NWs by a VLS reaction, an in situ heating TEM experiment was conducted from room temperature to 840 °C. During the experiment, the melting of the Ag2S catalyst in the direction of the ZnS NWs was first observed at approximately 480 °C along with the formation of a carbon (C) shell. Subsequently, the Ag2S catalyst melted completely into the ZnS NWs at approximately 825 °C. As the temperature further increased, the Ag2S and ZnS NWs continuously melted and vaporized up to 840 °C, leaving only the C shell behind. Finally, a possible growth mechanism was proposed based on the structural and chemical investigations.

  5. In situ transmission electron microscopy studies of microstructure evolution in Ba(Zr0.2Ti0.8)O3-x(Ba0.7Ca0.3)TiO3 piezoceramic

    International Nuclear Information System (INIS)

    Zakhozheva, Marina

    2016-01-01

    The purpose of this work is to understand the microstructural features which contribute to the strong electromechanical properties of the lead-free Ba (Zr 0.2 Ti 0.8 )O 3 -x(Ba 0.7 Ca 0.3 )TiO 3 (BZT-xBCT) piezoelectric ceramic. Detailed conventional transmission electron microscopy (TEM) studies on a broad variety of BZT - xBCT were performed in order to demonstrate the composition dependent structural changes. Moreover, several in situ TEM techniques, including in situ hot- and cold-stage, in situ electric field and in situ electric field with simultaneous cooling, were successfully applied in order to monitor the domain morphology evolution in real time. By means of in situ temperature dependent TEM experiments it was shown that during rhombohedral → orthorhombic → tetragonal phase transition the domain morphology changed according to the crystal structure present. During in situ electric field investigations the displacement of the domain walls and changes in the domain configuration during electrical poling were observed, which indicates a high extrinsic contribution to the piezoelectric response in all BZT - xBCT compositions studied. From the results of in situ electric field TEM experiments with simultaneous cooling, we obtained experimental evidence that the further the composition deviates from the polymorphic phase boundary, the higher the electric field required to fully pole the material.

  6. Nanoparticle Metamorphosis: An in Situ High-Temperature Transmission Electron Microscopy Study of the Structural Evolution of Heterogeneous Au:Fe 2 O 3 Nanoparticles

    KAUST Repository

    Baumgardner, William J.

    2014-05-27

    High-temperature in situ electron microscopy and X-ray diffraction have revealed that Au and Fe2O3 particles fuse in a fluid fashion at temperatures far below their size-reduced melting points. With increasing temperature, the fused particles undergo a sequence of complex structural transformations from surface alloy to phase segregated and ultimately core-shell structures. The combination of in situ electron microscopy and spectroscopy provides insights into fundamental thermodynamic and kinetic aspects governing the formation of heterogeneous nanostructures. The observed structural transformations present an interesting analogy to thin film growth on the curved surface of a nanoparticle. Using single-particle observations, we constructed a phase diagram illustrating the complex relationships among composition, morphology, temperature, and particle size. © 2014 American Chemical Society.

  7. Nanoparticle Metamorphosis: An in Situ High-Temperature Transmission Electron Microscopy Study of the Structural Evolution of Heterogeneous Au:Fe 2 O 3 Nanoparticles

    KAUST Repository

    Baumgardner, William J.; Yu, Yingchao; Hovden, Robert; Honrao, Shreyas; Hennig, Richard G.; Abruñ a, Hé ctor D.; Muller, David; Hanrath, Tobias

    2014-01-01

    High-temperature in situ electron microscopy and X-ray diffraction have revealed that Au and Fe2O3 particles fuse in a fluid fashion at temperatures far below their size-reduced melting points. With increasing temperature, the fused particles undergo a sequence of complex structural transformations from surface alloy to phase segregated and ultimately core-shell structures. The combination of in situ electron microscopy and spectroscopy provides insights into fundamental thermodynamic and kinetic aspects governing the formation of heterogeneous nanostructures. The observed structural transformations present an interesting analogy to thin film growth on the curved surface of a nanoparticle. Using single-particle observations, we constructed a phase diagram illustrating the complex relationships among composition, morphology, temperature, and particle size. © 2014 American Chemical Society.

  8. Using environmental transmission electron microscope to study the in-situ reduction of Co3O4 supported on α-Al2O3

    DEFF Research Database (Denmark)

    Dehghan-Niri, R.; Hansen, Thomas Willum; Wagner, Jakob Birkedal

    in specialized Transmission Electron Microscope (TEM) instruments with differentially pumped columns at pressures in the range up to 20 mbar. 1-3 The objective of this work is to study the reduction of Co3O4 nanoparticles directly and observe their morphology and crystallography. The catalysts were produced...... by dispersion of crushed powder directly on steel grids and gold grids. TEM analysis was performed with an FEI TITAN E-cell electron microscope operating at 300 kV. Reduction was done at 360°C and 3.4 mbar H2 flow. The samples were studied before and after reduction by High Resolution TEM (HRTEM) imaging, high...

  9. Transmission electron microscopy of bone

    NARCIS (Netherlands)

    Everts, Vincent; Niehof, Anneke; Tigchelaar-Gutter, Wikky; Beertsen, Wouter

    2012-01-01

    This chapter describes procedures to process mineralized tissues obtained from different sources for transmission electron microscopy (TEM). Methods for fixation, resin embedding, staining of semi-thin sections and ultrathin sections are presented. In addition, attention will be paid to processing

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

    Science.gov (United States)

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

    2017-12-01

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

  11. In situ observation of Cu-Ni alloy nanoparticle formation by X-ray diffraction, X-ray absorption spectroscopy, and transmission electron microscopy: Influence of Cu/Ni ratio

    DEFF Research Database (Denmark)

    Wu, Qiongxiao; Duchstein, Linus Daniel Leonhard; Chiarello, Gian Luca

    2014-01-01

    Silica-supported, bimetallic Cu-Ni nanomaterials were prepared with different ratios of Cu to Ni by incipient wetness impregnation without a specific calcination step before reduction. Different in situ characterization techniques, in particular transmission electron microscopy (TEM), X-ray...... diffraction (XRD), and X-ray absorption spectroscopy (XAS), were applied to follow the reduction and alloying process of Cu-Ni nanoparticles on silica. In situ reduction of Cu-Ni samples with structural characterization by combined synchrotron XRD and XAS reveals a strong interaction between Cu and Ni species......, which results in improved reducibility of the Ni species compared with monometallic Ni. At high Ni concentrations silica-supported Cu-Ni alloys form a homogeneous solid solution of Cu and Ni, whereas at lower Ni contents Cu and Ni are partly segregated and form metallic Cu and Cu-Ni alloy phases. Under...

  12. Fabrication and electric measurements of nanostructures inside transmission electron microscope.

    Science.gov (United States)

    Chen, Qing; Peng, Lian-Mao

    2011-06-01

    Using manipulation holders specially designed for transmission electron microscope (TEM), nanostructures can be characterized, measured, modified and even fabricated in-situ. In-situ TEM techniques not only enable real-time study of structure-property relationships of materials at atomic scale, but also provide the ability to control and manipulate materials and structures at nanoscale. This review highlights in-situ electric measurements and in-situ fabrication and structure modification using manipulation holder inside TEM. Copyright © 2011 Elsevier B.V. All rights reserved.

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

    International Nuclear Information System (INIS)

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

    1985-12-01

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

  14. Development of the Atomic-Resolution Environmental Transmission Electron Microscope

    DEFF Research Database (Denmark)

    Gai, Pratibha L.; Boyes, Edward D.; Yoshida, Kenta

    2016-01-01

    The development of the novel atomic-resolution environmental transmission electron microscope (atomic-resolution ETEM) for directly probing dynamic gas–solid reactions in situ at the atomic level under controlled reaction conditions consisting of gas environment and elevated temperatures is descr......The development of the novel atomic-resolution environmental transmission electron microscope (atomic-resolution ETEM) for directly probing dynamic gas–solid reactions in situ at the atomic level under controlled reaction conditions consisting of gas environment and elevated temperatures...... is used to study steels, graphene, nanowires, etc. In this chapter, the experimental setup of the microscope column and its peripherals are described....

  15. Fabrication and electric measurements of nanostructures inside transmission electron microscope

    International Nuclear Information System (INIS)

    Chen, Qing; Peng, Lian-Mao

    2011-01-01

    Using manipulation holders specially designed for transmission electron microscope (TEM), nanostructures can be characterized, measured, modified and even fabricated in-situ. In-situ TEM techniques not only enable real-time study of structure-property relationships of materials at atomic scale, but also provide the ability to control and manipulate materials and structures at nanoscale. This review highlights in-situ electric measurements and in-situ fabrication and structure modification using manipulation holder inside TEM. -- Research highlights: → We review in-situ works using manipulation holder in TEM. → In-situ electric measurements, fabrication and structure modification are focused. → We discuss important issues that should be considered for reliable results. → In-situ TEM is becoming a very powerful tool for many research fields.

  16. In-situ transmission electron microscopy study of ion-irradiated copper : comparison of the temperature dependence of cascade collapse in FCC- and BCC- metals.

    Energy Technology Data Exchange (ETDEWEB)

    Daulton, T. L.

    1998-10-23

    The kinetics which drive cascade formation and subsequent collapse into point-defect clusters is investigated by analyzing the microstructure produced in situ by low fluence 100 keV Kr ion irradiations of fcc-Cu over a wide temperature range (18-873 K). The yield of collapsed point-defect clusters is demonstrated unequivocally to be temperature dependent, remaining approximately constant up to lattice temperatures of 573 K and then abruptly decreasing with increasing temperature. This drop in yield is not caused by defect loss during or following ion irradiation. This temperature dependence can be explained by a thermal spike effect. These in-situ yield measurements are compared to previous ex-situ yield measurements in fcc-Ni and bcc-Mo.

  17. In situ transmission electron microscopy study of ion-irradiated copper: comparison of the temperature dependence of cascade collapse in fcc- and bcc-metals

    International Nuclear Information System (INIS)

    Daulton, T.L.; Kirk, M.A.; Rehn, L.E.

    2000-01-01

    The kinetics which drive cascade formation and subsequent collapse into point-defect clusters are investigated by analyzing the microstructure produced in situ by low fluence 100 keV Kr ion irradiations of fcc-Cu over a wide temperature range (18-873 K). The yield of collapsed point-defect clusters is demonstrated unequivocally to be temperature dependent, remaining approximately constant up to lattice temperatures of 573 K and then abruptly decreasing with increasing temperature. This drop in yield is not caused by defect loss during or following ion irradiation. In addition, this temperature dependence can be explained by a thermal spike effect. These in situ yield measurements are compared to previous ex situ yield measurements in fcc-Ni and bcc-Mo

  18. Direct transmission electron microscopy observations of martensitic transformations in Ni-rich NiTi single crystals during in situ cooling and straining

    Czech Academy of Sciences Publication Activity Database

    Kröger, A.; Dziaszyk, S.; Frenzel, J.; Somsen, Ch.; Dlouhý, Antonín; Eggeler, G.

    2008-01-01

    Roč. 481, Sp. Iss. (2008), s. 452-456 ISSN 0921-5093. [ESOMAT 2006. Bochum, 10.09.2006-15.09.2006] Institutional research plan: CEZ:AV0Z20410507 Keywords : In situ TEM * NiTi single crystal * Martensitic transformations Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.806, year: 2008

  19. Monochromated scanning transmission electron microscopy

    International Nuclear Information System (INIS)

    Rechberger, W.; Kothleitner, G.; Hofer, F.

    2006-01-01

    Full text: Electron energy-loss spectroscopy (EELS) has developed into an established technique for chemical and structural analysis of thin specimens in the (scanning) transmission electron microscope (S)TEM. The energy resolution in EELS is largely limited by the stability of the high voltage supply, by the resolution of the spectrometer and by the energy spread of the source. To overcome this limitation a Wien filter monochromator was recently introduced with commercially available STEMs, offering the advantage to better resolve EELS fine structures, which contain valuable bonding information. The method of atomic resolution Z-contrast imaging within an STEM, utilizing a high-angle annular dark-field (HAADF) detector can perfectly complement the excellent energy resolution, since EELS spectra can be collected simultaneously. In combination with a monochromator microscope not only high spatial resolution images can be recorded but also high energy resolution EELS spectra are attainable. In this work we investigated the STEM performance of a 200 kV monochromated Tecnai F20 with a high resolution Gatan Imaging Filter (HR-GIF). (author)

  20. In-situ transmission electron microscopy study of glissile grain boundary dislocation relaxation in a near Σ = 3 {1 1 1} grain boundary in copper

    International Nuclear Information System (INIS)

    Couzinie, J.P.; Decamps, B.; Boulanger, L.; Priester, L.

    2005-01-01

    An in-situ annealing experiment has been performed on an intergranular dislocation configuration composed only of glissile grain boundary dislocations observed in a near Σ = 3 {1 1 1} grain boundary in copper. Relaxation phenomena are not obvious than those predicted by theoretical models. Upon annealing, glissile intergranular dislocations are shown to overcome dislocation obstacles by node movement leading to a decrease of the total grain boundary energy

  1. Stress-induced martensitic transformations in a Cu-Al-Ni shape memory alloy studied by in situ transmission electron microscopy

    Czech Academy of Sciences Publication Activity Database

    Zárubová, Niva; Gemperlová, Juliana; Gärtnerová, Viera; Gemperle, Antonín

    481-482, č. 5 (2008), s. 457-461 ISSN 0921-5093 R&D Projects: GA ČR GA202/04/2016; GA AV ČR(CZ) IAA200100627 Institutional research plan: CEZ:AV0Z10100520 Keywords : in situ TEM straining * CuAlNi shape memory alloy * stress -induced formation of martensite Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.806, year: 2008

  2. A Discovery of Strong Metal-Support Bonding in Nanoengineered Au-Fe3O4 Dumbbell-like Nanoparticles by in Situ Transmission Electron Microscopy.

    Science.gov (United States)

    Han, Chang Wan; Choksi, Tej; Milligan, Cory; Majumdar, Paulami; Manto, Michael; Cui, Yanran; Sang, Xiahan; Unocic, Raymond R; Zemlyanov, Dmitry; Wang, Chao; Ribeiro, Fabio H; Greeley, Jeffrey; Ortalan, Volkan

    2017-08-09

    The strength of metal-support bonding in heterogeneous catalysts determines their thermal stability, therefore, a tremendous amount of effort has been expended to understand metal-support interactions. Herein, we report the discovery of an anomalous "strong metal-support bonding" between gold nanoparticles and "nano-engineered" Fe 3 O 4 substrates by in situ microscopy. During in situ vacuum annealing of Au-Fe 3 O 4 dumbbell-like nanoparticles, synthesized by the epitaxial growth of nano-Fe 3 O 4 on Au nanoparticles, the gold nanoparticles transform into the gold thin films and wet the surface of nano-Fe 3 O 4 , as the surface reduction of nano-Fe 3 O 4 proceeds. This phenomenon results from a unique coupling of the size-and shape-dependent high surface reducibility of nano-Fe 3 O 4 and the extremely strong adhesion between Au and the reduced Fe 3 O 4 . This strong metal-support bonding reveals the significance of controlling the metal oxide support size and morphology for optimizing metal-support bonding and ultimately for the development of improved catalysts and functional nanostructures.

  3. Transmission Electron Microscopy Physics of Image Formation

    CERN Document Server

    Kohl, Helmut

    2008-01-01

    Transmission Electron Microscopy: Physics of Image Formation presents the theory of image and contrast formation, and the analytical modes in transmission electron microscopy. The principles of particle and wave optics of electrons are described. Electron-specimen interactions are discussed for evaluating the theory of scattering and phase contrast. Also discussed are the kinematical and dynamical theories of electron diffraction and their applications for crystal-structure analysis and imaging of lattices and their defects. X-ray microanalysis and electron energy-loss spectroscopy are treated as analytical methods. Specimen damage and contamination by electron irradiation limits the resolution for biological and some inorganic specimens. This fifth edition includes discussion of recent progress, especially in the area of aberration correction and energy filtering; moreover, the topics introduced in the fourth edition have been updated. Transmission Electron Microscopy: Physics of Image Formation is written f...

  4. Transmission electron microscopy characterization of photocatalysts for water splitting

    DEFF Research Database (Denmark)

    Cavalca, Filippo; Laursen, Anders Bo; Dahl, Søren

    , it is necessary to understand the fundamentals of their reaction mechanisms, chemical behavior, structure and morphology before, during and after reaction using in situ investigations. Here, we focus on the in situ characterization of photocatalysts [1] in an environmental transmission electron microscope (ETEM......) [2]. Such fundamental insight can be used for further material optimization with respect to performance and stability [3]. In this work, we combine conventional TEM analysis of photocatalysts with environmental TEM (ETEM) and photoactivation using light. A novel type of TEM specimen holder...... that enables in situ illumination is developed to study light-induced phenomena in photoactive materials at the nanoscale under working conditions. Our experiments are aimed at exposing a specimen to light and detecting resulting microstructural and chemical changes using in situ TEM techniques...

  5. Transmission electron microscope CCD camera

    Science.gov (United States)

    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.

  6. Transmission electron microscope studies of extraterrestrial materials

    Science.gov (United States)

    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.

  7. Design of a transmission electron positron microscope

    International Nuclear Information System (INIS)

    Doyama, Masao; Inoue, M.; Kogure, Y.; Hayashi, Y.; Yoshii, T.; Kurihara, T.; Tsuno, K.

    2003-01-01

    This paper reports the plans and design of positron-electron microscopes being built at KEK (High Energy Accelerator Research Organization), Tsukuba, Japan. A used electron microscope is altered. The kinetic energies of positrons produced by accelerators or by nuclear decays are not a unique value but show a spread over in a wide range. Positron beam is guided to a transmission electron microscope (JEM100SX). Positrons are moderated by a tungsten foil, are accelerated and are focused on a nickel sheet. The monochromatic focused beam is injected into an electron microscope. The focusing and aberration of positrons are the same as electrons in a magnetic system which are used in commercial electron microscopes. Imaging plates are used to record positron images for the transmission electron microscope. (author)

  8. Oxidation mechanism of nickel particles studied in an environmental transmission electron microscope

    DEFF Research Database (Denmark)

    Jeangros, Q.; Hansen, Thomas Willum; Wagner, Jakob Birkedal

    2014-01-01

    The oxidation of nickel particles was studied in situ in an environmental transmission electron microscope in 3.2 mbar of O2 between ambient temperature and 600°C. Several different transmission electron microscopy imaging techniques, electron diffraction and electron energy-loss spectroscopy were...... diffusion of Ni2+ along NiO grain boundaries, self-diffusion of Ni2+ ions and vacancies, growth of NiO grains and nucleation of voids at Ni/NiO interfaces. We also observed the formation of transverse cracks in a growing NiO film in situ in the electron microscope....

  9. New developments in transmission electron microscopy for nanotechnology

    International Nuclear Information System (INIS)

    Wang, Z.L.

    2003-01-01

    High-resolution transmission electron microscopy (HRTEM) is one of the most powerful tools used for characterizing nanomaterials, and it is indispensable for nanotechnology. This paper reviews some of the most recent developments in electron microscopy techniques for characterizing nanomaterials. The review covers the following areas: in-situ microscopy for studying dynamic shape transformation of nanocrystals; in-situ nanoscale property measurements on the mechanical, electrical and field emission properties of nanotubes/nanowires; environmental microscopy for direct observation of surface reactions; aberration-free angstrom-resolution imaging of light elements (such as oxygen and lithium); high-angle annular-dark-field scanning transmission electron microscopy (STEM); imaging of atom clusters with atomic resolution chemical information; electron holography of magnetic materials; and high-spatial resolution electron energy-loss spectroscopy (EELS) for nanoscale electronic and chemical analysis. It is demonstrated that the picometer-scale science provided by HRTEM is the foundation of nanometer-scale technology. (Abstract Copyright [2003], Wiley Periodicals, Inc.)

  10. Transmission electron microscopy of amyloid fibrils.

    Science.gov (United States)

    Gras, Sally L; Waddington, Lynne J; Goldie, Kenneth N

    2011-01-01

    Transmission Electron Microscopy of negatively stained and cryo-prepared specimens allows amyloid fibrils to be visualised at high resolution in a dried or a hydrated state, and is an essential method for characterising the morphology of fibrils and pre-fibrillar species. We outline the key steps involved in the preparation and observation of samples using negative staining and cryo-electron preservation. We also discuss methods to measure fibril characteristics, such as fibril width, from electron micrographs.

  11. Exploring the environmental transmission electron microscope

    DEFF Research Database (Denmark)

    Wagner, Jakob B.; Cavalca, Filippo; Damsgaard, Christian D.

    2012-01-01

    of the opportunities that the environmental TEM (ETEM) offers when combined with other in situ techniques will be explored, directly in the microscope, by combining electron-based and photon-based techniques and phenomena. In addition, application of adjacent setups using sophisticated transfer methods...

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

    Energy Technology Data Exchange (ETDEWEB)

    Zakhozheva, Marina

    2016-10-21

    The purpose of this work is to understand the microstructural features which contribute to the strong electromechanical properties of the lead-free Ba (Zr{sub 0.2}Ti{sub 0.8})O{sub 3}-x(Ba{sub 0.7}Ca{sub 0.3})TiO{sub 3} (BZT-xBCT) piezoelectric ceramic. Detailed conventional transmission electron microscopy (TEM) studies on a broad variety of BZT - xBCT were performed in order to demonstrate the composition dependent structural changes. Moreover, several in situ TEM techniques, including in situ hot- and cold-stage, in situ electric field and in situ electric field with simultaneous cooling, were successfully applied in order to monitor the domain morphology evolution in real time. By means of in situ temperature dependent TEM experiments it was shown that during rhombohedral → orthorhombic → tetragonal phase transition the domain morphology changed according to the crystal structure present. During in situ electric field investigations the displacement of the domain walls and changes in the domain configuration during electrical poling were observed, which indicates a high extrinsic contribution to the piezoelectric response in all BZT - xBCT compositions studied. From the results of in situ electric field TEM experiments with simultaneous cooling, we obtained experimental evidence that the further the composition deviates from the polymorphic phase boundary, the higher the electric field required to fully pole the material.

  13. Quantitative transmission electron microscopy at atomic resolution

    International Nuclear Information System (INIS)

    Allen, L J; D'Alfonso, A J; Forbes, B D; Findlay, S D; LeBeau, J M; Stemmer, S

    2012-01-01

    In scanning transmission electron microscopy (STEM) it is possible to operate the microscope in bright-field mode under conditions which, by the quantum mechanical principle of reciprocity, are equivalent to those in conventional transmission electron microscopy (CTEM). The results of such an experiment will be presented which are in excellent quantitative agreement with theory for specimens up to 25 nm thick. This is at variance with the large contrast mismatch (typically between two and five) noted in equivalent CTEM experiments. The implications of this will be discussed.

  14. Time resolved electron microscopy for in situ experiments

    International Nuclear Information System (INIS)

    Campbell, Geoffrey H.; McKeown, Joseph T.; Santala, Melissa K.

    2014-01-01

    Transmission electron microscopy has functioned for decades as a platform for in situ observation of materials and processes with high spatial resolution. Yet, the dynamics often remain elusive, as they unfold too fast to discern at these small spatial scales under traditional imaging conditions. Simply shortening the exposure time in hopes of capturing the action has limitations, as the number of electrons will eventually be reduced to the point where noise overtakes the signal in the image. Pulsed electron sources with high instantaneous current have successfully shortened exposure times (thus increasing the temporal resolution) by about six orders of magnitude over conventional sources while providing the necessary signal-to-noise ratio for dynamic imaging. We describe here the development of this new class of microscope and the principles of its operation, with examples of its application to problems in materials science

  15. Time resolved electron microscopy for in situ experiments

    Energy Technology Data Exchange (ETDEWEB)

    Campbell, Geoffrey H., E-mail: ghcampbell@llnl.gov; McKeown, Joseph T.; Santala, Melissa K. [Lawrence Livermore National Laboratory, Livermore, California 94550 (United States)

    2014-12-15

    Transmission electron microscopy has functioned for decades as a platform for in situ observation of materials and processes with high spatial resolution. Yet, the dynamics often remain elusive, as they unfold too fast to discern at these small spatial scales under traditional imaging conditions. Simply shortening the exposure time in hopes of capturing the action has limitations, as the number of electrons will eventually be reduced to the point where noise overtakes the signal in the image. Pulsed electron sources with high instantaneous current have successfully shortened exposure times (thus increasing the temporal resolution) by about six orders of magnitude over conventional sources while providing the necessary signal-to-noise ratio for dynamic imaging. We describe here the development of this new class of microscope and the principles of its operation, with examples of its application to problems in materials science.

  16. Transmission Electron Microscope Measures Lattice Parameters

    Science.gov (United States)

    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.

  17. Ponderomotive phase plate for transmission electron microscopes

    Science.gov (United States)

    Reed, Bryan W [Livermore, CA

    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.

  18. Isotope analysis in the transmission electron microscope.

    Science.gov (United States)

    Susi, Toma; Hofer, Christoph; Argentero, Giacomo; Leuthner, Gregor T; Pennycook, Timothy J; Mangler, Clemens; Meyer, Jannik C; Kotakoski, Jani

    2016-10-10

    The Ångström-sized probe of the scanning transmission electron microscope can visualize and collect spectra from single atoms. This can unambiguously resolve the chemical structure of materials, but not their isotopic composition. Here we differentiate between two isotopes of the same element by quantifying how likely the energetic imaging electrons are to eject atoms. First, we measure the displacement probability in graphene grown from either 12 C or 13 C and describe the process using a quantum mechanical model of lattice vibrations coupled with density functional theory simulations. We then test our spatial resolution in a mixed sample by ejecting individual atoms from nanoscale areas spanning an interface region that is far from atomically sharp, mapping the isotope concentration with a precision better than 20%. Although we use a scanning instrument, our method may be applicable to any atomic resolution transmission electron microscope and to other low-dimensional materials.

  19. Interaction of electrons with light metal hydrides in the transmission electron microscope.

    Science.gov (United States)

    Wang, Yongming; Wakasugi, Takenobu; Isobe, Shigehito; Hashimoto, Naoyuki; Ohnuki, Somei

    2014-12-01

    Transmission electron microscope (TEM) observation of light metal hydrides is complicated by the instability of these materials under electron irradiation. In this study, the electron kinetic energy dependences of the interactions of incident electrons with lithium, sodium and magnesium hydrides, as well as the constituting element effect on the interactions, were theoretically discussed, and electron irradiation damage to these hydrides was examined using in situ TEM. The results indicate that high incident electron kinetic energy helps alleviate the irradiation damage resulting from inelastic or elastic scattering of the incident electrons in the TEM. Therefore, observations and characterizations of these materials would benefit from increased, instead decreased, TEM operating voltage. © The Author 2014. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

  20. Elemental mapping in scanning transmission electron microscopy

    International Nuclear Information System (INIS)

    Allen, L J; D'Alfonso, A J; Lugg, N R; Findlay, S D; LeBeau, J M; Stemmer, S

    2010-01-01

    We discuss atomic resolution chemical mapping in scanning transmission electron microscopy (STEM) based on core-loss electron energy loss spectroscopy (EELS) and also on energy dispersive X-ray (EDX) imaging. Chemical mapping using EELS can yield counterintuitive results which, however, can be understood using first principles calculations. Experimental chemical maps based on EDX bear out the thesis that such maps are always likely to be directly interpretable. This can be explained in terms of the local nature of the effective optical potential for ionization under those imaging conditions. This is followed by an excursion into the complementary technique of elemental mapping using energy-filtered transmission electron microscopy (EFTEM) in a conventional transmission electron microscope. We will then consider the widely used technique of Z-contrast or high-angle annular dark field (HAADF) imaging, which is based on phonon excitation, where it has recently been shown that intensity variations can be placed on an absolute scale by normalizing the measured intensities to the incident beam. Results, showing excellent agreement between theory and experiment to within a few percent, are shown for Z-contrast imaging from a sample of PbWO 4 .

  1. Transmission Electron Microscopy of Minerals and Rocks

    Science.gov (United States)

    McLaren, Alex C.

    1991-04-01

    Of the many techniques that have been applied to the study of crystal defects, none has contributed more to our understanding of their nature and influence on the physical and chemical properties of crystalline materials than transmission electron microscopy (TEM). TEM is now used extensively by an increasing number of earth scientists for direct observation of defect microstructures in minerals and rocks. Transmission Electron Microscopy of Rocks and Minerals is an introduction to the principles of the technique and is the only book to date on the subject written specifically for geologists and mineralogists. The first part of the book deals with the essential physics of the transmission electron microscope and presents the basic theoretical background required for the interpretation of images and electron diffraction patterns. The final chapters are concerned with specific applications of TEM in mineralogy and deal with such topics as planar defects, intergrowths, radiation-induced defects, dislocations and deformation-induced microstructures. The examples cover a wide range of rock-forming minerals from crustal rocks to those in the lower mantle, and also take into account the role of defects in important mineralogical and geological processes.

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

    NARCIS (Netherlands)

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

    2017-01-01

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

  3. Transmission electron microscopy in micro-nanoelectronics

    CERN Document Server

    Claverie, Alain

    2013-01-01

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

  4. Transmission Electron Microscopy and Diffractometry of Materials

    CERN Document Server

    Fultz, Brent

    2013-01-01

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

  5. Enhanced thermal stability of a polymer solar cell blend induced by electron beam irradiation in the transmission electron microscope

    Energy Technology Data Exchange (ETDEWEB)

    Bäcke, Olof, E-mail: obacke@chalmers.se [Department of Applied Physics, Chalmers University of Technology, 41296 Göteborg (Sweden); Lindqvist, Camilla; Diaz de Zerio Mendaza, Amaia [Department of Chemistry and Chemical Engineering, Chalmers University of Technology, 41296 Göteborg (Sweden); Gustafsson, Stefan [Department of Applied Physics, Chalmers University of Technology, 41296 Göteborg (Sweden); Wang, Ergang; Andersson, Mats R.; Müller, Christian [Department of Chemistry and Chemical Engineering, Chalmers University of Technology, 41296 Göteborg (Sweden); Kristiansen, Per Magnus [Institute of Polymer Nanotechnology (INKA), FHNW University of Applied Science and Arts Northwestern Switzerland, 5210 Windisch (Switzerland); Laboratory for Micro- and Nanotechnology, Paul Scherrer Institute, 5232 Villigen (Switzerland); Olsson, Eva, E-mail: eva.olsson@chalmers.se [Department of Applied Physics, Chalmers University of Technology, 41296 Göteborg (Sweden)

    2017-05-15

    We show by in situ microscopy that the effects of electron beam irradiation during transmission electron microscopy can be used to lock microstructural features and enhance the structural thermal stability of a nanostructured polymer:fullerene blend. Polymer:fullerene bulk-heterojunction thin films show great promise for use as active layers in organic solar cells but their low thermal stability is a hindrance. Lack of thermal stability complicates manufacturing and influences the lifetime of devices. To investigate how electron irradiation affects the thermal stability of polymer:fullerene films, a model bulk-heterojunction film based on a thiophene-quinoxaline copolymer and a fullerene derivative was heat-treated in-situ in a transmission electron microscope. In areas of the film that exposed to the electron beam the nanostructure of the film remained stable, while the nanostructure in areas not exposed to the electron beam underwent large phase separation and nucleation of fullerene crystals. UV–vis spectroscopy shows that the polymer:fullerene films are stable for electron doses up to 2000 kGy. - Highlights: • Thermal stability of a polymer: fullerne blend is increased using electron irradiation. • Using in-situ transmission electron microscopy the nanostructure is studied. • Electron irradiation stops phase separation between the polymer and fullerene. • Electron irradiation quenches the formation and nucleation of fullerene crystals.

  6. In Situ Electron Microscopy of Lactomicroselenium Particles in Probiotic Bacteria

    Directory of Open Access Journals (Sweden)

    Gabor Nagy

    2016-06-01

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

  7. Transmission electron microscopy of mercury metal

    KAUST Repository

    Anjum, Dalaver H.

    2016-03-28

    Summary: 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. © 2016 Royal Microscopical Society.

  8. Transmission electron microscope studies of crystalline LiNbO3

    International Nuclear Information System (INIS)

    Pareja, R.; Gonzalez, R.; Chen, Y.

    1984-01-01

    Transmission electron microscope investigations in both as-grown and hydrogen-reduced LiNbO 3 reveal that niobium oxide precipitates can be produced by in situ irradiations in the electron microscope. The precipitation process is produced by a combined effect of ionizing electrons and the thermal heating of the specimens during irradiation. It is proposed that the composition of the precipitates is primarily Nb 2 O 5

  9. Cathodoluminescence in the scanning transmission electron microscope

    Energy Technology Data Exchange (ETDEWEB)

    Kociak, M., E-mail: mathieu.kociak@u-psud.fr [Laboratoire de Physique des Solides, Université Paris-SudParis-Sud, CNRS-UMR 8502, Orsay 91405 (France); Zagonel, L.F. [“Gleb Wataghin” Institute of Physics University of Campinas - UNICAMP, 13083-859 Campinas, São Paulo (Brazil)

    2017-05-15

    Cathodoluminescence (CL) is a powerful tool for the investigation of optical properties of materials. In recent years, its combination with scanning transmission electron microscopy (STEM) has demonstrated great success in unveiling new physics in the field of plasmonics and quantum emitters. Most of these results were not imaginable even twenty years ago, due to conceptual and technical limitations. The purpose of this review is to present the recent advances that broke these limitations, and the new possibilities offered by the modern STEM-CL technique. We first introduce the different STEM-CL operating modes and the technical specificities in STEM-CL instrumentation. Two main classes of optical excitations, namely the coherent one (typically plasmons) and the incoherent one (typically light emission from quantum emitters) are investigated with STEM-CL. For these two main classes, we describe both the physics of light production under electron beam irradiation and the physical basis for interpreting STEM-CL experiments. We then compare STEM-CL with its better known sister techniques: scanning electron microscope CL, photoluminescence, and electron energy-loss spectroscopy. We finish by comprehensively reviewing recent STEM-CL applications. - Highlights: • Reviews the field of STEM-CL. • Introduces the technical requirements and challenges for STEM-CL. • Introduces the different types of excitations probed by STEM-CL. • Gives comprehensive overview of the last fifteenth years in the field.

  10. Quantitative biological measurement in Transmission Electron Tomography

    International Nuclear Information System (INIS)

    Mantell, Judith M; Verkade, Paul; Arkill, Kenton P

    2012-01-01

    It has been known for some time that biological sections shrink in the transmission electron microscope from exposure to the electron beam. This phenomenon is especially important in Electron Tomography (ET). The effect on shrinkage of parameters such as embedding medium or sample type is less well understood. In addition anisotropic area shrinkage has largely been ignored. The intention of this study is to explore the shrinkage on a number of samples ranging in thickness from 200 nm to 500 nm. A protocol was developed to determine the shrinkage in area and thickness using the gold fiducials used in electron tomography. In brief: Using low dose philosophy on the section, a focus area was used prior to a separate virgin study area for a series of known exposures on a tilted sample. The shrinkage was determined by measurements on the gold beads from both sides of the section as determined by a confirmatory tomogram. It was found that the shrinkage in area (approximately to 90-95% of the original) and the thickness (approximately 65% of the original at most) agreed with pervious authors, but that a lmost all the shrinkage was in the first minute and that although the direction of the in-plane shrinkage (in x and y) was sometimes uneven the end result was consistent. It was observed, in general, that thinner samples showed more percentage shrinkage than thicker ones. In conclusion, if direct quantitative measurements are required then the protocol described should be used for all areas studied.

  11. Quantitative biological measurement in Transmission Electron Tomography

    Science.gov (United States)

    Mantell, Judith M.; Verkade, Paul; Arkill, Kenton P.

    2012-07-01

    It has been known for some time that biological sections shrink in the transmission electron microscope from exposure to the electron beam. This phenomenon is especially important in Electron Tomography (ET). The effect on shrinkage of parameters such as embedding medium or sample type is less well understood. In addition anisotropic area shrinkage has largely been ignored. The intention of this study is to explore the shrinkage on a number of samples ranging in thickness from 200 nm to 500 nm. A protocol was developed to determine the shrinkage in area and thickness using the gold fiducials used in electron tomography. In brief: Using low dose philosophy on the section, a focus area was used prior to a separate virgin study area for a series of known exposures on a tilted sample. The shrinkage was determined by measurements on the gold beads from both sides of the section as determined by a confirmatory tomogram. It was found that the shrinkage in area (approximately to 90-95% of the original) and the thickness (approximately 65% of the original at most) agreed with pervious authors, but that a lmost all the shrinkage was in the first minute and that although the direction of the in-plane shrinkage (in x and y) was sometimes uneven the end result was consistent. It was observed, in general, that thinner samples showed more percentage shrinkage than thicker ones. In conclusion, if direct quantitative measurements are required then the protocol described should be used for all areas studied.

  12. Characterization of nanomaterials with transmission electron microscopy

    KAUST Repository

    Anjum, Dalaver H.

    2016-08-01

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

  13. Thermal diffuse scattering in transmission electron microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Forbes, B.D.; D' Alfonso, A.J. [School of Physics, University of Melbourne, Parkville, Victoria 3010 (Australia); Findlay, S.D. [School of Physics, Monash University, Victoria 3800 (Australia); Van Dyck, D. [EMAT, University of Antwerp, Groenenborgerlaan 171, B-2020 Antwerp (Belgium); LeBeau, J.M. [North Carolina State University, Raleigh, NC 27695-7907 (United States); Stemmer, S. [Materials Department, University of California, Santa Barbara, CA 93106-5050 (United States); Allen, L.J., E-mail: lja@unimelb.edu.au [School of Physics, University of Melbourne, Parkville, Victoria 3010 (Australia)

    2011-12-15

    In conventional transmission electron microscopy, thermal scattering significantly affects the image contrast. It has been suggested that not accounting for this correctly is the main cause of the Stobbs factor, the ubiquitous, large contrast mismatch found between theory and experiment. In the case where a hard aperture is applied, we show that previous conclusions drawn from work using bright field scanning transmission electron microscopy and invoking the principle of reciprocity are reliable in the presence of thermal scattering. In the aperture-free case it has been suggested that even the most sophisticated mathematical models for thermal diffuse scattering lack in their numerical implementation, specifically that there may be issues in sampling, including that of the contrast transfer function of the objective lens. We show that these concerns can be satisfactorily overcome with modest computing resources; thermal scattering can be modelled accurately enough for the purpose of making quantitative comparison between simulation and experiment. Spatial incoherence of the source is also investigated. Neglect or inadequate handling of thermal scattering in simulation can have an appreciable effect on the predicted contrast and can be a significant contribution to the Stobbs factor problem. -- Highlights: Black-Right-Pointing-Pointer We determine the numerical requirements for accurate simulation of TDS in CTEM. Black-Right-Pointing-Pointer TDS can be simulated to high precision using the Born-Oppenheimer model. Black-Right-Pointing-Pointer Such calculations establish the contribution of TDS to the Stobbs factor problem. Black-Right-Pointing-Pointer Treating spatial incoherence using envelope functions increases image contrast. Black-Right-Pointing-Pointer Rigorous treatment of spatial incoherence significantly reduces image contrast.

  14. Desorption of hydrogen from magnesium hydride: in-situ electron diffraction study

    International Nuclear Information System (INIS)

    Paik, B.; Jones, I.P.; Walton, A.; Mann, V.; Book, D.; Harris, I.R.

    2009-01-01

    The dynamics of a phase change has been studied where electron beam in Transmission Electron Microscope (TEM) has been used to transform MgH 2 into magnesium. A combination of in-situ Electron Diffraction (ED) and an in-situ Electron Energy Loss Spectroscopy (EELS) study under ED mode describes the phase transformation in terms of, respectively, change in the crystal structure and Plasmon energy shift. The orientation relation [001] MgH2 //[-2110] Mg and (-110) MgH2 //(0001) Mg , obtained from the ED study, has been used to propose a model for the movements of magnesium atoms in the structural change to describe the dynamics of the process. The in-situ EELS study has been compared with the existing H-desorption model. The study aims to describe the sorption dynamics of hydrogen in MgH 2 which is a base material for a number of promising hydrogen storage systems. (author)

  15. Transmission electron microscope interfaced with ion accelerators and its application to materials science

    Energy Technology Data Exchange (ETDEWEB)

    Abe, Hiroaki; Naramoto, Hiroshi [Japan Atomic Energy Research Inst., Takasaki, Gunma (Japan). Takasaki Radiation Chemistry Research Establishment; Hojou, Kiichi; Furuno, Shigemi; Tsukamoto, Tetsuo

    1997-03-01

    We have developed the transmission/analytical electron microscope interfaced with two sets of ion accelerators (TEM-Accelerators Facility) at JAERI-Takasaki. The facility is expected to provide quantitative insights into radiation effects, such as damage evolution, irradiation-induced phase transformation and their stability, through in-situ observation and analysis under ion and/or electron irradiation. The TEM-Accelerators Facility and its application to materials research are reviewed. (author)

  16. Transmission of electrons through Al2O3 nanocapillaries

    DEFF Research Database (Denmark)

    Milosavljević, A.R.; Jureta, J.J.; Víkor, Gy.

    2012-01-01

    We investigate transmission of low-energy electrons (250 eV) through insulating AlO nanocapillaries (270 nm diameter and 15 μm length). Kinetic energy distribution of electrons transmitted through the nanocapillaries in the straightforward direction, time dependence of the transmission rate both...

  17. Transmission electron microscopy physics of image formation and microanalysis

    CERN Document Server

    Reimer, Ludwig

    1993-01-01

    "Transmission Electron Microscopy" presents the theory of image and contrastformation, and the analytical modes in transmission electron microscopy Theprinciples of particle and wave optics of electrons are described Electron-specimen interactions are discussed for evaluating the theory of scattering and phase contrast Also analysed are the kinetical and dynamical theories of electron diffraction and their applications for crystal-structure determination and imaging of lattices and their defects X-ray microanalysis and electron energy-loss spectroscopy are treated as analytical methods The third edition includes a brief discussionof Schottky emission guns, some clarification of minor details, and references to the recent literature

  18. In situ mechanical TEM: seeing and measuring under stress with electrons

    International Nuclear Information System (INIS)

    Legros, M.

    2014-01-01

    From the first observation of moving dislocations in 1956 to the latest developments of piezo-actuated sample holders and direct electron sensing cameras in modern transmission electron microscopes (TEM), in situ mechanical testing has brought an unequaled view of the involved mechanisms during the plastic deformation of materials. Although MEMS-based or load-cell equipped holders provide an almost direct measure of these quantities, deriving stress and strain from in situ TEM experiments has an extensive history. Nowadays, the realization of a complete mechanical test while observing the evolution of a dislocation structure is possible, and it constitutes the perfect combination to explore size effects in plasticity. New cameras, data acquisition rates and intrinsic image-related techniques, such as holography, should extend the efficiency and capabilities of in situ deformation inside a TEM. (author)

  19. An electromechanical material testing system for in situ electron microscopy and applications.

    Science.gov (United States)

    Zhu, Yong; Espinosa, Horacio D

    2005-10-11

    We report the development of a material testing system for in situ electron microscopy (EM) mechanical testing of nanostructures. The testing system consists of an actuator and a load sensor fabricated by means of surface micromachining. This previously undescribed nanoscale material testing system makes possible continuous observation of the specimen deformation and failure with subnanometer resolution, while simultaneously measuring the applied load electronically with nanonewton resolution. This achievement was made possible by the integration of electromechanical and thermomechanical components based on microelectromechanical system technology. The system capabilities are demonstrated by the in situ EM testing of free-standing polysilicon films, metallic nanowires, and carbon nanotubes. In particular, a previously undescribed real-time instrumented in situ transmission EM observation of carbon nanotubes failure under tensile load is presented here.

  20. In situ electron backscattered diffraction of individual GaAs nanowires

    Energy Technology Data Exchange (ETDEWEB)

    Prikhodko, S.V. [Department of Materials Science and Engineering, University of California Los Angeles, Los Angeles, CA 90095 (United States)], E-mail: sergey@seas.ucla.edu; Sitzman, S. [Oxford Instruments America, Concord, MA 01742 (United States); Gambin, V. [Northrop Grumman Space Technology, Redondo Beach, CA 90278 (United States); Kodambaka, S. [Department of Materials Science and Engineering, University of California Los Angeles, Los Angeles, CA 90095 (United States)

    2008-12-15

    We suggest and demonstrate that electron backscattered diffraction, a scanning electron microscope-based technique, can be used for non-destructive structural and morphological characterization of statistically significant number of nanowires in situ on their growth substrate. We obtain morphological, crystal phase, and crystal orientation information of individual GaAs nanowires in situ on the growth substrate GaAs(1 1 1) B. Our results, verified using transmission electron microscopy and selected area electron diffraction analyses of the same set of wires, indicate that most wires possess a wurtzite structure with a high density of thin structural defects aligned normal to the wire growth axis, while others grow defect-free with a zincblende structure. The demonstrated approach is general, applicable to other material systems, and is expected to provide important insights into the role of substrate structure on nanowire structure on nanowire crystallinity and growth orientation.

  1. Transmission electron microscopy on live catalysts

    NARCIS (Netherlands)

    Bremmer, G.M.

    2017-01-01

    The dissertation describes TEM experiments on heterogeneous catalysts. Starting with characterization of (Ni/Co)MoS2 on Alumina and the effect of oxidation, and sequential resulfidation. After that, Co-based catalysts are used for high-resolution (S)TEM/EDX caracterization studies, and in situ

  2. Transmission Electron Microscopy of Itokawa Regolith Grains

    Science.gov (United States)

    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

  3. In situ electron beam irradiated rapid growth of bismuth nanoparticles in bismuth-based glass dielectrics at room temperature

    International Nuclear Information System (INIS)

    Singh, Shiv Prakash; Karmakar, Basudeb

    2011-01-01

    In this study, in situ control growth of bismuth nanoparticles (Bi 0 NPs) was demonstrated in bismuth-based glass dielectrics under an electron beam (EB) irradiation at room temperature. The effects of EB irradiation were investigated in situ using transmission electron microscopy (TEM), selected-area electron diffraction and high-resolution transmission electron microscopy. The EB irradiation for 2–8 min enhanced the construction of bismuth nanoparticles with a rhombohedral structure and diameter of 4–9 nm. The average particle size was found to increase with the irradiation time. Bismuth metal has a melting point of 271 °C and this low melting temperature makes easy the progress of energy induced structural changes during in situ TEM observations. This is a very useful technique in nano-patterning for integrated optics and other applications.

  4. Enhanced thermal stability of a polymer solar cell blend induced by electron beam irradiation in the transmission electron microscope.

    Science.gov (United States)

    Bäcke, Olof; Lindqvist, Camilla; de Zerio Mendaza, Amaia Diaz; Gustafsson, Stefan; Wang, Ergang; Andersson, Mats R; Müller, Christian; Kristiansen, Per Magnus; Olsson, Eva

    2017-05-01

    We show by in situ microscopy that the effects of electron beam irradiation during transmission electron microscopy can be used to lock microstructural features and enhance the structural thermal stability of a nanostructured polymer:fullerene blend. Polymer:fullerene bulk-heterojunction thin films show great promise for use as active layers in organic solar cells but their low thermal stability is a hindrance. Lack of thermal stability complicates manufacturing and influences the lifetime of devices. To investigate how electron irradiation affects the thermal stability of polymer:fullerene films, a model bulk-heterojunction film based on a thiophene-quinoxaline copolymer and a fullerene derivative was heat-treated in-situ in a transmission electron microscope. In areas of the film that exposed to the electron beam the nanostructure of the film remained stable, while the nanostructure in areas not exposed to the electron beam underwent large phase separation and nucleation of fullerene crystals. UV-vis spectroscopy shows that the polymer:fullerene films are stable for electron doses up to 2000kGy. Copyright © 2016 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

    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

  6. Transmission electron microscopy physics of image formation and microanalysis

    CERN Document Server

    Reimer, Ludwig

    1997-01-01

    Transmission Electron Microscopy presents the theory of image and contrast formation, and the analytical modes in transmission electron microscopy. The principles of particle and wave optics of electrons are described. Electron-specimen interactions are discussed for evaluating the theory of scattering and phase contrast. Also discussed are the kinematical and dynamical theories of electron diffraction and their applications for crystal-structure analysis and imaging of lattices and their defects. X-ray micronanalysis and electron energy-loss spectroscopy are treated as analytical methods. Specimen damage and contamination by electron irradiation limits the resolution for biological and some inorganic specimens. This fourth edition includes discussion of recent progress, especially in the area of Schottky emission guns, convergent-beam electron diffraction, electron tomography, holography and the high resolution of crystal lattices.

  7. Complex band structure and electronic transmission eigenchannels

    DEFF Research Database (Denmark)

    Jensen, Anders; Strange, Mikkel; Smidstrup, Soren

    2017-01-01

    and complex band structure, in this case individual eigenchannel transmissions and different complex bands. We present calculations of decay constants for the two most conductive states as determined by complex band structure and standard DFT Landauer transport calculations for one semi-conductor and two...

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2018-04-20

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

  9. Solid-state nanopores of controlled geometry fabricated in a transmission electron microscope

    Science.gov (United States)

    Qian, Hui; Egerton, Ray F.

    2017-11-01

    Energy-filtered transmission electron microscopy and electron tomography were applied to in situ studies of the formation, shape, and diameter of nanopores formed in a silicon nitride membrane in a transmission electron microscope. The nanopore geometry was observed in three dimensions by electron tomography. Drilling conditions, such as probe current, beam convergence angle, and probe position, affect the formation rate and the geometry of the pores. With a beam convergence semi-angle of α = 22 mrad, a conical shaped nanopore is formed but at α = 45 mrad, double-cone (hourglass-shaped) nanopores were produced. Nanopores with an effective diameter between 10 nm and 1.8 nm were fabricated by controlling the drilling time.

  10. Three-Dimensional scanning transmission electron microscopy of biological specimens

    KAUST Repository

    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

  11. Low-energy electron transmission and secondary-electron emission experiments on crystalline and molten long-chain alkanes

    International Nuclear Information System (INIS)

    Ueno, N.; Sugita, K.; Seki, K.; Inokuchi, H.

    1986-01-01

    This paper describes the results of low-energy electron transmission and secondary-electron emission experiments on thin films of long-chain alkanes deposited on metal substrates. The spectral changes due to crystal-melt phase transition were measured in situ in both experiments. The ground-state energy V 0 of the quasifree electron in crystalline state was determined to be 0.5 +- 0.1 eV. The value of V 0 for the molten state was found to be negative. Further, in the crystalline state evidence is found for a direct correspondence between the transmission maxima and the high value of the density of states in the conduction bands

  12. Calculation of electron transmission through aluminium foil

    International Nuclear Information System (INIS)

    Abroyan, M.A.; Mel'ker, A.I.; Mikhajlin, A.I.; Sirotinkin, V.V.; Tokmakov, I.L.

    1987-01-01

    Calculated by Monte Carlo method energy and angular distributions of electrons transmitted through aluminium foil with 50 μm thickness are presented. 200-500 electron energy ranges and angles of electron incidence on foil from 0 to 40 deg C are considered. That allows to use results for more universal accelerator group, for example, for accelerators with scanning beam used in industry. The received values of angular and energy characteristics allow to increase essentially estimation accuracy of accelerator extraction devices and dose distribution on irradiating item

  13. Bio-camouflage of anatase nanoparticles explored by in situ high-resolution electron microscopy.

    Science.gov (United States)

    Ribeiro, Ana R; Mukherjee, Arijita; Hu, Xuan; Shafien, Shayan; Ghodsi, Reza; He, Kun; Gemini-Piperni, Sara; Wang, Canhui; Klie, Robert F; Shokuhfar, Tolou; Shahbazian-Yassar, Reza; Borojevic, Radovan; Rocha, Luis A; Granjeiro, José M

    2017-08-03

    While titanium is the metal of choice for most prosthetics and inner body devices due to its superior biocompatibility, the discovery of Ti-containing species in the adjacent tissue as a result of wear and corrosion has been associated with autoimmune diseases and premature implant failures. Here, we utilize the in situ liquid cell transmission electron microscopy (TEM) in a liquid flow holder and graphene liquid cells (GLCs) to investigate, for the first time, the in situ nano-bio interactions between titanium dioxide nanoparticles and biological medium. This imaging and spectroscopy methodology showed the process of formation of an ionic and proteic bio-camouflage surrounding Ti dioxide (anatase) nanoparticles that facilitates their internalization by bone cells. The in situ understanding of the mechanisms of the formation of the bio-camouflage of anatase nanoparticles may contribute to the definition of strategies aimed at the manipulation of these NPs for bone regenerative purposes.

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

    Science.gov (United States)

    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. Published by Elsevier B.V.

  15. A single well pumping and recovery test to measure in situ acrotelm transmissivity in raised bogs

    NARCIS (Netherlands)

    Schaaf, van der S.

    2004-01-01

    A quasi-steady-state single pit pumping and recovery test to measure in situ the transmissivity of the highly permeable upper layer of raised bogs, the acrotelm, is described and discussed. The basic concept is the expanding depression cone during both pumping and recovery. It is shown that applying

  16. In situ Measurements of Phytoplankton Fluorescence Using Low Cost Electronics

    Directory of Open Access Journals (Sweden)

    Dana L. Wright

    2013-06-01

    Full Text Available Chlorophyll a fluorometry has long been used as a method to study phytoplankton in the ocean. In situ fluorometry is used frequently in oceanography to provide depth-resolved estimates of phytoplankton biomass. However, the high price of commercially manufactured in situ fluorometers has made them unavailable to some individuals and institutions. Presented here is an investigation into building an in situ fluorometer using low cost electronics. The goal was to construct an easily reproducible in situ fluorometer from simple and widely available electronic components. The simplicity and modest cost of the sensor makes it valuable to students and professionals alike. Open source sharing of architecture and software will allow students to reconstruct and customize the sensor on a small budget. Research applications that require numerous in situ fluorometers or expendable fluorometers can also benefit from this study. The sensor costs US$150.00 and can be constructed with little to no previous experience. The sensor uses a blue LED to excite chlorophyll a and measures fluorescence using a silicon photodiode. The sensor is controlled by an Arduino microcontroller that also serves as a data logger.

  17. The Titan Environmental Transmission Electron Microscope

    DEFF Research Database (Denmark)

    Hansen, Thomas Willum; Wagner, Jakob Birkedal; Jinschek, Jörg R.

    2009-01-01

    University of Denmark (DTU) provides a unique combination of techniques for studying materials of interest to the catalytic as well as the electronics and other communities [5]. DTU’s ETEM is based on the FEI Titan platform providing ultrahigh microscope stability pushing the imaging resolution into the sub...

  18. Scanning transmission low-energy electron microscopy

    Czech Academy of Sciences Publication Activity Database

    Müllerová, Ilona; Hovorka, Miloš; Konvalina, Ivo; Unčovský, M.; Frank, Luděk

    2011-01-01

    Roč. 55, č. 4 (2011), 2:1-6 ISSN 0018-8646 R&D Projects: GA AV ČR IAA100650902; GA MŠk ED0017/01/01 Institutional research plan: CEZ:AV0Z20650511 Keywords : TEM * STEM * SEM Subject RIV: JA - Electronics ; Optoelectronics, Electrical Engineering Impact factor: 0.723, year: 2011

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-01-14

    In this paper we present in situ transmission electron microscopy (TEM) of soft, synthetic nanoparticles with a comparative analysis using conventional TEM methods. This comparison is made with the simple aim of describing what is an unprecedented example of in situ imaging by TEM. However, we contend the technique will quickly become essential in the characterization of analogous systems, especially where dynamics are of interest in the solvated state. In this case, particles were studied which were obtained from the direct polymerization of an oxaliplatin analog, designed for an ongoing program in novel chemotherapeutic delivery systems. The resulting nanoparticles provided sufficient contrast for facile imaging in situ, and point toward key design parameters that enable this new characterization approach for organic nanomaterials. We describe the preparation of the synthetic micellar nanoparticles to- gether with their characterization in liquid water.

  20. Long distance electron transmission in marine sediment

    DEFF Research Database (Denmark)

    Risgaard-Petersen, Nils; Nielsen, Lars Peter

    processes leads to formation of electrical fields, which modifies ion transport. The local proton producing and proton consuming half reactions induces pH extremes that accelerate dissolution of iron sul-phides and calcium carbonates in anoxic layers and promotes the formation of Mg-calcite and iron oxides......Geochemical observations in marine sediment have recently shown that electric currents may intimately couple spatially separated biogeochemical processes like oxygen reduction at the sediment surface and hydrogen sul-phide oxidation in anoxic layers centimeters below 1. Further experimental studies...... suggest that the electron conductance is mediated by microorgan-isms. The spatial separation of electron and proton donors and acceptors has major impacts on element cycling by redox processes, pH balances, mineral dissolution/precipitations, and electromigration of ions. The sepa-ration of redox...

  1. Transmission electron microscopy and diffractometry of materials

    CERN Document Server

    Fultz, Brent

    2001-01-01

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

  2. Transmission environmental scanning electron microscope with scintillation gaseous detection device

    International Nuclear Information System (INIS)

    Danilatos, Gerasimos; Kollia, Mary; Dracopoulos, Vassileios

    2015-01-01

    A transmission environmental scanning electron microscope with use of a scintillation gaseous detection device has been implemented. This corresponds to a transmission scanning electron microscope but with addition of a gaseous environment acting both as environmental and detection medium. A commercial type of low vacuum machine has been employed together with appropriate modifications to the detection configuration. This involves controlled screening of various emitted signals in conjunction with a scintillation gaseous detection device already provided with the machine for regular surface imaging. Dark field and bright field imaging has been obtained along with other detection conditions. With a progressive series of modifications and tests, the theory and practice of a novel type of microscopy is briefly shown now ushering further significant improvements and developments in electron microscopy as a whole. - Highlights: • Novel scanning transmission electron microscopy (STEM) with an environmental scanning electron microscope (ESEM) called TESEM. • Use of the gaseous detection device (GDD) in scintillation mode that allows high resolution bright and dark field imaging in the TESEM. • Novel approach towards a unification of both vacuum and environmental conditions in both bulk/surface and transmission mode of electron microscopy

  3. Simulation of loss electron in vacuum magnetically insulated transmission lines

    International Nuclear Information System (INIS)

    Zhang Pengfei; Li Yongdong; Liu Chunliang; Wang Hongguang; Guo Fan; Yang Hailiang; Qiu Aici; Su Zhaofeng; Sun Jianfeng; Sun Jiang; Gao Yi

    2011-01-01

    In the beginning of magnetic insulated period, loss electron in coaxial vacuum magnetically insulated transmission line (MITL) strikes anode and the bremsstrahlung photons are generated in the mean time. Based on the self-limited flow model, velocity in direction of energy transport, energy spectrum and angular distribution of loss electron are simulated by PIC code, energy spectrum of bremsstrahlung photons as well calculated though Monte Carlo method. Computational results show that the velocity of loss electron is less than 2.998 x 108 m/s, the angular excursion of electron is not much in a board extent of energy spectrum. These results show an indirect diagnosis of vacuum insulted transmission line working status based on loss electron bremsstrahlung. (authors)

  4. Analysis on electronic control unit of continuously variable transmission

    Science.gov (United States)

    Cao, Shuanggui

    Continuously variable transmission system can ensure that the engine work along the line of best fuel economy, improve fuel economy, save fuel and reduce harmful gas emissions. At the same time, continuously variable transmission allows the vehicle speed is more smooth and improves the ride comfort. Although the CVT technology has made great development, but there are many shortcomings in the CVT. The CVT system of ordinary vehicles now is still low efficiency, poor starting performance, low transmission power, and is not ideal controlling, high cost and other issues. Therefore, many scholars began to study some new type of continuously variable transmission. The transmission system with electronic systems control can achieve automatic control of power transmission, give full play to the characteristics of the engine to achieve optimal control of powertrain, so the vehicle is always traveling around the best condition. Electronic control unit is composed of the core processor, input and output circuit module and other auxiliary circuit module. Input module collects and process many signals sent by sensor and , such as throttle angle, brake signals, engine speed signal, speed signal of input and output shaft of transmission, manual shift signals, mode selection signals, gear position signal and the speed ratio signal, so as to provide its corresponding processing for the controller core.

  5. Experimental procedures to mitigate electron beam induced artifacts during in situ fluid imaging of nanomaterials

    International Nuclear Information System (INIS)

    Woehl, Taylor J.; Jungjohann, Katherine L.; Evans, James E.; Arslan, Ilke; Ristenpart, William D.; Browning, Nigel D.

    2013-01-01

    Scanning transmission electron microscopy of various fluid and hydrated nanomaterial samples has revealed multiple imaging artifacts and electron beam–fluid interactions. These phenomena include growth of crystals on the fluid stage windows, repulsion of particles from the irradiated area, bubble formation, and the loss of atomic information during prolonged imaging of individual nanoparticles. Here we provide a comprehensive review of these fluid stage artifacts, and we present new experimental evidence that sheds light on their origins in terms of experimental apparatus issues and indirect electron beam sample interactions with the fluid layer. A key finding is that many artifacts are a result of indirect electron beam interactions, such as production of reactive radicals in the water by radiolysis, and the associated crystal growth. The results presented here will provide a methodology for minimizing fluid stage imaging artifacts and acquiring quantitative in situ observations of nanomaterial behavior in a liquid environment

  6. Experimental procedures to mitigate electron beam induced artifacts during in situ fluid imaging of nanomaterials

    Energy Technology Data Exchange (ETDEWEB)

    Woehl, Taylor J., E-mail: tjwoehl@ucdavis.edu [Department of Chemical Engineering and Materials Science, University of California, Davis, Davis, CA 95616 (United States); Jungjohann, Katherine L. [Department of Chemical Engineering and Materials Science, University of California, Davis, Davis, CA 95616 (United States); Evans, James E. [Department of Molecular and Cellular Biology, University of California, Davis, Davis, CA 95616 (United States); Pacific Northwest National Laboratory, Richland, WA 99352 (United States); Arslan, Ilke [Department of Chemical Engineering and Materials Science, University of California, Davis, Davis, CA 95616 (United States); Pacific Northwest National Laboratory, Richland, WA 99352 (United States); Ristenpart, William D. [Department of Chemical Engineering and Materials Science, University of California, Davis, Davis, CA 95616 (United States); Department of Food Science and Technology, University of California, Davis, Davis, CA 95616 (United States); Browning, Nigel D. [Department of Chemical Engineering and Materials Science, University of California, Davis, Davis, CA 95616 (United States); Department of Molecular and Cellular Biology, University of California, Davis, Davis, CA 95616 (United States); Pacific Northwest National Laboratory, Richland, WA 99352 (United States)

    2013-04-15

    Scanning transmission electron microscopy of various fluid and hydrated nanomaterial samples has revealed multiple imaging artifacts and electron beam–fluid interactions. These phenomena include growth of crystals on the fluid stage windows, repulsion of particles from the irradiated area, bubble formation, and the loss of atomic information during prolonged imaging of individual nanoparticles. Here we provide a comprehensive review of these fluid stage artifacts, and we present new experimental evidence that sheds light on their origins in terms of experimental apparatus issues and indirect electron beam sample interactions with the fluid layer. A key finding is that many artifacts are a result of indirect electron beam interactions, such as production of reactive radicals in the water by radiolysis, and the associated crystal growth. The results presented here will provide a methodology for minimizing fluid stage imaging artifacts and acquiring quantitative in situ observations of nanomaterial behavior in a liquid environment.

  7. Review of possible correlations between in situ stress and PFL fracture transmissivity data at Forsmark

    Energy Technology Data Exchange (ETDEWEB)

    Martin, Derek (University of Alberta (United States)); Follin, Sven (SF GeoLogic AB (Sweden))

    2011-11-15

    In laboratory samples, the fracture transmissivity decreases significantly as the confining stress increases. While these experimental relationships are widely accepted and validated on laboratory samples, it is unknown if such relationships exist in situ or if these relationships can be scaled from the centimetre-scale laboratory tests to the metre-scale of in situ fractures. The purpose of this work is to assess the relationship between the structural-hydraulic data gathered in deep, cored boreholes at Forsmark and the in situ stress state acting on the these fractures. In conclusion, there does not appear to be sufficient evidence from these analyses to support the notion that the magnitude of the flow along the fractures at Forsmark is solely controlled by the in situ stress acting on the fracture. This should not be surprising because the majority of the fractures formed more than 1 billion years ago and the current in situ stress state has only been active for the past 12 million years. It is more likely that the transmissivity values are controlled by fracture roughness, open channels within the fracture, fracture stiffness and fracture infilling material

  8. Processing scarce biological samples for light and transmission electron microscopy

    Directory of Open Access Journals (Sweden)

    P Taupin

    2008-06-01

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

  9. Catalysts under Controlled Atmospheres in the Transmission Electron Microscope

    DEFF Research Database (Denmark)

    Hansen, Thomas Willum; Wagner, Jakob Birkedal

    2014-01-01

    of resolution. Using suitably clean gases, modified pumping schemes, and short pathways through dense gas regions, these issues are now circumvented. Here we provide an account of best practice using environmental transmission electron microscopy on catalytic systems illustrated using select examples from......Over time, there has been an increasing interest in observing catalysts in their operating environment at high spatial resolution and ultimately to determine the structure of a catalytically active surface. One tool with the potential to do exactly this in direct space is the transmission electron...

  10. Selection of electron acceptors and strategies for in situ bioremediation

    International Nuclear Information System (INIS)

    Norris, R.D.

    1995-01-01

    The most critical aspect of designing in situ bioremediation systems is, typically, the selection and method of delivery of the electron acceptor. Nitrate, sulfate, and several forms of oxygen can be introduced, depending on the contaminants and the site conditions. Oxygen can be added as air, pure oxygen, hydrogen peroxide, or an oxygen release compound. Simplistic cost calculations can illustrate the advantages of some methods over others, providing technical requirements can be met

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

    International Nuclear Information System (INIS)

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

    1983-01-01

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

  12. Structure Identification in High-Resolution Transmission Electron Microscopic Images

    DEFF Research Database (Denmark)

    Vestergaard, Jacob Schack; Kling, Jens; Dahl, Anders Bjorholm

    2014-01-01

    A connection between microscopic structure and macroscopic properties is expected for almost all material systems. High-resolution transmission electron microscopy is a technique offering insight into the atomic structure, but the analysis of large image series can be time consuming. The present ...

  13. Three-Dimensional Orientation Mapping in the Transmission Electron Microscope

    DEFF Research Database (Denmark)

    Liu, Haihua; Schmidt, Søren; Poulsen, Henning Friis

    2011-01-01

    resolution of 200 nanometers (nm). We describe here a nondestructive technique that enables 3D orientation mapping in the transmission electron microscope of mono- and multiphase nanocrystalline materials with a spatial resolution reaching 1 nm. We demonstrate the technique by an experimental study...

  14. Ion source for thinning of specimen in transmission electron microscopy

    International Nuclear Information System (INIS)

    Hammer, K.; Rothe, R.

    1983-01-01

    Thinning of specimen for transmission electron microscopy is carried out by means of sputtering. Construction, design, and operation parameters of an ion source are presented. Because the plasma is produced by means of hollow cathode glow discharges, no special focusing system is used

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

    Science.gov (United States)

    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. Copyright © 2016 Elsevier B.V. All rights reserved.

  16. Transmission electron microscopy study of dislocation motion in icosahedral Al-Pd-Mn

    International Nuclear Information System (INIS)

    Mompiou, F.; Caillard, D.

    2005-01-01

    Perfect and imperfect dislocations trailing phason faults in quasi-crystals are introduced using a simplified two-dimensional aperiodic structure. Then, on the basis of observations of deformed specimens as well as in situ experiments in a transmission electron microscope, the motion of dislocations in icosahedral Al-Pd-Mn is shown to take place exclusively by climb. Under such conditions, the very high brittleness of Al-Pd-Mn at low and medium temperatures is proposed to be a consequence of the difficulty of glide, which itself appears to be an intrinsic property of the quasi-crystalline structure

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

    International Nuclear Information System (INIS)

    Taniguchi, Yoshifumi; Matsumoto, Hiroaki; Harada, Ken

    2012-01-01

    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. Foucault imaging by using non-dedicated transmission electron microscope

    Science.gov (United States)

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Taniguchi, Yoshifumi [Science and Medical Systems Business Group, Hitachi High-Technologies Corp., Ichige, Hitachinaka, Ibaraki 312-8504 (Japan); Matsumoto, Hiroaki [Corporate Manufacturing Strategy Group, Hitachi High-Technologies Corp., Ishikawa-cho, Hitachinaka, Ibaraki 312-1991 (Japan); Harada, Ken [Central Research Laboratory, Hitachi Ltd., Hatoyama, Saitama 350-0395 (Japan)

    2012-08-27

    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.

  20. Measurement of suprathermal electron confinement by cyclotron transmission

    International Nuclear Information System (INIS)

    Kirkwood, R.; Hutchinson, I.H.; Luckhardt, S.C.; Porkolab, M.; Squire, J.P.

    1990-01-01

    The confinement time of suprathermal electrons is determined experimentally from the distribution function determined via wave transmission measurements. Measurements of the lowest moment of the distribution perpendicular to the B field as a function of the parallel electron momentum as well as the global input power allow the suprathermal electron confinement time (τ se ) to be calculated during lower-hybrid and inductive current drive. Finite particle confinement is found to be the dominant energy loss term for the suprathermals and improves with plasma current and density

  1. Transmission environmental scanning electron microscope with scintillation gaseous detection device.

    Science.gov (United States)

    Danilatos, Gerasimos; Kollia, Mary; Dracopoulos, Vassileios

    2015-03-01

    A transmission environmental scanning electron microscope with use of a scintillation gaseous detection device has been implemented. This corresponds to a transmission scanning electron microscope but with addition of a gaseous environment acting both as environmental and detection medium. A commercial type of low vacuum machine has been employed together with appropriate modifications to the detection configuration. This involves controlled screening of various emitted signals in conjunction with a scintillation gaseous detection device already provided with the machine for regular surface imaging. Dark field and bright field imaging has been obtained along with other detection conditions. With a progressive series of modifications and tests, the theory and practice of a novel type of microscopy is briefly shown now ushering further significant improvements and developments in electron microscopy as a whole. Copyright © 2014 Elsevier B.V. All rights reserved.

  2. In situ laser processing in a scanning electron microscope

    Energy Technology Data Exchange (ETDEWEB)

    Roberts, Nicholas A.; Magel, Gregory A.; Hartfield, Cheryl D.; Moore, Thomas M.; Fowlkes, Jason D.; Rack, Philip D. [Department of Materials Science and Engineering, University of Tennessee, Knoxville, Tennessee 37996 (United States) and Omniprobe, Inc., an Oxford Instruments Company, 10410 Miller Rd., Dallas, Texas 75238 (United States); Omniprobe, Inc., an Oxford Instruments Company, 10410 Miller Rd., Dallas, Texas 75238 (United States); Center for Nanophase Materials Sciences, Oak Ridge National Laboratory, Oak Ridge, Tennessee 37831 (United States); Department of Materials Science and Engineering, University of Tennessee, Knoxville, Tennessee 37996 (United States) and Center for Nanophase Materials Sciences, Oak Ridge National Laboratory, Oak Ridge, Tennessee 37831 (United States)

    2012-07-15

    Laser delivery probes using multimode fiber optic delivery and bulk focusing optics have been constructed and used for performing materials processing experiments within scanning electron microscope/focused ion beam instruments. Controlling the current driving a 915-nm semiconductor diode laser module enables continuous or pulsed operation down to sub-microsecond durations, and with spot sizes on the order of 50 {mu}m diameter, achieving irradiances at a sample surface exceeding 1 MW/cm{sup 2}. Localized laser heating has been used to demonstrate laser chemical vapor deposition of Pt, surface melting of silicon, enhanced purity, and resistivity via laser annealing of Au deposits formed by electron beam induced deposition, and in situ secondary electron imaging of laser induced dewetting of Au metal films on SiO{sub x}.

  3. In situ TEM/SEM electronic/mechanical characterization of nano material with MEMS chip

    International Nuclear Information System (INIS)

    Wang Yuelin; Li Tie; Zhang Xiao; Zeng Hongjiang; Jin Qinhua

    2014-01-01

    Our investigation of in situ observations on electronic and mechanical properties of nano materials using a scanning electron microscope (SEM) and a transmission electron microscope (TEM) with the help of traditional micro-electro-mechanical system (MEMS) technology has been reviewed. Thanks to the stability, continuity and controllability of the loading force from the electrostatic actuator and the sensitivity of the sensor beam, a MEMS tensile testing chip for accurate tensile testing in the nano scale is obtained. Based on the MEMS chips, the scale effect of Young's modulus in silicon has been studied and confirmed directly in a tensile experiment using a transmission electron microscope. Employing the nanomanipulation technology and FIB technology, Cu and SiC nanowires have been integrated into the tensile testing device and their mechanical, electronic properties under different stress have been achieved, simultaneously. All these will aid in better understanding the nano effects and contribute to the designation and application in nano devices. (invited papers)

  4. Electronic Biometric Transmission Specification. Version 1.2

    Science.gov (United States)

    2006-11-08

    Prescribed by ANSI Std Z39-18 Electronic Biometric Transmission Specification DIN: DOD_BTF_TS_EBTS_ Nov06_01.02.00 i Revision History Revision...contains: • the ORI • a Greenwich Mean (a.k.a. Zulu or UTC) date/time stamp • a code for the software used at the point of collection/transmission...long names and would generally include the tribe name. Subfield 1 Item 1 Character Type AS Characters 1 to 50 Special Characters: Any 7-bit non

  5. Atomistic observations and analyses of lattice defects in transmission electron microscopes

    CERN Document Server

    Abe, H

    2003-01-01

    The transmission electron microscope (TEM) -accelerators was developed. TEM-Accelerator made possible to observe in situ experiments of ion irradiation and implantation. The main results are the experimental proof of new lattice defects by irradiation, the formation process and synthesized conditions of carbon onion by ion implantation, the microstructure and phase transformation conditions of graphite by ion irradiated phase transformation, the irradiation damage formation process by simultaneous irradiation of electron and ion and behavior of fullerene whisker under irradiation. The microstructural evolution of defect clusters in copper irradiated with 240-keV Cu sup + ions and a high resolution electron micrograph of carbon onions synthesized by ion implantation are explained as the examples of recent researches. (S.Y.)

  6. ''In situ'' electronic testing method of a neutron detector performance

    International Nuclear Information System (INIS)

    Gonzalez, J.M.; Levai, F.

    1987-01-01

    The method allows detection of any important change in the electrical characteristics of a neutron sensor channel. It checks the response signal produced by an electronic detector circuit when a pulse generator is connected as input signal in the high voltage supply. The electronic circuit compares the detector capacitance value, previously measured, against a reference value, which is adjusted in a window type comparator electronic circuit to detect any important degrading condition of the capacitance value in a detector-cable system. The ''in-situ'' electronic testing method of neutron detector performance has been verified in a laboratory atmosphere to be a potential method to detect any significant change in the capacitance value of a nuclear sensor and its connecting cable, also checking: detector disconnections, cable disconnections, length changes of the connecting cable, electric short-opened circuits in the sensor channel, and any electrical trouble in the detector-connector-cable system. The experimental practices were carried out by simulation of several electric changes in a nuclear sensor-cable system from a linear D.C. channel which measures reactor power during nuclear reactor operation. It was made at the Training Reactor Electronic Laboratory. The results and conclusions obtained at the Laboratory were proved, satisfactorily, in the Electronic Instrumentation of Budapest Technical University Training Reactor, Hungary

  7. In situ and ex situ electron microscopy and X-ray diffraction characterization of the evolution of a catalytic system - from synthesis to deactivation

    DEFF Research Database (Denmark)

    Gardini, Diego

    Heterogeneous catalysis represents a research field of undeniable importance for a multitude of technological and industrial processes. Supported catalysts are nowadays at the base of the large-scale production of most chemicals and are used for the removal of air pollutants from automotive engines...... the understanding of the structural properties and mechanisms at the origin of catalytic activity. This thesis presents the potential and uniqueness of ex situ and in situ transmission electron microscopy (TEM) and X-ray diffraction (XRD) techniques in the characterization of several supported material systems...... TEM (HRTEM) and electron energy loss spectroscopy (EELS) revealed the degradation of the supported carbide particles probably due to the formation of volatile molybdenum hydroxide species. The activity of silver nanoparticles as catalyst for soot oxidation was studied in operative conditions...

  8. Electron transmission through a periodically driven graphene magnetic barrier

    Energy Technology Data Exchange (ETDEWEB)

    Biswas, R., E-mail: rbiswas.pkc@gmail.com [Department of Physics, P. K. College, Contai, Purba Medinipur, West Bengal – 721401 (India); Maiti, S. [Ajodhya Hills G.S.A.T High School, Ajodhya, Purulia, West Bengal – 723152 (India); Mukhopadhyay, S. [Purulia Zilla School, Dulmi Nadiha, Purulia, West Bengal – 723102 (India); Sinha, C. [Department of Physics, P. K. College, Contai, Purba Medinipur, West Bengal – 721401 (India); Department of Theoretical Physics, Indian Association for the Cultivation of Science, Jadavpur – 700032 (India)

    2017-05-10

    Electronic transport through graphene magnetic barriers is studied theoretically in presence of an external time harmonic scalar potential in the framework of non-perturbative Landau–Floquet Formalism. The oscillating field mostly suppresses the transmission for rectangular magnetic barrier structure and exhibits the Fano resonance for multiphoton processes due to the presence of bound state inside the barrier. While, for a pair of delta function barriers of larger separation, the oscillating potential suppresses the usual Fabry–Perot oscillations in the transmission and a new type of asymmetric Fano resonance is noted for smaller separation, occurring due to extended states between the barriers. - Highlights: • Tunnelling of the Dirac Fermions through oscillating pure magnetic barriers is reported for the first time. • The high energy transmission through a graphene magnetic barrier is suppressed by the application of time periodic modulation. • Suppression of the Fabry Perot transmission is noted due to the application of an external time harmonic potential. • Two kinds of the Fano resonances are noted in transmission through a pair of modulated δ-function magnetic barriers.

  9. Transmission of high-power electron beams through small apertures

    International Nuclear Information System (INIS)

    Tschalär, C.; Alarcon, R.; Balascuta, S.; Benson, S.V.; Bertozzi, W.; Boyce, J.R.; Cowan, R.; Douglas, D.; Evtushenko, P.; Fisher, P.; Ihloff, E.; Kalantarians, N.; Kelleher, A.; Legg, R.; Milner, R.G.; Neil, G.R.; Ou, L.; Schmookler, B.; Tennant, C.; Williams, G.P.

    2013-01-01

    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 h continuous run

  10. Cross-sectional transmission electron microscopy of semiconductors

    International Nuclear Information System (INIS)

    Sadana, D.K.

    1982-10-01

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

  11. Reciprocity relations in transmission electron microscopy: A rigorous derivation.

    Science.gov (United States)

    Krause, Florian F; Rosenauer, Andreas

    2017-01-01

    A concise derivation of the principle of reciprocity applied to realistic transmission electron microscopy setups is presented making use of the multislice formalism. The equivalence of images acquired in conventional and scanning mode is thereby rigorously shown. The conditions for the applicability of the found reciprocity relations is discussed. Furthermore the positions of apertures in relation to the corresponding lenses are considered, a subject which scarcely has been addressed in previous publications. Copyright © 2016 Elsevier Ltd. All rights reserved.

  12. Multistage linear electron acceleration using pulsed transmission lines

    International Nuclear Information System (INIS)

    Miller, R.B.; Prestwich, K.R.; Poukey, J.W.; Epstein, B.G.; Freeman, J.R.; Sharpe, A.W.; Tucker, W.K.; Shope, S.L.

    1981-01-01

    A four-stage linear electron accelerator is described which uses pulsed radial transmission lines as the basic accelerating units. An annular electron beam produced by a foilless diode is guided through the accelerator by a strong axial magnetic field. Synchronous firing of the injector and the acccelerating modules is accomplished with self-breaking oil switches. The device has accelerated beam currents of 25 kA to kinetic energies of 9 MV, with 90% current transport efficiency. The average accelerating gradient is 3 MV/m

  13. Pulsed Power for a Dynamic Transmission Electron Microscope

    Energy Technology Data Exchange (ETDEWEB)

    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.

  14. Pulsed Power for a Dynamic Transmission Electron Microscope

    International Nuclear Information System (INIS)

    DeHope, W.J.; Browning, N.; Campbell, G.; Cook, E.; King, W.; Lagrange, T.; Reed, B.; Stuart, B.; Shuttlesworth, R.; Pyke, B.

    2009-01-01

    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

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

    Directory of Open Access Journals (Sweden)

    J. P. Martin

    2009-03-01

    Full Text Available 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≥2  MV.

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

    Energy Technology Data Exchange (ETDEWEB)

    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.

  17. Transmission electron microscopy physics of image formation and microanalysis

    CERN Document Server

    Reimer, Ludwig

    1984-01-01

    The aim of this book is to outline the physics of image formation, electron­ specimen interactions and image interpretation in transmission electron mic­ roscopy. The book evolved from lectures delivered at the University of Munster and is a revised version of the first part of my earlier book Elek­ tronenmikroskopische Untersuchungs- und Priiparationsmethoden, omitting the part which describes specimen-preparation methods. In the introductory chapter, the different types of electron microscope are compared, the various electron-specimen interactions and their applications are summarized and the most important aspects of high-resolution, analytical and high-voltage electron microscopy are discussed. The optics of electron lenses is discussed in Chapter 2 in order to bring out electron-lens properties that are important for an understanding of the function of an electron microscope. In Chapter 3, the wave optics of elec­ trons and the phase shifts by electrostatic and magnetic fields are introduced; Fresne...

  18. Development of a secondary electron energy analyzer for a transmission electron microscope.

    Science.gov (United States)

    Magara, Hideyuki; Tomita, Takeshi; Kondo, Yukihito; Sato, Takafumi; Akase, Zentaro; Shindo, Daisuke

    2018-04-01

    A secondary electron (SE) energy analyzer was developed for a transmission electron microscope. The analyzer comprises a microchannel plate (MCP) for detecting electrons, a coil for collecting SEs emitted from the specimen, a tube for reducing the number of backscattered electrons incident on the MCP, and a retarding mesh for selecting the energy of SEs incident on the MCP. The detection of the SEs associated with charging phenomena around a charged specimen was attempted by performing electron holography and SE spectroscopy using the energy analyzer. The results suggest that it is possible to obtain the energy spectra of SEs using the analyzer and the charging states of a specimen by electron holography simultaneously.

  19. Miniaturized Environmental Scanning Electron Microscope for In Situ Planetary Studies

    Science.gov (United States)

    Gaskin, Jessica; Abbott, Terry; Medley, Stephanie; Gregory, Don; Thaisen, Kevin; Taylor , Lawrence; Ramsey, Brian; Jerman, Gregory; Sampson, Allen; Harvey, Ralph

    2010-01-01

    The exploration of remote planetary surfaces calls for the advancement of low power, highly-miniaturized instrumentation. Instruments of this nature that are capable of multiple types of analyses will prove to be particularly useful as we prepare for human return to the moon, and as we continue to explore increasingly remote locations in our Solar System. To this end, our group has been developing a miniaturized Environmental-Scanning Electron Microscope (mESEM) capable of remote investigations of mineralogical samples through in-situ topographical and chemical analysis on a fine scale. The functioning of an SEM is well known: an electron beam is focused to nanometer-scale onto a given sample where resulting emissions such as backscattered and secondary electrons, X-rays, and visible light are registered. Raster scanning the primary electron beam across the sample then gives a fine-scale image of the surface topography (texture), crystalline structure and orientation, with accompanying elemental composition. The flexibility in the types of measurements the mESEM is capable of, makes it ideally suited for a variety of applications. The mESEM is appropriate for use on multiple planetary surfaces, and for a variety of mission goals (from science to non-destructive analysis to ISRU). We will identify potential applications and range of potential uses related to planetary exploration. Over the past few of years we have initiated fabrication and testing of a proof-of-concept assembly, consisting of a cold-field-emission electron gun and custom high-voltage power supply, electrostatic electron-beam focusing column, and scanning-imaging electronics plus backscatter detector. Current project status will be discussed. This effort is funded through the NASA Research Opportunities in Space and Earth Sciences - Planetary Instrument Definition and Development Program.

  20. Transmission Electron Microscopy Studies of Electron-Selective Titanium Oxide Contacts in Silicon Solar Cells

    KAUST Repository

    Ali, Haider; Yang, Xinbo; Weber, Klaus; Schoenfeld, Winston V.; Davis, Kristopher O.

    2017-01-01

    In this study, the cross-section of electron-selective titanium oxide (TiO2) contacts for n-type crystalline silicon solar cells were investigated by transmission electron microscopy. It was revealed that the excellent cell efficiency of 21

  1. Method for local temperature measurement in a nanoreactor for in situ high-resolution electron microscopy.

    Science.gov (United States)

    Vendelbo, S B; Kooyman, P J; Creemer, J F; Morana, B; Mele, L; Dona, P; Nelissen, B J; Helveg, S

    2013-10-01

    In situ high-resolution transmission electron microscopy (TEM) of solids under reactive gas conditions can be facilitated by microelectromechanical system devices called nanoreactors. These nanoreactors are windowed cells containing nanoliter volumes of gas at ambient pressures and elevated temperatures. However, due to the high spatial confinement of the reaction environment, traditional methods for measuring process parameters, such as the local temperature, are difficult to apply. To address this issue, we devise an electron energy loss spectroscopy (EELS) method that probes the local temperature of the reaction volume under inspection by the electron beam. The local gas density, as measured using quantitative EELS, is combined with the inherent relation between gas density and temperature, as described by the ideal gas law, to obtain the local temperature. Using this method we determined the temperature gradient in a nanoreactor in situ, while the average, global temperature was monitored by a traditional measurement of the electrical resistivity of the heater. The local gas temperatures had a maximum of 56 °C deviation from the global heater values under the applied conditions. The local temperatures, obtained with the proposed method, are in good agreement with predictions from an analytical model. Copyright © 2013 Elsevier B.V. All rights reserved.

  2. Sample Preparation and Imaging of Exosomes by Transmission Electron Microscopy.

    Science.gov (United States)

    Jung, Min Kyo; Mun, Ji Young

    2018-01-04

    Exosomes are nano-sized extracellular vesicles secreted by body fluids and are known to represent the characteristics of cells that secrete them. The contents and morphology of the secreted vesicles reflect cell behavior or physiological status, for example cell growth, migration, cleavage, and death. The exosomes' role may depend highly on size, and the size of exosomes varies from 30 to 300 nm. The most widely used method for exosome imaging is negative staining, while other results are based on Cryo-Transmission Electron Microscopy, Scanning Electron Microscopy, and Atomic Force Microscopy. The typical exosome's morphology assessed through negative staining is a cup-shape, but further details are not yet clear. An exosome well-characterized through structural study is necessary particular in medical and pharmaceutical fields. Therefore, function-dependent morphology should be verified by electron microscopy techniques such as labeling a specific protein in the detailed structure of exosome. To observe detailed structure, ultrathin sectioned images and negative stained images of exosomes were compared. In this protocol, we suggest transmission electron microscopy for the imaging of exosomes including negative staining, whole mount immuno-staining, block preparation, thin section, and immuno-gold labelling.

  3. Aberration-corrected scanning transmission electron microscopy of semiconductors

    International Nuclear Information System (INIS)

    Krivanek, O L; Dellby, N; Murfitt, M F

    2011-01-01

    The scanning transmission electron microscope (STEM) has been able to image individual heavy atoms in a light matrix for some time. It is now able to do much more: it can resolve individual atoms as light as boron in monolayer materials; image atomic columns as light as hydrogen, identify the chemical type of individual isolated atoms from the intensity of their annular dark field (ADF) image and by electron energy loss spectroscopy (EELS); and map elemental composition at atomic resolution by EELS and energy-dispersive X-ray spectroscopy (EDXS). It can even map electronic states, also by EELS, at atomic resolution. The instrumentation developments that have made this level of performance possible are reviewed, and examples of applications to semiconductors and oxides are shown.

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

    Science.gov (United States)

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

    2018-04-01

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

  5. Optimization of Beam Transmission of PAL-PNF Electron Linac

    Energy Technology Data Exchange (ETDEWEB)

    Shin, S. G.; Kim, S. K.; Kim, E. A. [Pohang University of Science and Technology, Pohang (Korea, Republic of)

    2012-05-15

    The PNF (Pohang Neutron Facility) electron Linac is providing converted neutrons and photons from electron beams to users for nuclear physics experiments and high energy gamma-ray exposures. This linac is capable of producing 100 MeV electron beams with a beam current of pulsed 100 mA. The pulse length is 2 {mu}s and the pulse repetition rate is typically 30 Hz. This linac consists of two SLAC-type S-band accelerating columns and the thermionic RF gun. They are powered by one klystron and the matching pulse modulator. The electron beams emitted from the RF gun are bunched as they pass through the alpha magnet and are injected into the accelerating column thereafter. In this paper, we discuss procedures and results of the beam transmission optimization with technical details of the accelerator system. We also briefly discuss the future upgrade plan to obtain short-pulse or electron beams for neutron TOF experiments by adopting a triode type thermionic DC electron gun

  6. Development of spin-polarized transmission electron microscope

    International Nuclear Information System (INIS)

    Kuwahara, M; Saitoh, K; Tanaka, N; Takeda, Y; Ujihara, T; Asano, H; Nakanishi, T

    2011-01-01

    In order to study spin related phenomena in nano-size materials, spin-polarized electron source (PES) has been employed for the incident beam in transmission electron microscope (TEM). The PES has been designed and constructed with optimizing for spin-polarized TEM. The illuminating system of TEM is also designed to focus the spin-polarized electron beam emitted from a semiconductor photocathode with a negative electron affinity (NEA) surface. The beam energy is set to below 40 keV which is lower energy type as a TEM, because the spin interaction with condensed matters is very small corresponding with a Coulomb interaction. The polarized electron gun has realized in an extra high vacuum (XHV) condition and high field gradient of 4 MV/m on a surface of photocathode. Furthermore, it demonstrated that 40-keV polarized electron beam was operated with a sub-milli second pulse mode by using the backside excitation type photocathode. This high performance PES will make it possible to observe dynamically a magnetic field images with high contrast and highspeed temporal imaging in TEM.

  7. Three-Dimensional scanning transmission electron microscopy of biological specimens

    KAUST Repository

    De Jonge, Niels

    2010-01-18

    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. © 2010 Microscopy Society of America.

  8. Structural Fingerprinting of Nanocrystals in the Transmission Electron Microscope

    Science.gov (United States)

    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

  9. Characterization of catalysts by scanning transmission electron microscopy

    International Nuclear Information System (INIS)

    Targos, W.M.; Bradley, S.A.

    1989-01-01

    The dedicated scanning transmission electron microscope (STEM) is an integral tool for characterizing catalysts because of its unique ability to image and analyze nanosized volumes. This information is valuable in optimizing catalyst formulations and determining causes for reduced catalyst performance. For many commercial catalysts direct correlations between structural features of metal crystallites and catalytic performance are not attainable. When these instances occur, determination of elemental distribution may be the only information available. In this paper the authors discuss some of the techniques employed and limitations associated with characterizing commercial catalysts

  10. Transmission electron microscopic study of reduced Ca2UO5

    International Nuclear Information System (INIS)

    Krasevec, V.; Prodan, A.; Holc, J.; Kolar, D.

    1983-01-01

    Structural changes of Ca 2 UO 5 during reduction in hydrogen were studied by transmission electron microscopy. It was shown that monoclinic Ca 2 UO 5 changes into triclinic Ca 4 U 2 O 9 . They are related, respectively, to the fluorite and the bixbyite (C-M 2 O 3 ) structures, so that the product is a superstructure of the latter. Reduction occurs along the (100)/sub t/ planes originating from the (006)/sub m/ planes of the parent structure by diminishing the coordination number of the Ca cation from 7 to 6. 5 figures

  11. Transmission electron microscopy investigation of Bi-2223/Ag tapes

    DEFF Research Database (Denmark)

    Andersen, L.G.; Bals, S.; Tendeloo, G. Van

    2001-01-01

    during the tape processing, (3) a study of the grain boundaries on an atomic scale, including intergrowth investigations. Tapes with different process parameters have been compared with respect to the microstructure. A fully processed tape has on the average 50% thicker Bi-2223 grains than a tape after......The microstructure of (Bi,Pb)(2)Sr2Ca2CuOx (Bi-2223) tapes has been investigated by means of transmission electron microscopy (TEM) and high-resolution TEM. The emphasis has been placed on: (1) an examination of the grain morphology and size, (2) grain and colony boundary angles, which are formed...

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

    International Nuclear Information System (INIS)

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

    2016-01-01

    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. - Highlights: • We propose a novel technique to image the structure of polycrystalline TEM-samples. • Correlation coefficients maps highlights the evolution of the diffracting signal. • 3D views of grain boundaries are provided for nano-particles or polycrystals.

  13. Correction of bubble size distributions from transmission electron microscopy observations

    International Nuclear Information System (INIS)

    Kirkegaard, P.; Eldrup, M.; Horsewell, A.; Skov Pedersen, J.

    1996-01-01

    Observations by transmission electron microscopy of a high density of gas bubbles in a metal matrix yield a distorted size distribution due to bubble overlap and bubble escape from the surface. A model is described that reconstructs 3-dimensional bubble size distributions from 2-dimensional projections on taking these effects into account. Mathematically, the reconstruction is an ill-posed inverse problem, which is solved by regularization technique. Extensive Monte Carlo simulations support the validity of our model. (au) 1 tab., 32 ills., 32 refs

  14. Determination of redox reaction rates and orders by in situ liquid cell electron microscopy of Pd and Au solution growth.

    Science.gov (United States)

    Sutter, Eli A; Sutter, Peter W

    2014-12-03

    In-situ liquid cell transmission and scanning transmission electron microscopy (TEM/STEM) experiments are important, as they provide direct insight into processes in liquids, such as solution growth of nanoparticles, among others. In liquid cell TEM/STEM redox reaction experiments, the hydrated electrons e(-)aq created by the electron beam are responsible for the reduction of metal-ion complexes. Here we investigate the rate equation of redox reactions involving reduction by e(-)aq generated by the electron beam during in situ liquid TEM/STEM. Specifically we consider the growth of Pd on Au seeds in aqueous solutions containing Pd-chloro complexes. From the quantification of the rate of Pd deposition at different electron beam currents and as a function of distance from a stationary, nanometer-sized exciting beam, we determine that the reaction is first order with respect to the concentration of hydrated electrons, [e(-)aq]. By comparing Pd- and Au-deposition, we further demonstrate that measurements of the local deposition rate on nanoparticles in the solution via real-time imaging can be used to measure not only [e(-)aq] but also the rate of reduction of a metal-ion complex to zerovalent metal atoms in solution.

  15. Optical and Optoelectronic Property Analysis of Nanomaterials inside Transmission Electron Microscope.

    Science.gov (United States)

    Fernando, Joseph F S; Zhang, Chao; Firestein, Konstantin L; Golberg, Dmitri

    2017-12-01

    In situ transmission electron microscopy (TEM) allows one to investigate nanostructures at high spatial resolution in response to external stimuli, such as heat, electrical current, mechanical force and light. This review exclusively focuses on the optical, optoelectronic and photocatalytic studies inside TEM. With the development of TEMs and specialized TEM holders that include in situ illumination and light collection optics, it is possible to perform optical spectroscopies and diverse optoelectronic experiments inside TEM with simultaneous high resolution imaging of nanostructures. Optical TEM holders combining the capability of a scanning tunneling microscopy probe have enabled nanomaterial bending/stretching and electrical measurements in tandem with illumination. Hence, deep insights into the optoelectronic property versus true structure and its dynamics could be established at the nanometer-range precision thus evaluating the suitability of a nanostructure for advanced light driven technologies. This report highlights systems for in situ illumination of TEM samples and recent research work based on the relevant methods, including nanomaterial cathodoluminescence, photoluminescence, photocatalysis, photodeposition, photoconductivity and piezophototronics. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Imaging and Quantification of Extracellular Vesicles by Transmission Electron Microscopy.

    Science.gov (United States)

    Linares, Romain; Tan, Sisareuth; Gounou, Céline; Brisson, Alain R

    2017-01-01

    Extracellular vesicles (EVs) are cell-derived vesicles that are present in blood and other body fluids. EVs raise major interest for their diverse physiopathological roles and their potential biomedical applications. However, the characterization and quantification of EVs constitute major challenges, mainly due to their small size and the lack of methods adapted for their study. Electron microscopy has made significant contributions to the EV field since their initial discovery. Here, we describe the use of two transmission electron microscopy (TEM) techniques for imaging and quantifying EVs. Cryo-TEM combined with receptor-specific gold labeling is applied to reveal the morphology, size, and phenotype of EVs, while their enumeration is achieved after high-speed sedimentation on EM grids.

  17. Advances in imaging and electron physics the scanning transmission electron microscope

    CERN Document Server

    Hawkes, Peter W

    2009-01-01

    Advances in Imaging and Electron Physics merges two long-running serials--Advances in Electronics and Electron Physics and Advances in Optical and Electron Microscopy. This series features extended articles on the physics of electron devices (especially semiconductor devices), particle optics at high and low energies, microlithography, image science and digital image processing, electromagnetic wave propagation, electron microscopy, and the computing methods used in all these domains.  This particular volume presents several timely articles on the scanning transmission electron microscope. Updated with contributions from leading international scholars and industry experts Discusses hot topic areas and presents current and future research trends Provides an invaluable reference and guide for physicists, engineers and mathematicians.

  18. Reconstruction and visualization of nanoparticle composites by transmission electron tomography

    Energy Technology Data Exchange (ETDEWEB)

    Wang, X.Y. [National Institute for Nanotechnology, 11421 Saskatchewan Drive, Edmonton, Canada T6H 2M9 (Canada); Department of Physics, University of Alberta, Edmonton, Canada T6G 2G7 (Canada); Lockwood, R. [National Institute for Nanotechnology, 11421 Saskatchewan Drive, Edmonton, Canada T6H 2M9 (Canada); Malac, M., E-mail: marek.malac@nrc-cnrc.gc.ca [National Institute for Nanotechnology, 11421 Saskatchewan Drive, Edmonton, Canada T6H 2M9 (Canada); Department of Physics, University of Alberta, Edmonton, Canada T6G 2G7 (Canada); Furukawa, H. [SYSTEM IN FRONTIER INC., 2-8-3, Shinsuzuharu bldg. 4F, Akebono-cho, Tachikawa-shi, Tokyo 190-0012 (Japan); Li, P.; Meldrum, A. [National Institute for Nanotechnology, 11421 Saskatchewan Drive, Edmonton, Canada T6H 2M9 (Canada)

    2012-02-15

    This paper examines the limits of transmission electron tomography reconstruction methods for a nanocomposite object composed of many closely packed nanoparticles. Two commonly used reconstruction methods in TEM tomography were examined and compared, and the sources of various artefacts were explored. Common visualization methods were investigated, and the resulting 'interpretation artefacts' ( i.e., deviations from 'actual' particle sizes and shapes arising from the visualization) were determined. Setting a known or estimated nanoparticle volume fraction as a criterion for thresholding does not in fact give a good visualization. Unexpected effects associated with common built-in image filtering methods were also found. Ultimately, this work set out to establish the common problems and pitfalls associated with electron beam tomographic reconstruction and visualization of samples consisting of closely spaced nanoparticles. -- Highlights: Black-Right-Pointing-Pointer Electron tomography limits were explored by both experiment and simulation. Black-Right-Pointing-Pointer Reliable quantitative volumetry using electron tomography is not presently feasible. Black-Right-Pointing-Pointer Volume rendering appears to be better choice for visualization of composite samples.

  19. Characterization of strained semiconductor structures using transmission electron microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Oezdoel, Vasfi Burak

    2011-08-15

    Today's state-of-the-art semiconductor electronic devices utilize the charge transport within very small volumes of the active device regions. The structural, chemical and optical material properties in these small dimensions can critically affect the performance of these devices. The present thesis is focused on the nanometer scale characterization of the strain state in semiconductor structures using transmission electron microscopy (TEM). Although high-resolution TEM has shown to provide the required accuracy at the nanometer scale, optimization of imaging conditions is necessary for accurate strain measurements. An alternative HRTEM method based on strain mapping on complex-valued exit face wave functions is developed to reduce the artifacts arising from objective lens aberrations. However, a much larger field of view is crucial for mapping strain in the active regions of complex structures like latest generation metal-oxide-semiconductor field-effect transistors (MOSFETs). To overcome this, a complementary approach based on electron holography is proposed. The technique relies on the reconstruction of the phase shifts in the diffracted electron beams from a focal series of dark-field images using recently developed exit-face wave function reconstruction algorithm. Combining high spatial resolution, better than 1 nm, with a field of view of about 1 {mu}m in each dimension, simultaneous strain measurements on the array of MOSFETs are possible. Owing to the much lower electron doses used in holography experiments when compared to conventional quantitative methods, the proposed approach allows to map compositional distribution in electron beam sensitive materials such as InGaN heterostructures without alteration of the original morphology and chemical composition. Moreover, dark-field holography experiments can be performed on thicker specimens than the ones required for high-resolution TEM, which in turn reduces the thin foil relaxation. (orig.)

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

    NARCIS (Netherlands)

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

    2005-01-01

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

  1. Instrumentation for in situ flow electrochemical Scanning Transmission X-ray Microscopy (STXM)

    Science.gov (United States)

    Prabu, Vinod; Obst, Martin; Hosseinkhannazer, Hooman; Reynolds, Matthew; Rosendahl, Scott; Wang, Jian; Hitchcock, Adam P.

    2018-06-01

    We report the design and performance of a 3-electrode device for real time in situ scanning transmission X-ray microscopy studies of electrochemical processes under both static (sealed, non-flow) conditions and with a continuous flow of electrolytes. The device was made using a combination of silicon microfabrication and 3D printing technologies. The performance is illustrated by results of a study of copper deposition and stripping at a gold working electrode. X-ray absorption spectromicroscopy at the Cu 2p edge was used to follow the evolution as a function of potential and time of the spatial distributions of Cu(0) and Cu(i) species electro-deposited from an aqueous solution of copper sulphate. The results are interpreted in terms of competing mechanisms for the reduction of Cu(ii).

  2. Avoiding drying-artifacts in transmission electron microscopy: Characterizing the size and colloidal state of nanoparticles

    Science.gov (United States)

    Michen, Benjamin; Geers, Christoph; Vanhecke, Dimitri; Endes, Carola; Rothen-Rutishauser, Barbara; Balog, Sandor; Petri-Fink, Alke

    2015-01-01

    Standard transmission electron microscopy nanoparticle sample preparation generally requires the complete removal of the suspending liquid. Drying often introduces artifacts, which can obscure the state of the dispersion prior to drying and preclude automated image analysis typically used to obtain number-weighted particle size distribution. Here we present a straightforward protocol for prevention of the onset of drying artifacts, thereby allowing the preservation of in-situ colloidal features of nanoparticles during TEM sample preparation. This is achieved by adding a suitable macromolecular agent to the suspension. Both research- and economically-relevant particles with high polydispersity and/or shape anisotropy are easily characterized following our approach (http://bsa.bionanomaterials.ch), which allows for rapid and quantitative classification in terms of dimensionality and size: features that are major targets of European Union recommendations and legislation. PMID:25965905

  3. Rapid solidification growth mode transitions in Al-Si alloys by dynamic transmission electron microscopy

    International Nuclear Information System (INIS)

    Roehling, John D.; Coughlin, Daniel R.; Gibbs, John W.; Baldwin, J. Kevin; Mertens, James C.E.; Campbell, Geoffrey H.; Clarke, Amy J.; McKeown, Joseph T.

    2017-01-01

    In situ dynamic transmission electron microscope (DTEM) imaging of Al-Si thin-film alloys was performed to investigate rapid solidification behavior. Solidification of alloys with compositions from 1 to 15 atomic percent Si was imaged during pulsed laser melting and subsequent solidification. Solely α-Al solidification was observed in Al-1Si and Al-3Si alloys, and solely kinetically modified eutectic growth was observed in Al-6Si and Al-9Si alloys. A transition in the solidification mode in eutectic and hypereutectic alloys (Al-12Si and Al-15Si) from nucleated α-Al dendrites at lower solidification velocities to planar eutectic growth at higher solidification velocities was observed, departing from trends previously seen in laser-track melting experiments. Comparisons of the growth modes and corresponding velocities are compared with previous solidification models, and implications regarding the models are discussed.

  4. Electron Source Brightness and Illumination Semi-Angle Distribution Measurement in a Transmission Electron Microscope.

    Science.gov (United States)

    Börrnert, Felix; Renner, Julian; Kaiser, Ute

    2018-05-21

    The electron source brightness is an important parameter in an electron microscope. Reliable and easy brightness measurement routes are not easily found. A determination method for the illumination semi-angle distribution in transmission electron microscopy is even less well documented. Herein, we report a simple measurement route for both entities and demonstrate it on a state-of-the-art instrument. The reduced axial brightness of the FEI X-FEG with a monochromator was determined to be larger than 108 A/(m2 sr V).

  5. Transmission electron microscopy in molecular structural biology: A historical survey.

    Science.gov (United States)

    Harris, J Robin

    2015-09-01

    In this personal, historic account of macromolecular transmission electron microscopy (TEM), published data from the 1940s through to recent times is surveyed, within the context of the remarkable progress that has been achieved during this time period. The evolution of present day molecular structural biology is described in relation to the associated biological disciplines. The contribution of numerous electron microscope pioneers to the development of the subject is discussed. The principal techniques for TEM specimen preparation, thin sectioning, metal shadowing, negative staining and plunge-freezing (vitrification) of thin aqueous samples are described, with a selection of published images to emphasise the virtues of each method. The development of digital image analysis and 3D reconstruction is described in detail as applied to electron crystallography and reconstructions from helical structures, 2D membrane crystals as well as single particle 3D reconstruction of icosahedral viruses and macromolecules. The on-going development of new software, algorithms and approaches is highlighted before specific examples of the historical progress of the structural biology of proteins and viruses are presented. Copyright © 2014 Elsevier Inc. All rights reserved.

  6. Iterative reconstruction of magnetic induction using Lorentz transmission electron tomography

    International Nuclear Information System (INIS)

    Phatak, C.; Gürsoy, D.

    2015-01-01

    Intense ongoing research on complex nanomagnetic structures requires a fundamental understanding of the 3D magnetization and the stray fields around the nano-objects. 3D visualization of such fields offers the best way to achieve this. Lorentz transmission electron microscopy provides a suitable combination of high resolution and ability to quantitatively visualize the magnetization vectors using phase retrieval methods. In this paper, we present a formalism to represent the magnetic phase shift of electrons as a Radon transform of the magnetic induction of the sample. Using this formalism, we then present the application of common tomographic methods particularly the iterative methods, to reconstruct the 3D components of the vector field. We present an analysis of the effect of missing wedge and the limited angular sampling as well as reconstruction of complex 3D magnetization in a nanowire using simulations. - Highlights: • We present a formalism to represent electron-optical magnetic phase shift as a Radon transform of the 3D magnetic induction of the nano-object. • We have analyzed four different tomographic reconstruction methods for vectorial data reconstruction. • Reconstruction methods were tested for varying experimental limitations such as limited tilt range and limited angular sampling. • The analysis showed that Gridrec and SIRT methods performed better with lower errors than other reconstruction methods

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

    Science.gov (United States)

    Kobler, Aaron; Kübel, Christian

    2018-01-01

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

  8. A simple way to obtain backscattered electron images in a scanning transmission electron microscope.

    Science.gov (United States)

    Tsuruta, Hiroki; Tanaka, Shigeyasu; Tanji, Takayoshi; Morita, Chiaki

    2014-08-01

    We have fabricated a simple detector for backscattered electrons (BSEs) and incorporated the detector into a scanning transmission electron microscope (STEM) sample holder. Our detector was made from a 4-mm(2) Si chip. The fabrication procedure was easy, and similar to a standard transmission electron microscopy (TEM) sample thinning process based on ion milling. A TEM grid containing particle objects was fixed to the detector with a silver paste. Observations were carried out using samples of Au and latex particles at 75 and 200 kV. Such a detector provides an easy way to obtain BSE images in an STEM. © The Author 2014. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

  9. Investigation of superthermal asymmetric electron distributions using electron cyclotron wave transmission in tokamaks

    International Nuclear Information System (INIS)

    Giruzzi, G.; Fidone, I.; Marcha, M.J.

    1991-01-01

    The asymmetric electron distribution generated during lower hybrid current drive has been computed using a 3-D Fokker-Planck code. The superthermal tail and the resulting current are generally a combination of two components streaming in opposite toroidal directions. An appropriate diagnostic method for experimental investigation of the two superthermal populations is wave transmission of two equivalent rays with equal and opposite values of the refractive index. These equivalent rays can be realized by launching the waves from symmetric positions with respect ot the equatorial plane at equal and opposite angles in the toroidal direction. Using an appropriate ray tracing code, the damping of the two rays is computed and it is shown that it results from electrons with opposite parallel velocities. The differential transmission is then a measure of the overall asymmetry of the electron momentum distribution. (author). 12 refs, 8 figs

  10. Directly Observing Micelle Fusion and Growth in Solution by Liquid-Cell Transmission Electron Microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Parent, Lucas R. [Department; amp, Biochemistry, University of California, San Diego, La Jolla, California 92093, United States; Bakalis, Evangelos [Dipartimento; Ramírez-Hernández, Abelardo [Materials; Institute; Kammeyer, Jacquelin K. [Department; amp, Biochemistry, University of California, San Diego, La Jolla, California 92093, United States; Park, Chiwoo [Department; de Pablo, Juan [Materials; Institute; Zerbetto, Francesco [Dipartimento; Patterson, Joseph P. [Department; amp, Biochemistry, University of California, San Diego, La Jolla, California 92093, United States; Laboratory; Gianneschi, Nathan C. [Department; amp, Biochemistry, University of California, San Diego, La Jolla, California 92093, United States

    2017-11-16

    Amphiphilic small molecules and polymers form commonplace nanoscale macromolecular compartments and bilayers, and as such are truly essential components in all cells and in many cellular processes. The nature of these architectures, including their formation, phase changes, and stimuli-response behaviors, is necessary for the most basic functions of life, and over the past half-century, these natural micellar structures have inspired a vast diversity of industrial products, from biomedicines to detergents, lubricants, and coatings. The importance of these materials and their ubiquity have made them the subject of intense investigation regarding their nanoscale dynamics with increasing interest in obtaining sufficient temporal and spatial resolution to directly observe nanoscale processes. However, the vast majority of experimental methods involve either bulk-averaging techniques including light, neutron, and X-ray scattering, or are static in nature including even the most advanced cryogenic transmission electron microscopy techniques. Here, we employ in situ liquid-cell transmission electron microscopy (LCTEM) to directly observe the evolution of individual amphiphilic block copolymer micellar nanoparticles in solution, in real time with nanometer spatial resolution. These observations, made on a proof-of-concept bioconjugate polymer amphiphile, revealed growth and evolution occurring by unimer addition processes and by particle-particle collision-and-fusion events. The experimental approach, combining direct LCTEM observation, quantitative analysis of LCTEM data, and correlated in silico simulations, provides a unique view of solvated soft matter nanoassemblies as they morph and evolve in time and space, enabling us to capture these phenomena in solution.

  11. Secondary Electron Emission Materials for Transmission Dynodes in Novel Photomultipliers: A Review

    Directory of Open Access Journals (Sweden)

    Shu Xia Tao

    2016-12-01

    Full Text Available Secondary electron emission materials are reviewed with the aim of providing guidelines for the future development of novel transmission dynodes. Materials with reflection secondary electron yield higher than three and transmission secondary electron yield higher than one are tabulated for easy reference. Generations of transmission dynodes are listed in the order of the invention time with a special focus on the most recent atomic-layer-deposition synthesized transmission dynodes. Based on the knowledge gained from the survey of secondary election emission materials with high secondary electron yield, an outlook of possible improvements upon the state-of-the-art transmission dynodes is provided.

  12. In situ fatigue loading stage inside scanning electron microscope

    Science.gov (United States)

    Telesman, Jack; Kantzos, Peter; Brewer, David

    1988-01-01

    A fatigue loading stage inside a scanning electron microscopy (SEM) was developed. The stage allows dynamic and static high-magnification and high-resolution viewing of the fatigue crack initiation and crack propagation processes. The loading stage is controlled by a closed-loop servohydraulic system. Maximum load is 1000 lb (4450 N) with test frequencies ranging up to 30 Hz. The stage accommodates specimens up to 2 inches (50 mm) in length and tolerates substantial specimen translation to view the propagating crack. At room temperature, acceptable working resolution is obtainable for magnifications ranging up to 10,000X. The system is equipped with a high-temperature setup designed for temperatures up to 2000 F (1100 C). The signal can be videotaped for further analysis of the pertinent fatigue damage mechanisms. The design allows for quick and easy interchange and conversion of the SEM from a loading stage configuration to its normal operational configuration and vice versa. Tests are performed entirely in the in-situ mode. In contrast to other designs, the NASA design has greatly extended the life of the loading stage by not exposing the bellows to cyclic loading. The loading stage was used to investigate the fatigue crack growth mechanisms in the (100)-oriented PWA 1480 single-crystal, nickel-based supperalloy. The high-magnification observations revealed the details of the crack growth processes.

  13. In situ occupational and general public exposure to VHF/UHF transmission for air traffic communication.

    Science.gov (United States)

    Joseph, Wout; Goeminne, Francis; Verloock, Leen; Vermeeren, Günter; Martens, Luc

    2012-09-01

    Occupational and general public exposure due to very high frequency (VHF)/ultra high frequency (UHF) transmission centres for verbal communication for air traffic control is investigated in situ for the first time. These systems are used for communication with aircraft, resulting in different human exposure from that of classical broadcasting. Measurement methods are proposed for the exposure assessment, and a measurement campaign is executed in three transmission centres. By investigating the temporal behaviour of the VHF signals for 6 d, a realistic worst-case duty cycle of 29 % is determined. Periods of high exposures corresponding with high aircraft traffic are from 7 a.m. to 1 p.m. and in the evening. All measured electric-field values satisfy the International Commission on Non-ionizing Radiation Protection guidelines. Fields vary from 0.2 to 21.1 V m(-1) for occupational exposure and from 0.007 to 8.0 V m(-1) for general public exposure. The average fields equal 5.2 V m(-1) for workers, and 0.7 V m(-1) for general public.

  14. In situ occupational and general public exposure to VHF/UHF transmission for air traffic communication

    International Nuclear Information System (INIS)

    Joseph, W.; Goeminne, F.; Verloock, L.; Vermeeren, G.; Martens, L.

    2012-01-01

    Occupational and general public exposure due to very high frequency (VHF)/ultra high frequency (UHF) transmission centres for verbal communication for air traffic control is investigated in situ for the first time. These systems are used for communication with aircraft, resulting in different human exposure from that of classical broadcasting. Measurement methods are proposed for the exposure assessment, and a measurement campaign is executed in three transmission centres. By investigating the temporal behaviour of the VHF signals for 6 d, a realistic worst-case duty cycle of 29 % is determined. Periods of high exposures corresponding with high aircraft traffic are from 7 a.m. to 1 p.m. and in the evening. All measured electric field values satisfy the International Commission on Non-ionizing Radiation Protection guidelines. Fields vary from 0.2 to 21.1 V m -1 for occupational exposure and from 0.007 to 8.0 V m -1 for general public exposure. The average fields equal 5.2 V m -1 for workers, and 0.7 V m -1 for general public. (authors)

  15. On the role of the gas environment, electron-dose-rate, and sample on the image resolution in transmission electron microscopy

    DEFF Research Database (Denmark)

    Ek, Martin; Jespersen, Sebastian Pirel Fredsgaard; Damsgaard, Christian Danvad

    2016-01-01

    on the electron-dose-rate. In this article, we demonstrate that both the total and areal electron-dose-rates work as descriptors for the dose-rate-dependent resolution and are related through the illumination area. Furthermore, the resolution degradation was observed to occur gradually over time after......The introduction of gaseous atmospheres in transmission electron microscopy offers the possibility of studying materials in situ under chemically relevant environments. The presence of a gas environment can degrade the resolution. Surprisingly, this phenomenon has been shown to depend...... initializing the illumination of the sample and gas by the electron beam. The resolution was also observed to be sensitive to the electrical conductivity of the sample. These observations can be explained by a charge buildup over the electron-illuminated sample area, caused by the beam–gas–sample interaction...

  16. Visualization of bacterial polysaccharides by scanning transmission electron microscopy.

    Science.gov (United States)

    Wolanski, B S; McAleer, W J; Hilleman, M R

    1983-04-01

    Highly purified capsular polysaccharides of Neisseria meningitidis groups A, B, and C have been visualized by high resolution Scanning Transmission Electron Microscopy (STEM). Spheroidal macromolecules approximately 200 A in diameter are characteristic of the Meningococcus A and C polysaccharides whereas filaments that are 400-600 A in length are found in Meningococcus B polysaccharide preparations. Filaments are occasionally found associated with the spheroidal Meningococcus A and C polysaccharides and it is proposed that these structures are composed of a long (1-4 microns) filament or filaments that are arranged in spheroidal molecules or micelles of high molecular weight. The Meningococcus B polysaccharide, by contrast, is a short flexuous filament or strand of relatively low molecular weight. A relationship between morphology and antigenicity is proposed.

  17. Transmission electron microscopy analysis of hydroxyapatite nanocrystals from cattle bones

    International Nuclear Information System (INIS)

    Patel, Sangeeta; Wei, Shanghai; Han, Jie; Gao, Wei

    2015-01-01

    In this present study, hydroxyapatite which was obtained from cattle bones has been heat treated at temperature 400 °C and 600 °C. The microstructure after the treatment has been studied in detail using Transmission electron microscopy (TEM) and X-ray diffraction techniques. The TEM results indicate that natural bone consists of collagen and hydroxyapatite nano-crystals which are needle shaped. The heat treatment influences the crystallinity and growth of these hydroxyapatite nano-crystals known as ‘crystal maturation’ or ‘crystal ageing’. - Highlights: • Hydroxyapatite is obtained from cattle bones. • Material has been characterised using XRD and TEM. • Crystal growth and orientation has been studied in detail.

  18. Transmission electron microscope sample holder with optical features

    Science.gov (United States)

    Milas, Mirko [Port Jefferson, NY; Zhu, Yimei [Stony Brook, NY; Rameau, Jonathan David [Coram, NY

    2012-03-27

    A sample holder for holding a sample to be observed for research purposes, particularly in a transmission electron microscope (TEM), generally includes an external alignment part for directing a light beam in a predetermined beam direction, a sample holder body in optical communication with the external alignment part and a sample support member disposed at a distal end of the sample holder body opposite the external alignment part for holding a sample to be analyzed. The sample holder body defines an internal conduit for the light beam and the sample support member includes a light beam positioner for directing the light beam between the sample holder body and the sample held by the sample support member.

  19. Transmission electron microscope cells for use with liquid samples

    Science.gov (United States)

    Khalid, Waqas; Alivisatos, Paul A.; Zettl, Alexander K.

    2016-08-09

    This disclosure provides systems, methods, and devices related to transmission electron microscopy cells for use with liquids. In one aspect a device includes a substrate, a first graphene layer, and a second graphene layer. The substrate has a first surface and a second surface. The first surface defines a first channel, a second channel, and an outlet channel. The first channel and the second channel are joined to the outlet channel. The outlet channel defines a viewport region forming a though hole in the substrate. The first graphene layer overlays the first surface of the substrate, including an interior area of the first channel, the second channel, and the outlet channel. The second graphene layer overlays the first surface of the substrate, including open regions defined by the first channel, the second channel, and the outlet channel.

  20. Transmission electron microscopy analysis of hydroxyapatite nanocrystals from cattle bones

    Energy Technology Data Exchange (ETDEWEB)

    Patel, Sangeeta, E-mail: spt658@aucklanduni.ac.nz [Department of Chemical and Materials Engineering, The University of Auckland, 20 Symonds Street, Auckland 1010 (New Zealand); Wei, Shanghai [Department of Chemical and Materials Engineering, The University of Auckland, 20 Symonds Street, Auckland 1010 (New Zealand); Han, Jie [Department of Civil and Environmental Engineering, University of Illinois at Urbana-Champaign, 205 North Mathews Avenue, Urbana, IL (United States); Gao, Wei [Department of Chemical and Materials Engineering, The University of Auckland, 20 Symonds Street, Auckland 1010 (New Zealand)

    2015-11-15

    In this present study, hydroxyapatite which was obtained from cattle bones has been heat treated at temperature 400 °C and 600 °C. The microstructure after the treatment has been studied in detail using Transmission electron microscopy (TEM) and X-ray diffraction techniques. The TEM results indicate that natural bone consists of collagen and hydroxyapatite nano-crystals which are needle shaped. The heat treatment influences the crystallinity and growth of these hydroxyapatite nano-crystals known as ‘crystal maturation’ or ‘crystal ageing’. - Highlights: • Hydroxyapatite is obtained from cattle bones. • Material has been characterised using XRD and TEM. • Crystal growth and orientation has been studied in detail.

  1. Study of electron transmission through thin metallic films by the electron moessbauer spectroscopy

    International Nuclear Information System (INIS)

    Babikova, Yu.F.; Vakar, O.M.; Gruzin, O.M.; Petrikin, Yu.V.

    1983-01-01

    Results of the experimental study of the transmission of conversion electrons through aluminium, iron, tin and gold films are presented. Absorption of resonance electrons of the Moessbauer nuclide 57 Fe, formed during target irradiation with γ-quanta of 57 Co source in chromium matrix has been studied. It is asserted that absorption of conversion electrons in films of different elements is similar; at that, like in the case of β-particles, the law of absorption of resonance electrons, emitted from the flat layer, is exponential For conversion electrons of the Moessbauer nuclide 57 Fe the absorption coefficient is (0.025+-0.002) cm 2 /μg, which in the case of iron absorbing film corresponds to (20.0+-1.0)x10 4 cm -1

  2. Development of wave length-dispersive soft x-ray emission spectrometers for transmission electron microscopes - an introduction of valence electron spectroscopy for transmission electron microscopy

    International Nuclear Information System (INIS)

    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 Mα-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 π- and σ-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. (author)

  3. Scanning transmission electron microscopy: Albert Crewe's vision and beyond

    International Nuclear Information System (INIS)

    Krivanek, Ondrej L.; Chisholm, Matthew F.; Murfitt, Matthew F.; Dellby, Niklas

    2012-01-01

    Some four decades were needed to catch up with the vision that Albert Crewe and his group had for the scanning transmission electron microscope (STEM) in the nineteen sixties and seventies: attaining 0.5 Å resolution, and identifying single atoms spectroscopically. With these goals now attained, STEM developments are turning toward new directions, such as rapid atomic resolution imaging and exploring atomic bonding and electronic properties of samples at atomic resolution. The accomplishments and the future challenges are reviewed and illustrated with practical examples. -- Highlights: ► TV-rate STEM imaging of heavy atoms is demonstrated. ► DNA sequencing by STEM dark field imaging should be possible at a rate of 10 6 bases/s. ► Individual silicon atom impurities in graphene are imaged atom-by-atom. ► Single atoms of nitrogen and boron incorporated in graphene are imaged spectroscopically. ► Bonding of individual atoms can be probed by analyzing the fine structures of their EEL spectra.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2003-09-01

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

  5. High-resolution imaging in the scanning transmission electron microscope

    International Nuclear Information System (INIS)

    Pennycook, S.J.; Jesson, D.E.

    1992-03-01

    The high-resolution imaging of crystalline materials in the scanning transmission electron microscopy (STEM) is reviewed with particular emphasis on the conditions under which an incoherent image can be obtained. It is shown that a high-angle annular detector can be used to break the coherence of the imaging process, in the transverse plane through the geometry of the detector, or in three dimensions if multiphonon diffuse scattering is detected. In the latter case, each atom can be treated as a highly independent source of high-angle scattering. The most effective fast electron states are therefore tightly bound s-type Bloch states. Furthermore, they add constructively for each incident angle in the coherent STEM probe, so that s states are responsible for practically the entire image contrast. Dynamical effects are largely removed, and almost perfect incoherent imaging is achieved. s states are relatively insensitive to neighboring strings, so that incoherent imaging is maintained for superlattice and interfaces, and supercell calculations are unnecessary. With an optimum probe profile, the incoherent image represents a direct image of the crystal projection, with compositional sensitivity built in through the strong dependence of the scattering cross sections on atomic number Z

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

    Energy Technology Data Exchange (ETDEWEB)

    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).

  7. Transmission electron microscopy a textbook for materials science

    CERN Document Server

    Williams, David B

    1996-01-01

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

  8. Transmission Electron Microscopy of Magnetite Plaquettes in Orgueil

    Science.gov (United States)

    Chan, Q. H. S.; Han, J.; Zolensky, M.

    2016-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2010-04-15

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

  10. Real-time studies of battery electrochemical reactions inside a transmission electron microscope.

    Energy Technology Data Exchange (ETDEWEB)

    Leung, Kevin; Hudak, Nicholas S.; Liu, Yang; Liu, Xiaohua H.; Fan, Hongyou; Subramanian, Arunkumar; Shaw, Michael J.; Sullivan, John Patrick; Huang, Jian Yu

    2012-01-01

    We report the development of new experimental capabilities and ab initio modeling for real-time studies of Li-ion battery electrochemical reactions. We developed three capabilities for in-situ transmission electron microscopy (TEM) studies: a capability that uses a nanomanipulator inside the TEM to assemble electrochemical cells with ionic liquid or solid state electrolytes, a capability that uses on-chip assembly of battery components on to TEM-compatible multi-electrode arrays, and a capability that uses a TEM-compatible sealed electrochemical cell that we developed for performing in-situ TEM using volatile battery electrolytes. These capabilities were used to understand lithiation mechanisms in nanoscale battery materials, including SnO{sub 2}, Si, Ge, Al, ZnO, and MnO{sub 2}. The modeling approaches used ab initio molecular dynamics to understand early stages of ethylene carbonate reduction on lithiated-graphite and lithium surfaces and constrained density functional theory to understand ethylene carbonate reduction on passivated electrode surfaces.

  11. Digital acquisition and processing of electron micrographs using a scanning transmission electron microscope

    International Nuclear Information System (INIS)

    Engel, A.; Christen, F.; Michel, B.

    1981-01-01

    A digital acquisition system that collects multichannel information from a scanning transmission electron microscope (STEM) and its application are described. The hardware comprises (i) single electron counting detectors, (ii) a digital scan generator, (iii) a digital multi-channel on-line processor, (iv) an interface to a minicomputer, and (v) a display system. Experimental results characterizing these components are presented, and their performance is discussed. The software includes assembler coded programs for dynamic file maintenance and fast acquisition of image data, a display driver, and FORTRAN coded application programs. The usefulness of digitized STEM is illustrated by a variety of biological applications. (orig.)

  12. Scanning transmission X-ray microscopy probe for in situ mechanism study of graphene-oxide-based resistive random access memory.

    Science.gov (United States)

    Nho, Hyun Woo; Kim, Jong Yun; Wang, Jian; Shin, Hyun-Joon; Choi, Sung-Yool; Yoon, Tae Hyun

    2014-01-01

    Here, an in situ probe for scanning transmission X-ray microscopy (STXM) has been developed and applied to the study of the bipolar resistive switching (BRS) mechanism in an Al/graphene oxide (GO)/Al resistive random access memory (RRAM) device. To perform in situ STXM studies at the C K- and O K-edges, both the RRAM junctions and the I0 junction were fabricated on a single Si3N4 membrane to obtain local XANES spectra at these absorption edges with more delicate I0 normalization. Using this probe combined with the synchrotron-based STXM technique, it was possible to observe unique chemical changes involved in the BRS process of the Al/GO/Al RRAM device. Reversible oxidation and reduction of GO induced by the externally applied bias voltages were observed at the O K-edge XANES feature located at 538.2 eV, which strongly supported the oxygen ion drift model that was recently proposed from ex situ transmission electron microscope studies.

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

    Science.gov (United States)

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

    2018-02-01

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

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

    KAUST Repository

    Zhang, Daliang

    2018-01-18

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

  15. Cryo-transmission electron microscopy of Ag nanoparticles grown on an ionic liquid substrate

    KAUST Repository

    Anjum, Dalaver H.

    2010-07-01

    We report a novel method of growing silver nanostructures by cathodic sputtering onto an ionic liquid (IL) and our visualization by transmission cryo-electron microscopy to avoid beam-induced motion of the nanoparticles. By freezing the IL suspension and controlling electron dose, we can assess properties of particle size, morphology, crystallinity, and aggregation in situ and at high detail. We observed round silver nanoparticles with a well-defined diameter of 7.0 ± 1.5 nm that are faceted with crystalline cubic structures and ∼80% of the particles have multiply twinned faults. We also applied cryo-electron tomography to investigate the structure of the nanoparticles and to directly visualize the IL wetting around them. In addition to particles, we observed nanorods that appear to have assembled from individual nanoparticles. Reexamination of the samples after 4-5 days from initial preparation showed significant changes in morphology, and potential mechanisms for this are discussed. © 2010 Materials Research Society.

  16. Electron beam dynamics in an ultrafast transmission electron microscope with Wehnelt electrode.

    Science.gov (United States)

    Bücker, K; Picher, M; Crégut, O; LaGrange, T; Reed, B W; Park, S T; Masiel, D J; Banhart, F

    2016-12-01

    High temporal resolution transmission electron microscopy techniques have shown significant progress in recent years. Using photoelectron pulses induced by ultrashort laser pulses on the cathode, these methods can probe ultrafast materials processes and have revealed numerous dynamic phenomena at the nanoscale. Most recently, the technique has been implemented in standard thermionic electron microscopes that provide a flexible platform for studying material's dynamics over a wide range of spatial and temporal scales. In this study, the electron pulses in such an ultrafast transmission electron microscope are characterized in detail. The microscope is based on a thermionic gun with a Wehnelt electrode and is operated in a stroboscopic photoelectron mode. It is shown that the Wehnelt bias has a decisive influence on the temporal and energy spread of the picosecond electron pulses. Depending on the shape of the cathode and the cathode-Wehnelt distance, different emission patterns with different pulse parameters are obtained. The energy spread of the pulses is determined by space charge and Boersch effects, given by the number of electrons in a pulse. However, filtering effects due to the chromatic aberrations of the Wehnelt electrode allow the extraction of pulses with narrow energy spreads. The temporal spread is governed by electron trajectories of different length and in different electrostatic potentials. High temporal resolution is obtained by excluding shank emission from the cathode and aberration-induced halos in the emission pattern. By varying the cathode-Wehnelt gap, the Wehnelt bias, and the number of photoelectrons in a pulse, tradeoffs between energy and temporal resolution as well as beam intensity can be made as needed for experiments. Based on the characterization of the electron pulses, the optimal conditions for the operation of ultrafast TEMs with thermionic gun assembly are elaborated. Copyright © 2016 Elsevier B.V. All rights reserved.

  17. Collaborative Research and Development. Delivery Order 0006: Transmission Electron Microscope Image Modeling and Semiconductor Heterointerface Characterization

    National Research Council Canada - National Science Library

    Mahalingam, Krishnamurthy

    2006-01-01

    .... Transmission electron microscope (TEM) characterization studies were performed on a variety of novel III-V semiconductor heterostructures being developed for advanced optoelectronic device applications...

  18. In situ hybridization at the electron microscope level: hybrid detection by autoradiography and colloidal gold.

    Science.gov (United States)

    Hutchison, N J; Langer-Safer, P R; Ward, D C; Hamkalo, B A

    1982-11-01

    In situ hybridization has become a standard method for localizing DNA or RNA sequences in cytological preparations. We developed two methods to extend this technique to the transmission electron microscope level using mouse satellite DNA hybridization to whole mount metaphase chromosomes as the test system. The first method devised is a direct extension of standard light microscope level using mouse satellite DNA hybridization to whole mount metaphase chromosomes as the test system. The first method devised is a direct extension of standard light microscope in situ hybridization. Radioactively labeled complementary RNA (cRNA) is hybridized to metaphase chromosomes deposited on electron microscope grids and fixed in 70 percent ethanol vapor; hybridixation site are detected by autoradiography. Specific and intense labeling of chromosomal centromeric regions is observed even after relatively short exposure times. Inerphase nuclei present in some of the metaphase chromosome preparations also show defined paatterms of satellite DNA labeling which suggests that satellite-containing regions are associate with each other during interphase. The sensitivity of this method is estimated to at least as good as that at the light microscope level while the resolution is improved at least threefold. The second method, which circumvents the use of autoradiogrphic detection, uses biotin-labeled polynucleotide probes. After hybridization of these probes, either DNA or RNA, to fixed chromosomes on grids, hybrids are detected via reaction is improved at least threefold. The second method, which circumvents the use of autoradiographic detection, uses biotin-labeled polynucleotide probes. After hybridization of these probes, either DNA or RNA, to fixed chromosomes on grids, hybrids are detected via reaction with an antibody against biotin and secondary antibody adsorbed to the surface of over centromeric heterochromatin and along the associated peripheral fibers. Labeling is on average

  19. Non-uniform shrinkage of multiple-walled carbon nanotubes under in situ electron beam irradiation

    Energy Technology Data Exchange (ETDEWEB)

    Li, Lunxiong [South China Normal University, Brain Science Institute, Guangzhou (China); Xiamen University, China-Australia Joint Laboratory for Functional Nanomaterials and Physics Department, Xiamen (China); Su, Jiangbin [Xiamen University, China-Australia Joint Laboratory for Functional Nanomaterials and Physics Department, Xiamen (China); Chang Zhou University, School of Mathematics and Physics, Changzhou (China); Zhu, Xianfang [Xiamen University, China-Australia Joint Laboratory for Functional Nanomaterials and Physics Department, Xiamen (China)

    2016-10-15

    Instability of multiple-walled carbon nanotubes (MWCNTs) was investigated by in situ transmission electron microscopy at room temperature. Specially, the non-uniform shrinkage of tubes was found: The pristine MWCNT shrank preferentially in its axial direction from the most curved free cap end of the tube, but the shrinkage of the tube diameter was offset by the axial shrinkage: For the complex MWCNT, the two inner MWCNTs also preferentially axially shrank from their most curved cap ends and separated from each other. However, for the effect of the radial pressure from the out walls which enveloped the two inner tubes and the tube amorphization, the two inner tubes were extruded to come close to each other and finally touched again. The new ''evaporation'' and ''diffusion'' mechanisms of carbon atoms as driven by the nano-curvature of CNT and the electron beam-induced athermal activation were suggested to explain the above phenomena. (orig.)

  20. AIMgSil Alloy Characterization Using Transmission Electron Microscope (TEM)

    International Nuclear Information System (INIS)

    Masrukan; Elman, P.

    1996-01-01

    The aging alloy of AIMgSil containing Mg 2 Si of 1.29 % has been done with the following steps: e.q (a) part of the specimen was heated at 400 o C during 3 hours, and (b) the other part was done with solution treatment at 550 o C followed by quenching. After quenching a part of the specimen was aged at room temperature and other specimen was aged at 160 o C during 16 hours. After the specimen had been heated, then it was shaped into thin foil to be examined by Transmission Electron Microscope. The result showed that the heating at temperature of 400 o C during 3 hours created a second phase (i.e.Mg 2 Si) was like stick shape with the hexagonal structure at [0111] orientation and matrix [001], and the hardness was 31 HB. The aging of specimen at room temperature gave result a GP zone which was like the needles shape in the dislocation area of the face center cubic structure at [111] orientation and [111] matrix. The hardness obtained was 64 HB. In the other hand the aging process at temperature of 160 o C within 16 hours have resulted the precipitate which was greater than that of the former needle shaped as the face center cubic structure without dislocation at matrix with [111] orientation and [114] matrix. The hardness at this condition was 94 HB

  1. Visualizing aquatic bacteria by light and transmission electron microscopy.

    Science.gov (United States)

    Silva, Thiago P; Noyma, Natália P; Duque, Thabata L A; Gamalier, Juliana P; Vidal, Luciana O; Lobão, Lúcia M; Chiarini-Garcia, Hélio; Roland, Fábio; Melo, Rossana C N

    2014-01-01

    The understanding of the functional role of aquatic bacteria in microbial food webs is largely dependent on methods applied to the direct visualization and enumeration of these organisms. While the ultrastructure of aquatic bacteria is still poorly known, routine observation of aquatic bacteria by light microscopy requires staining with fluorochromes, followed by filtration and direct counting on filter surfaces. Here, we used a new strategy to visualize and enumerate aquatic bacteria by light microscopy. By spinning water samples from varied tropical ecosystems in a cytocentrifuge, we found that bacteria firmly adhere to regular slides, can be stained by fluorochoromes with no background formation and fast enumerated. Significant correlations were found between the cytocentrifugation and filter-based methods. Moreover, preparations through cytocentrifugation were more adequate for bacterial viability evaluation than filter-based preparations. Transmission electron microscopic analyses revealed a morphological diversity of bacteria with different internal and external structures, such as large variation in the cell envelope and capsule thickness, and presence or not of thylakoid membranes. Our results demonstrate that aquatic bacteria represent an ultrastructurally diverse population and open avenues for easy handling/quantification and better visualization of bacteria by light microscopy without the need of filter membranes.

  2. Observations of silicon carbide by high resolution transmission electron microscopy

    International Nuclear Information System (INIS)

    Smith, D.J.; Jepps, N.W.; Page, T.F.

    1978-01-01

    High resolution transmission electron microscopy techniques, principally involving direct lattice imaging, have been used as part of a study of the crystallography and phase transformation mechanics of silicon carbide polytypes. In particular, the 3C (cubic) and 6H (hexagonal) polytypes have been examined together with partially transformed structural mixtures. Although direct observation of two-dimensional atomic structures was not possible at an operating voltage of 100 kV, considerable microstructural information has been obtained by careful choice of the experimental conditions. In particular, tilted beam observations of the 0.25 nm lattice fringes have been made in the 3C polytype for two different brace 111 brace plane arrays in order to study the dimensions and coherency of finely-twinned regions together with brace 0006 brace and brace 1 0 bar1 2 brace lattice images in the 6H polytype which allow the detailed stacking operations to be resolved. Lower resolution lattice images formed with axial illumination have also been used to study the nature of the 3C → 6H transformation and results are presented showing that the transformation interface may originate with fine twinning of the 3C structure followed by growth of the resultant 6H regions. Observations have been made of the detailed stepped structure of this interface together with the stacking fault distribution in the resultant 6H material. (author)

  3. Reference nano-dimensional metrology by scanning transmission electron microscopy

    International Nuclear Information System (INIS)

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

    2013-01-01

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

  4. Transmission electron microscopy of weakly deformed alkali halide crystals

    International Nuclear Information System (INIS)

    Strunk, H.

    1976-01-01

    Transmission electron microscopy (TEM) is applied to the investigation of the dislocation arrangement of [001]-orientated alkali halide crystals (orientation four quadruple slip) deformed into stage I of the work-hardenig curve. The investigations pertain mainly to NaCl - (0.1-1) mole-% NaBr crystals, because these exhibit a relatively long stage I. The time available for observing the specimens is limited by the ionization radiation damage occuring in the microscope. An optimum reduction of the damage rate is achieved by a combination of several experimental techniques that are briefly outlined. The crystals deform essentially in single glide. According to the observations, stage I deformation of pure and weakly alloyed NaCl crystals is characterized by the glide of screw dislocations, which bow out between jogs and drag dislocation dipoles behind them. In crystals with >= 0.5 mole-% NaBr this process is not observed to occur. This is attributed to the increased importance of solid solution hardening. (orig.) [de

  5. In situ atomic-level observation of the formation of platinum silicide at platinum-silicon oxide interfaces under electron irradiation

    Directory of Open Access Journals (Sweden)

    Takeshi Nagase

    2018-05-01

    Full Text Available In situ atomic-level observation of the formation of Pt2Si at Pt/SiOx interface by electronic excitation under electron irradiation was performed by using scanning transmission electron microscopy. Scanning of an electron-beam probe stimulates silicide formation at the Pt/SiOx interface; the change in the Pt column corresponding to Pt2Si formation with a crystallographic orientation of (001Pt//(001Pt2Si and [110]Pt//[110]Pt2Si was observed in high-angle annular dark-field images.

  6. Electron beam dynamics in an ultrafast transmission electron microscope with Wehnelt electrode

    Energy Technology Data Exchange (ETDEWEB)

    Bücker, K.; Picher, M.; Crégut, O. [Institut de Physique et Chimie des Matériaux de Strasbourg, UMR 7504 CNRS, Université de Strasbourg, 23 rue du Loess, 67034 Strasbourg (France); LaGrange, T. [Interdisciplinary Centre for Electron Microscopy, École Polytechnique Fédérale de Lausanne, 1015 Lausanne (Switzerland); Reed, B.W.; Park, S.T.; Masiel, D.J. [Integrated Dynamic Electron Solutions, Inc., 5653 Stoneridge Drive 117, Pleasanton, CA 94588 (United States); Banhart, F., E-mail: florian.banhart@ipcms.unistra.fr [Institut de Physique et Chimie des Matériaux de Strasbourg, UMR 7504 CNRS, Université de Strasbourg, 23 rue du Loess, 67034 Strasbourg (France)

    2016-12-15

    High temporal resolution transmission electron microscopy techniques have shown significant progress in recent years. Using photoelectron pulses induced by ultrashort laser pulses on the cathode, these methods can probe ultrafast materials processes and have revealed numerous dynamic phenomena at the nanoscale. Most recently, the technique has been implemented in standard thermionic electron microscopes that provide a flexible platform for studying material's dynamics over a wide range of spatial and temporal scales. In this study, the electron pulses in such an ultrafast transmission electron microscope are characterized in detail. The microscope is based on a thermionic gun with a Wehnelt electrode and is operated in a stroboscopic photoelectron mode. It is shown that the Wehnelt bias has a decisive influence on the temporal and energy spread of the picosecond electron pulses. Depending on the shape of the cathode and the cathode-Wehnelt distance, different emission patterns with different pulse parameters are obtained. The energy spread of the pulses is determined by space charge and Boersch effects, given by the number of electrons in a pulse. However, filtering effects due to the chromatic aberrations of the Wehnelt electrode allow the extraction of pulses with narrow energy spreads. The temporal spread is governed by electron trajectories of different length and in different electrostatic potentials. High temporal resolution is obtained by excluding shank emission from the cathode and aberration-induced halos in the emission pattern. By varying the cathode-Wehnelt gap, the Wehnelt bias, and the number of photoelectrons in a pulse, tradeoffs between energy and temporal resolution as well as beam intensity can be made as needed for experiments. Based on the characterization of the electron pulses, the optimal conditions for the operation of ultrafast TEMs with thermionic gun assembly are elaborated. - Highlights: • A detailed characterization of electron

  7. Direct observations of the MOF (UiO-66) structure by transmission electron microscopy

    KAUST Repository

    Zhu, Liangkui; Zhang, Daliang; Xue, Ming; Li, Huan; Qiu, Shilun

    2013-01-01

    As a demonstration of ab initio structure characterizations of nano metal organic framework (MOF) crystals by high resolution transmission electron microscopy (HRTEM) and electron diffraction tomography methods, a Zr-MOF (UiO-66) structure

  8. Tunable electronic transmission gaps in a graphene superlattice

    International Nuclear Information System (INIS)

    Lu Weitao; Wang Shunjin; Li Wen; Wang Yonglong; Jiang Hua

    2012-01-01

    The transmission in graphene superlattices with adjustable barrier height is investigated using transfer-matrix method. It is found that one could control the angular range of transmission by changing the ratio of incidence energy and barrier height. The transmission as a function of incidence energy has more than one gaps, due to the appearance of evanescent waves in different barriers. Accordingly, more than one conductivity minimums are induced. The transmission gaps could be controlled by adjusting the incidence angle, the barrier height, and the barrier number, which gives the possibility to construct an energy-dependent wavevector filter.

  9. In situ electrical and thermal monitoring of printed electronics by two-photon mapping

    DEFF Research Database (Denmark)

    Pastorelli, Francesco; Accanto, Nicolo; Jørgensen, Mikkel

    2017-01-01

    Printed electronics is emerging as a new, large scale and cost effective technology that will be disruptive in fields such as energy harvesting, consumer electronics and medical sensors. The performance of printed electronic devices relies principally on the carrier mobility and molecular packing...... of the polymer semiconductor material. Unfortunately, the analysis of such materials is generally performed with destructive techniques, which are hard to make compatible with in situ measurements, and pose a great obstacle for the mass production of printed electronics devices. A rapid, in situ, non...

  10. Precision controlled atomic resolution scanning transmission electron microscopy using spiral scan pathways

    Science.gov (United States)

    Sang, Xiahan; Lupini, Andrew R.; Ding, Jilai; Kalinin, Sergei V.; Jesse, Stephen; Unocic, Raymond R.

    2017-03-01

    Atomic-resolution imaging in an aberration-corrected scanning transmission electron microscope (STEM) can enable direct correlation between atomic structure and materials functionality. The fast and precise control of the STEM probe is, however, challenging because the true beam location deviates from the assigned location depending on the properties of the deflectors. To reduce these deviations, i.e. image distortions, we use spiral scanning paths, allowing precise control of a sub-Å sized electron probe within an aberration-corrected STEM. Although spiral scanning avoids the sudden changes in the beam location (fly-back distortion) present in conventional raster scans, it is not distortion-free. “Archimedean” spirals, with a constant angular frequency within each scan, are used to determine the characteristic response at different frequencies. We then show that such characteristic functions can be used to correct image distortions present in more complicated constant linear velocity spirals, where the frequency varies within each scan. Through the combined application of constant linear velocity scanning and beam path corrections, spiral scan images are shown to exhibit less scan distortion than conventional raster scan images. The methodology presented here will be useful for in situ STEM imaging at higher temporal resolution and for imaging beam sensitive materials.

  11. Effects of lattice fluctuations on electronic transmission in metal/conjugated-oligomer/metal structures

    International Nuclear Information System (INIS)

    Yu, Z.G.; Smith, D.L.; Saxena, A.; Bishop, A.R.

    1997-01-01

    The electronic transmission across metal/conjugated-oligomer/metal structures in the presence of lattice fluctuations is studied for short oligomer chains. The lattice fluctuations are approximated by static white noise disorder. Resonant transmission occurs when the energy of an incoming electron coincides with a discrete electronic level of the oligomer. The corresponding transmission peak diminishes in intensity with increasing disorder strength. Because of disorder there is an enhancement of the electronic transmission for energies that lie within the electronic gap of the oligomer. If fluctuations are sufficiently strong, a transmission peak within the gap is found at the midgap energy E=0 for degenerate conjugated oligomers (e.g., trans-polyacetylene) and E≠0 for AB-type degenerate oligomers. These results can be interpreted in terms of soliton-antisoliton states created by lattice fluctuations. copyright 1997 The American Physical Society

  12. Bright-field scanning confocal electron microscopy using a double aberration-corrected transmission electron microscope

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Peng; Behan, Gavin; Kirkland, Angus I. [Department of Materials, University of Oxford, Parks Road, Oxford OX1 3PH (United Kingdom); Nellist, Peter D., E-mail: peter.nellist@materials.ox.ac.uk [Department of Materials, University of Oxford, Parks Road, Oxford OX1 3PH (United Kingdom); Cosgriff, Eireann C.; D' Alfonso, Adrian J.; Morgan, Andrew J.; Allen, Leslie J. [School of Physics, University of Melbourne, Parkville, Victoria 3010 (Australia); Hashimoto, Ayako [Advanced Nano-characterization Center, National Institute for Materials Science (NIMS), 3-13 Sakura, Tsukuba 305-0003 (Japan); Takeguchi, Masaki [Advanced Nano-characterization Center, National Institute for Materials Science (NIMS), 3-13 Sakura, Tsukuba 305-0003 (Japan); High Voltage Electron Microscopy Station, NIMS, 3-13 Sakura, Tsukuba 305-0003 (Japan); Mitsuishi, Kazutaka [Advanced Nano-characterization Center, National Institute for Materials Science (NIMS), 3-13 Sakura, Tsukuba 305-0003 (Japan); Quantum Dot Research Center, NIMS, 3-13 Sakura, Tsukuba 305-0003 (Japan); Shimojo, Masayuki [High Voltage Electron Microscopy Station, NIMS, 3-13 Sakura, Tsukuba 305-0003 (Japan); Advanced Science Research Laboratory, Saitama Institute of Technology, 1690 Fusaiji, Fukaya 369-0293 (Japan)

    2011-06-15

    Scanning confocal electron microscopy (SCEM) offers a mechanism for three-dimensional imaging of materials, which makes use of the reduced depth of field in an aberration-corrected transmission electron microscope. The simplest configuration of SCEM is the bright-field mode. In this paper we present experimental data and simulations showing the form of bright-field SCEM images. We show that the depth dependence of the three-dimensional image can be explained in terms of two-dimensional images formed in the detector plane. For a crystalline sample, this so-called probe image is shown to be similar to a conventional diffraction pattern. Experimental results and simulations show how the diffracted probes in this image are elongated in thicker crystals and the use of this elongation to estimate sample thickness is explored. -- Research Highlights: {yields} The confocal probe image in a scanning confocal electron microscopy image reveals information about the thickness and height of the crystalline layer. {yields} The form of the contrast in a three-dimensional bright-field scanning confocal electron microscopy image can be explained in terms of the confocal probe image. {yields} Despite the complicated form of the contrast in bright-field scanning confocal electron microscopy, we see that depth information is transferred on a 10 nm scale.

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

    International Nuclear Information System (INIS)

    Dörfel, Ilona; Rooch, Heidemarie; Österle, Werner

    2012-01-01

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

  14. Bright-field scanning confocal electron microscopy using a double aberration-corrected transmission electron microscope.

    Science.gov (United States)

    Wang, Peng; Behan, Gavin; Kirkland, Angus I; Nellist, Peter D; Cosgriff, Eireann C; D'Alfonso, Adrian J; Morgan, Andrew J; Allen, Leslie J; Hashimoto, Ayako; Takeguchi, Masaki; Mitsuishi, Kazutaka; Shimojo, Masayuki

    2011-06-01

    Scanning confocal electron microscopy (SCEM) offers a mechanism for three-dimensional imaging of materials, which makes use of the reduced depth of field in an aberration-corrected transmission electron microscope. The simplest configuration of SCEM is the bright-field mode. In this paper we present experimental data and simulations showing the form of bright-field SCEM images. We show that the depth dependence of the three-dimensional image can be explained in terms of two-dimensional images formed in the detector plane. For a crystalline sample, this so-called probe image is shown to be similar to a conventional diffraction pattern. Experimental results and simulations show how the diffracted probes in this image are elongated in thicker crystals and the use of this elongation to estimate sample thickness is explored. Copyright © 2010 Elsevier B.V. All rights reserved.

  15. Low-energy electron transmission through high aspect ratio Al O nanocapillaries

    DEFF Research Database (Denmark)

    Milosavljević, A.R.; Jureta, J.; Víkor, G.

    2009-01-01

    Electron transmission through insulating AlO nanocapillaries of different diameters (40 and 270 nm) and 15 μm length has been investigated for low-energy electrons (2-120 V). The total intensity of transmitted current weakly depends on the incident electron energy and tilt angle defined with resp......Electron transmission through insulating AlO nanocapillaries of different diameters (40 and 270 nm) and 15 μm length has been investigated for low-energy electrons (2-120 V). The total intensity of transmitted current weakly depends on the incident electron energy and tilt angle defined...

  16. Path-separated electron interferometry in a scanning transmission electron microscope

    Science.gov (United States)

    Yasin, Fehmi S.; Harvey, Tyler R.; Chess, Jordan J.; Pierce, Jordan S.; McMorran, Benjamin J.

    2018-05-01

    We report a path-separated electron interferometer within a scanning transmission electron microscope. In this setup, we use a nanofabricated grating as an amplitude-division beamsplitter to prepare multiple spatially separated, coherent electron probe beams. We achieve path separations of 30 nm. We pass the  +1 diffraction order probe through amorphous carbon while passing the 0th and  ‑1 orders through vacuum. The probes are then made to interfere via imaging optics, and we observe an interference pattern at the CCD detector with up to 39.7% fringe visibility. We show preliminary experimental results in which the interference pattern was recorded during a 1D scan of the diffracted probes across a test phase object. These results qualitatively agree with a modeled interference predicted by an independent measurement of the specimen thickness. This experimental design can potentially be applied to phase contrast imaging and fundamental physics experiments, such as an exploration of electron wave packet coherence length.

  17. In situ observation of electron beam-induced phase transformation of CaCO3 to CaO via ELNES at low electron beam energies.

    Science.gov (United States)

    Golla-Schindler, Ute; Benner, Gerd; Orchowski, Alexander; Kaiser, Ute

    2014-06-01

    It is demonstrated that energy-filtered transmission electron microscope enables following of in situ changes of the Ca-L2,3 edge which can originate from variations in both local symmetry and bond lengths. Low accelerating voltages of 20 and 40 kV slow down radiation damage effects and enable study of the start and finish of phase transformations. We observed electron beam-induced phase transformation of single crystalline calcite (CaCO3) to polycrystalline calcium oxide (CaO) which occurs in different stages. The coordination of Ca in calcite is close to an octahedral one streched along the direction. Changes during phase transformation to an octahedral coordination of Ca in CaO go along with a bond length increase by 5 pm, where oxygen is preserved as a binding partner. Electron loss near-edge structure of the Ca-L2,3 edge show four separated peaks, which all shift toward lower energies during phase transformation at the same time the energy level splitting increases. We suggest that these changes can be mainly addressed to the change of the bond length on the order of picometers. An important pre-condition for such studies is stability of the energy drift in the range of meV over at least 1 h, which is achieved with the sub-Ångström low-voltage transmission electron microscope I prototype microscope.

  18. Dynamic Processes in Biology, Chemistry, and Materials Science: Opportunities for UltraFast Transmission Electron Microscopy - Workshop Summary Report

    Energy Technology Data Exchange (ETDEWEB)

    Kabius, Bernd C.; Browning, Nigel D.; Thevuthasan, Suntharampillai; Diehl, Barbara L.; Stach, Eric A.

    2012-07-25

    This report summarizes a 2011 workshop that addressed the potential role of rapid, time-resolved electron microscopy measurements in accelerating the solution of important scientific and technical problems. A series of U.S. Department of Energy (DOE) and National Academy of Science workshops have highlighted the critical role advanced research tools play in addressing scientific challenges relevant to biology, sustainable energy, and technologies that will fuel economic development without degrading our environment. Among the specific capability needs for advancing science and technology are tools that extract more detailed information in realistic environments (in situ or operando) at extreme conditions (pressure and temperature) and as a function of time (dynamic and time-dependent). One of the DOE workshops, Future Science Needs and Opportunities for Electron Scattering: Next Generation Instrumentation and Beyond, specifically addressed the importance of electron-based characterization methods for a wide range of energy-relevant Grand Scientific Challenges. Boosted by the electron optical advancement in the last decade, a diversity of in situ capabilities already is available in many laboratories. The obvious remaining major capability gap in electron microscopy is in the ability to make these direct in situ observations over a broad spectrum of fast (µs) to ultrafast (picosecond [ps] and faster) temporal regimes. In an effort to address current capability gaps, EMSL, the Environmental Molecular Sciences Laboratory, organized an Ultrafast Electron Microscopy Workshop, held June 14-15, 2011, with the primary goal to identify the scientific needs that could be met by creating a facility capable of a strongly improved time resolution with integrated in situ capabilities. The workshop brought together more than 40 leading scientists involved in applying and/or advancing electron microscopy to address important scientific problems of relevance to DOE’s research

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

    Science.gov (United States)

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

    2016-01-01

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

  20. Nanoporous metal film: An energy-dependent transmission device for electron waves

    International Nuclear Information System (INIS)

    Grech, S.; Degiovanni, A.; Lapena, L.; Morin, R.

    2011-01-01

    We measure electron transmission through free-standing ultrathin nanoporous gold films, using the coherent electron beam emitted by sharp field emission tips in a low energy electron projection microscope setup. Transmission coefficient versus electron wavelength plots show periodic oscillations between 75 and 850 eV. These oscillations result from the energy dependence of interference between paths through the gold and paths through the nanometer-sized pores of the film. We reveal that these films constitute high transmittance quantum devices acting on electron waves through a wavelength-dependent complex transmittance defined by the porosity and the thickness of the film.

  1. Thermal behavior of aerosol particles from biomass burning during the BBOP campaign using transmission electron microscopy

    Science.gov (United States)

    Adachi, K.; Ishimoto, H.; Sedlacek, A. J., III; Kleinman, L. I.; Chand, D.; Hubbe, J. M.; Buseck, P. R.

    2017-12-01

    Aerosol samples were collected from wildland and agricultural biomass fires in North America during the 2013 Biomass Burning Observation Project (BBOP). We show in-situ shape and size changes and variations in the compositions of individual particles before and after heating using a transmission electron microscope (TEM). The responses of aerosol particles to heating are important for measurements of their chemical, physical, and optical properties, classification, and determination of origin. However, the thermal behavior of organic aerosol particles is largely unknown. We provide a method to analyze such thermal behavior through heating from room temperature to >600°C by using a heating holder within TEM. The results indicate that individual tar balls (TB; spherical organic material) from biomass burning retained, on average, up to 30% of their volume when heated to 600°C. Chemical analysis reveals that K and Na remained in the residues, whereas S and O were lost. In contrast to bulk sample measurements of carbonaceous particles using thermal/optical carbon analyzers, our single-particle results imply that many individual organic particles consist of multiple types of organic matter having different thermal stabilities. Our results also suggest that because of their thermal stability, some organic particles may not be detectable by using aerosol mass spectrometry or thermal/optical carbon analyzers. This result can lead to an underestimate of the abundance of TBs and other organic particles, and therefore biomass burning may have a greater influence than is currently recognized in regional and global climate models.

  2. Volume changes upon heating of aerosol particles from biomass burning using transmission electron microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Adachi, Kouji [Meteorological Research Inst., Tsukuba (Japan). Atmospheric Environment and Applied Meteorology Research Dept.; Sedlacek, Arthur J. [Brookhaven National Lab. (BNL), Upton, NY (United States). Environmental and Climate Sciences; Kleinman, Lawrence [Brookhaven National Lab. (BNL), Upton, NY (United States). Environmental and Climate Sciences; Chand, Duli [Pacific Northwest National Lab. (PNNL), Richland, WA (United States). Atmospheric Sciences and Global Change Division; Hubbe, John M. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States). Atmospheric Sciences and Global Change Division; Buseck, Peter R. [Arizona State Univ., Tempe, AZ (United States). School of Earth and Space Exploration and School of Molecular Sciences

    2017-09-26

    The responses of aerosol particles to heating are important for measurements of their chemical, physical, and optical properties, classification, and determination of origin. However, the thermal behavior of organic aerosol particles is largely unknown. We provide a method to analyze such thermal behavior through heating from room temperature to >600°C by using a heating holder within a transmission electron microscope (TEM). Here we describe in-situ shape and size changes and variations in the compositions of individual particles before and after heating. We use ambient samples from wildland and agricultural biomass fires in North America collected during the 2013 Biomass Burn Observation Project (BBOP). The results indicate that individual tar balls (TB; spherical organic material) from biomass burning retained, on average, up to 30% of their volume when heated to 600°C. Chemical analysis reveals that K and Na remain in the residues, whereas S and O were lost. In contrast to bulk sample measurements of carbonaceous particles using thermal/optical carbon analyzers, our single-particle results imply that many individual organic particles consist of multiple types of organic matter having different thermal stabilities. Beyond TBs, our results suggest that because of their thermal stability some organic particles may not be detectable by using aerosol mass spectrometry or thermal/optical carbon analyzers. This result can lead to an underestimate of the abundance of TBs and other organic particles, and therefore biomass burning may have more influence than currently recognized in regional and global climate models.

  3. Atomic imaging using secondary electrons in a scanning transmission electron microscope: experimental observations and possible mechanisms.

    Science.gov (United States)

    Inada, H; Su, D; Egerton, R F; Konno, M; Wu, L; Ciston, J; Wall, J; Zhu, Y

    2011-06-01

    We report detailed investigation of high-resolution imaging using secondary electrons (SE) with a sub-nanometer probe in an aberration-corrected transmission electron microscope, Hitachi HD2700C. This instrument also allows us to acquire the corresponding annular dark-field (ADF) images both simultaneously and separately. We demonstrate that atomic SE imaging is achievable for a wide range of elements, from uranium to carbon. Using the ADF images as a reference, we studied the SE image intensity and contrast as functions of applied bias, atomic number, crystal tilt, and thickness to shed light on the origin of the unexpected ultrahigh resolution in SE imaging. We have also demonstrated that the SE signal is sensitive to the terminating species at a crystal surface. A possible mechanism for atomic-scale SE imaging is proposed. The ability to image both the surface and bulk of a sample at atomic-scale is unprecedented, and can have important applications in the field of electron microscopy and materials characterization. Copyright © 2010 Elsevier B.V. All rights reserved.

  4. Accurate virus quantitation using a Scanning Transmission Electron Microscopy (STEM) detector in a scanning electron microscope.

    Science.gov (United States)

    Blancett, Candace D; Fetterer, David P; Koistinen, Keith A; Morazzani, Elaine M; Monninger, Mitchell K; Piper, Ashley E; Kuehl, Kathleen A; Kearney, Brian J; Norris, Sarah L; Rossi, Cynthia A; Glass, Pamela J; Sun, Mei G

    2017-10-01

    A method for accurate quantitation of virus particles has long been sought, but a perfect method still eludes the scientific community. Electron Microscopy (EM) quantitation is a valuable technique because it provides direct morphology information and counts of all viral particles, whether or not they are infectious. In the past, EM negative stain quantitation methods have been cited as inaccurate, non-reproducible, and with detection limits that were too high to be useful. To improve accuracy and reproducibility, we have developed a method termed Scanning Transmission Electron Microscopy - Virus Quantitation (STEM-VQ), which simplifies sample preparation and uses a high throughput STEM detector in a Scanning Electron Microscope (SEM) coupled with commercially available software. In this paper, we demonstrate STEM-VQ with an alphavirus stock preparation to present the method's accuracy and reproducibility, including a comparison of STEM-VQ to viral plaque assay and the ViroCyt Virus Counter. Copyright © 2017 The Authors. Published by Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

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

    2012-01-01

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

  6. Automated grain mapping using wide angle convergent beam electron diffraction in transmission electron microscope for nanomaterials.

    Science.gov (United States)

    Kumar, Vineet

    2011-12-01

    The grain size statistics, commonly derived from the grain map of a material sample, are important microstructure characteristics that greatly influence its properties. The grain map for nanomaterials is usually obtained manually by visual inspection of the transmission electron microscope (TEM) micrographs because automated methods do not perform satisfactorily. While the visual inspection method provides reliable results, it is a labor intensive process and is often prone to human errors. In this article, an automated grain mapping method is developed using TEM diffraction patterns. The presented method uses wide angle convergent beam diffraction in the TEM. The automated technique was applied on a platinum thin film sample to obtain the grain map and subsequently derive grain size statistics from it. The grain size statistics obtained with the automated method were found in good agreement with the visual inspection method.

  7. Electron energy loss spectroscopy microanalysis and imaging in the transmission electron microscope: example of biological applications

    International Nuclear Information System (INIS)

    Diociaiuti, Marco

    2005-01-01

    This paper reports original results obtained in our laboratory over the past few years in the application of both electron energy loss spectroscopy (EELS) and electron spectroscopy imaging (ESI) to biological samples, performed in two transmission electron microscopes (TEM) equipped with high-resolution electron filters and spectrometers: a Gatan model 607 single magnetic sector double focusing EEL serial spectrometer attached to a Philips 430 TEM and a Zeiss EM902 Energy Filtering TEM. The primary interest was on the possibility offered by the combined application of these spectroscopic techniques with those offered by the TEM. In particular, the electron beam focusing available in a TEM allowed us to perform EELS and ESI on very small sample volumes, where high-resolution imaging and electron diffraction techniques can provide important structural information. I show that ESI was able to improve TEM performance, due to the reduced chromatic aberration and the possibility of avoiding the sample staining procedure. Finally, the analysis of the oscillating extended energy loss fine structure (EXELFS) beyond the ionization edges characterizing the EELS spectra allowed me, in a manner very similar to the extended X-ray absorption fine structure (EXAFS) analysis of the X-ray absorption spectra, to obtain short-range structural information for such light elements of biological interest as O or Fe. The Philips EM430 (250-300 keV) TEM was used to perform EELS microanalysis on Ca, P, O, Fe, Al and Si. The assessment of the detection limits of this method was obtained working with well-characterized samples containing Ca and P, and mimicking the actual cellular matrix. I applied EELS microanalysis to Ca detection in bone tissue during the mineralization process and to P detection in the cellular membrane of erythrocytes treated with an anti-tumoral drug, demonstrating that the cellular membrane is a drug target. I applied EELS microanalysis and selected area electron

  8. Literature survey: Relations between stress change, deformation and transmissivity for fractures and deformation zones based on in situ investigations

    Energy Technology Data Exchange (ETDEWEB)

    Fransson, Aasa (Chalmers Univ. of Technology, Goeteborg (Sweden))

    2009-02-15

    This literature survey is focused upon relations between stress change, deformation and transmissivity for fractures and deformation zones and aims at compiling and commenting on relevant information and references with focus on data from in situ investigations. Main issues to investigate are: - Impact of normal stress change and deformation on transmissivity, for fractures and deformation zones. - Impact of shear stress and displacement on transmissivity, for fractures and deformation zones for different normal load conditions. Considering the line of research within the area, the following steps in the development can be identified. During the 1970's and 1980's, the fundamentals of rock joint deformation were investigated and identification and description of mechanisms were made in the laboratory. In the 1990's, coupling of stress-flow properties of rock joints were made using hydraulic testing to identify and describe the mechanisms in the field. Both individual fractures and deformation zones were of interest. In situ investigations have also been the topic of interest the last ten years. Further identification and description of mechanisms in the field have been made including investigation and description of system of fractures, different types of fractures (interlocked/mated or mismatched/unmated) and how this is coupled to the hydromechanical behavior. In this report, data from in situ investigations are compiled and the parameters considered to be important to link fracture deformation and transmissivity are normal stiffness, k{sub n} and hydraulic aperture, b{sub h}. All data except for those from one site originate from investigations performed in granitic rock. Normal stiffness, k{sub n}, and hydraulic aperture, b{sub h}, are correlated, even though data are scattered. In general, the largest variation is seen for small hydraulic apertures and high normal stiffness. The increasing number of contact points (areas) and fracture filling are

  9. Design of electron wave filters in monolayer graphene by tunable transmission gap

    OpenAIRE

    Chen, Xi; Tao, Jia-Wei

    2009-01-01

    We have investigated the transmission in monolayer graphene barrier at nonzero angle of incidence. Taking the influence of parallel wave vector into account, the transmission as the function of incidence energy has a gap due to the evanescent waves in two cases of Klein tunneling and classical motion. The modulation of the transmission gap by the incidence angle, the height, and width of potential barrier may lead to potential applications in graphene-based electronic devices.

  10. Aberration corrected and monochromated environmental transmission electron microscopy: challenges and prospects for materials science

    DEFF Research Database (Denmark)

    Hansen, Thomas Willum; Wagner, Jakob Birkedal; Dunin-Borkowski, Rafal E.

    2010-01-01

    The latest generation of environmental transmission electron microscopes incorporates aberration correctors and monochromators, allowing studies of chemical reactions and growth processes with improved spatial resolution and spectral sensitivity. Here, we describe the performance of such an instr...

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

    DEFF Research Database (Denmark)

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

    2006-01-01

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

  12. INVIVO DEGRADATION OF PROCESSED DERMAL SHEEP COLLAGEN EVALUATED WITH TRANSMISSION ELECTRON-MICROSCOPY

    NARCIS (Netherlands)

    VANWACHEM, PB; VANLUYN, MJA; NIEUWENHUIS, P; KOERTEN, HK; DAMINK, LO; TENHOOPEN, H; FEIJEN, J

    The in vivo degradation of hexamethylenediisocyanate-tanned dermal sheep collagen was studied with transmission electron microscopy. Discs of hexamethylenediisocyanate-tanned dermal sheep collagen were subcutaneously implanted in rats. Both an intra- and an extracellular route of degradation could

  13. In vivo degradation of processed dermal sheep collagen evaluated with transmission electron microscopy

    NARCIS (Netherlands)

    van Wachem, P.B.; van Luyn, M.J.A.; Nieuwenhuis, P.; Koerten, H.K.; Olde damink, L.H.H.; Olde-Damink, L.; ten Hoopen, Hermina W.M.; Feijen, Jan

    1991-01-01

    The in vivo degradation of hexamethylenediisocyanate-tanned dermal sheep collagen was studied with transmission electron microscopy. Discs of hexamethylenediisocyanate-tanned dermal sheep collagen were subcutaneously implanted in rats. Both an intra- and an extracellular route of degradation could

  14. Cryo-transmission electron microscopy of Ag nanoparticles grown on an ionic liquid substrate

    KAUST Repository

    Anjum, Dalaver H.; Stiger, Rebecca M.; Finley, James J.; Conway, James F.

    2010-01-01

    We report a novel method of growing silver nanostructures by cathodic sputtering onto an ionic liquid (IL) and our visualization by transmission cryo-electron microscopy to avoid beam-induced motion of the nanoparticles. By freezing the IL

  15. Diffraction contrast as a sensitive indicator of femtosecond sub-nanoscale motion in ultrafast transmission electron microscopy

    Science.gov (United States)

    Cremons, Daniel R.; Schliep, Karl B.; Flannigan, David J.

    2013-09-01

    With ultrafast transmission electron microscopy (UTEM), access can be gained to the spatiotemporal scales required to directly visualize rapid, non-equilibrium structural dynamics of materials. This is achieved by operating a transmission electron microscope (TEM) in a stroboscopic pump-probe fashion by photoelectrically generating coherent, well-timed electron packets in the gun region of the TEM. These probe photoelectrons are accelerated down the TEM column where they travel through the specimen before reaching a standard, commercially-available CCD detector. A second laser pulse is used to excite (pump) the specimen in situ. Structural changes are visualized by varying the arrival time of the pump laser pulse relative to the probe electron packet at the specimen. Here, we discuss how ultrafast nanoscale motions of crystalline materials can be visualized and precisely quantified using diffraction contrast in UTEM. Because diffraction contrast sensitively depends upon both crystal lattice orientation as well as incoming electron wavevector, minor spatial/directional variations in either will produce dynamic and often complex patterns in real-space images. This is because sections of the crystalline material that satisfy the Laue conditions may be heterogeneously distributed such that electron scattering vectors vary over nanoscale regions. Thus, minor changes in either crystal grain orientation, as occurs during specimen tilting, warping, or anisotropic expansion, or in the electron wavevector result in dramatic changes in the observed diffraction contrast. In this way, dynamic contrast patterns observed in UTEM images can be used as sensitive indicators of ultrafast specimen motion. Further, these motions can be spatiotemporally mapped such that direction and amplitude can be determined.

  16. Origin of spin-dependent asymmetries in electron transmission through ultrathin ferromagnetic films

    International Nuclear Information System (INIS)

    Gokhale, M.P.; Mills, D.L.

    1991-01-01

    We present theoretical calculations of exchange asymmetries in the transmission of electrons through ultrathin films of ferromagnetic Fe. The results account nicely for the magnitude of the asymmetries observed by Pappas et al. in photoemission studies of Cu covered by an ultrathin film of Fe. We argue that exchange asymmetry in the transmissivity of the Fe film, rather than the spin dependence of the electron mean free path, is responsible for the effects reported by these authors

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

    International Nuclear Information System (INIS)

    Kashchieva, E.P.

    1997-01-01

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

  18. Transmission Electron Microscopy Studies of Electron-Selective Titanium Oxide Contacts in Silicon Solar Cells

    KAUST Repository

    Ali, Haider

    2017-08-15

    In this study, the cross-section of electron-selective titanium oxide (TiO2) contacts for n-type crystalline silicon solar cells were investigated by transmission electron microscopy. It was revealed that the excellent cell efficiency of 21.6% obtained on n-type cells, featuring SiO2/TiO2/Al rear contacts and after forming gas annealing (FGA) at 350°C, is due to strong surface passivation of SiO2/TiO2 stack as well as low contact resistivity at the Si/SiO2/TiO2 heterojunction. This can be attributed to the transformation of amorphous TiO2 to a conducting TiO2-x phase. Conversely, the low efficiency (9.8%) obtained on cells featuring an a-Si:H/TiO2/Al rear contact is due to severe degradation of passivation of the a-Si:H upon FGA.

  19. Angstrom analysis with dynamic in-situ aberration corrected electron microscopy

    International Nuclear Information System (INIS)

    Gai, P L; Boyes, E D

    2010-01-01

    Following the pioneering development of atomic resolution in-situ environmental TEM (ETEM) for direct probing of gas-solid reactions, recent developments are presented of dynamic real time in-situ studies at the Angstrom level in an aberration corrected electron microscope. The in-situ data from Pt-Pd nanoparticles on carbon with the corresponding FFT/optical diffractogram (OD) illustrate an achieved resolution of 0 C and higher, in a double aberration corrected JEOL 2200 FS TEM/STEM employing a wider gap objective pole piece and gas tolerant TMP column pumping system. Direct observations of dynamic biofuel catalysts under controlled calcinations conditions and quantified with catalytic reactivity and physico-chemical studies show the benefits in-situ aberration correction in unveiling the evolution of surface active sites necessary for the development efficient heterogeneous catalysts. The new results open up opportunities for dynamic studies of materials in an aberration corrected environment and direct future development activities.

  20. In situ electron-beam polymerization stabilized quantum dot micelles.

    Science.gov (United States)

    Travert-Branger, Nathalie; Dubois, Fabien; Renault, Jean-Philippe; Pin, Serge; Mahler, Benoit; Gravel, Edmond; Dubertret, Benoit; Doris, Eric

    2011-04-19

    A polymerizable amphiphile polymer containing PEG was synthesized and used to encapsulate quantum dots in micelles. The quantum dot micelles were then polymerized using a "clean" electron beam process that did not require any post-irradiation purification. Fluorescence spectroscopy revealed that the polymerized micelles provided an organic coating that preserved the quantum dot fluorescence better than nonpolymerized micelles, even under harsh conditions. © 2011 American Chemical Society

  1. A Novel Two-Axis Load Sensor Designed for in Situ Scratch Testing inside Scanning Electron Microscopes

    Directory of Open Access Journals (Sweden)

    Chengli Shi

    2013-02-01

    Full Text Available Because of a lack of available miniaturized multiaxial load sensors to measure the normal load and the lateral load simultaneously, quantitative in situ scratch devices inside scanning electron microscopes and the transmission electron microscopes have barely been developed up to now. A novel two-axis load sensor was designed in this paper. With an I-shaped structure, the sensor has the function of measuring the lateral load and the normal load simultaneously, and at the same time it has compact dimensions. Finite element simulations were carried out to evaluate stiffness and modal characteristics. A decoupling algorithm was proposed to resolve the cross-coupling between the two-axis loads. Natural frequency of the sensor was tested. Linearity and decoupling parameters were obtained from the calibration experiments, which indicate that the sensor has good linearity and the cross-coupling between the two axes is not strong. Via the decoupling algorithm and the corresponding decoupling parameters, simultaneous measurement of the lateral load and the normal load can be realized via the developed two-axis load sensor. Preliminary applications of the load sensor for scratch testing indicate that the load sensor can work well during the scratch testing. Taking advantage of the compact structure, it has the potential ability for applications in quantitative in situ scratch testing inside SEMs.

  2. In-situ measurements of the secondary electron yield in an accelerator environment: Instrumentation and methods

    International Nuclear Information System (INIS)

    Hartung, W.H.; Asner, D.M.; Conway, J.V.; Dennett, C.A.; Greenwald, S.; Kim, J.-S.; Li, Y.; Moore, T.P.; Omanovic, V.; Palmer, M.A.; Strohman, C.R.

    2015-01-01

    The performance of a particle accelerator can be limited by the build-up of an electron cloud (EC) in the vacuum chamber. Secondary electron emission from the chamber walls can contribute to EC growth. An apparatus for in-situ measurements of the secondary electron yield (SEY) in the Cornell Electron Storage Ring (CESR) was developed in connection with EC studies for the CESR Test Accelerator program. The CESR in-situ system, in operation since 2010, allows for SEY measurements as a function of incident electron energy and angle on samples that are exposed to the accelerator environment, typically 5.3 GeV counter-rotating beams of electrons and positrons. The system was designed for periodic measurements to observe beam conditioning of the SEY with discrimination between exposure to direct photons from synchrotron radiation versus scattered photons and cloud electrons. The samples can be exchanged without venting the CESR vacuum chamber. Measurements have been done on metal surfaces and EC-mitigation coatings. The in-situ SEY apparatus and improvements to the measurement tools and techniques are described

  3. In-situ measurements of the secondary electron yield in an accelerator environment: Instrumentation and methods

    Energy Technology Data Exchange (ETDEWEB)

    Hartung, W.H., E-mail: wh29@cornell.edu; Asner, D.M.; Conway, J.V.; Dennett, C.A.; Greenwald, S.; Kim, J.-S.; Li, Y.; Moore, T.P.; Omanovic, V.; Palmer, M.A.; Strohman, C.R.

    2015-05-21

    The performance of a particle accelerator can be limited by the build-up of an electron cloud (EC) in the vacuum chamber. Secondary electron emission from the chamber walls can contribute to EC growth. An apparatus for in-situ measurements of the secondary electron yield (SEY) in the Cornell Electron Storage Ring (CESR) was developed in connection with EC studies for the CESR Test Accelerator program. The CESR in-situ system, in operation since 2010, allows for SEY measurements as a function of incident electron energy and angle on samples that are exposed to the accelerator environment, typically 5.3 GeV counter-rotating beams of electrons and positrons. The system was designed for periodic measurements to observe beam conditioning of the SEY with discrimination between exposure to direct photons from synchrotron radiation versus scattered photons and cloud electrons. The samples can be exchanged without venting the CESR vacuum chamber. Measurements have been done on metal surfaces and EC-mitigation coatings. The in-situ SEY apparatus and improvements to the measurement tools and techniques are described.

  4. The effect of different electrodes on the electronic transmission of benzene junctions: Analytical approach

    Energy Technology Data Exchange (ETDEWEB)

    Mohebbi, Razie; Seyed-Yazdi, Jamileh, E-mail: j.seyedyazdi@vru.ac.ir

    2016-06-01

    In this paper we have investigated the electronic transmission of systems electrode–benzene–electrode using the Landauer approach. The effect of different electrodes made of metal (Au) and semiconductors (Si, TiO{sub 2}) is investigated. These three electrodes are compared between them and the results show that the electronic transmission of benzene junctions, when using semiconductor electrodes, is associated to a gap in transmission which is due to the electrodes band gap. As a consequence, a threshold voltage is necessary to obtain conducting channels.

  5. In-situ synthesis of Ag nanoparticles by electron beam irradiation

    International Nuclear Information System (INIS)

    Gong, Jiangfeng; Liu, Hongwei; Jiang, Yuwen; Yang, Shaoguang; Liao, Xiaozhou; Liu, Zongwen; Ringer, Simon

    2015-01-01

    Ag nanoparticles were synthesized by electron beam irradiation in the transmission electron microscope chamber at room temperature and the growth mechanism was explored in detail. The sizes of the Ag nanoparticles are controlled by the electron beam current density. Two nanoparticle growth stages were identified. The first growth stage was dominated by the discharging effect, while the second stage was controlled by the heating effect. The nanoparticle synthesis method should be applicable to the synthesis of other metallic nanoparticles. - Highlights: • Ag nanoparticles were synthesized by electron beam irradiation in the transmission electron microscope chamber. • The sizes of the Ag nanoparticles are controlled by the electron beam current density. • The growth mechanism was studied, two growth stages were confirmed. • The first growth stage was dominated by the discharging effect, and the second stage was controlled by the heating effect.

  6. An electromechanical material testing system for in situ electron microscopy and applications

    OpenAIRE

    Zhu, Yong; Espinosa, Horacio D.

    2005-01-01

    We report the development of a material testing system for in situ electron microscopy (EM) mechanical testing of nanostructures. The testing system consists of an actuator and a load sensor fabricated by means of surface micromachining. This previously undescribed nanoscale material testing system makes possible continuous observation of the specimen deformation and failure with subnanometer resolution, while simultaneously measuring the applied load electronically with nanonewton resolution...

  7. Submolecular Electronic Mapping of Single Cysteine Molecules by in Situ Scanning Tunneling Imaging

    DEFF Research Database (Denmark)

    Zhang, Jingdong; Chi, Qijin; Nazmutdinov, R. R.

    2009-01-01

    We have used L-Cysteine (Cys) as a model system to study the surface electronic structures of single molecules at the submolecular level in aqueous buffer solution by a combination of electrochemical scanning tunneling microscopy (in situ STM), electrochemistry including voltammetry and chronocou...

  8. In-situ observations of point-defect precipitation at dislocations in electron-irradiated silver

    International Nuclear Information System (INIS)

    Jenkins, M.L.; Hardy, G.J.; Kirk, M.A.

    1986-09-01

    In-situ weak-beam observations of the development of electron irradiation damage at dislocations in silver are described. Dislocations constrict and promote in their vicinity the formation of stacking-fault tetrahedra. The possibility that these are of interstitial nature is discussed

  9. In Situ Study of Live Specimens in an Environmental Scanning Electron Microscope

    Czech Academy of Sciences Publication Activity Database

    Tihlaříková, Eva; Neděla, Vilém; Shiojiri, M.

    2013-01-01

    Roč. 19, č. 4 (2013), s. 914-918 ISSN 1431-9276 R&D Projects: GA ČR GAP102/10/1410 Institutional support: RVO:68081731 Keywords : live biological sample * high-pressure environment * hydration system * in situ observation * Monte Carlo simulation * methodology Subject RIV: JA - Electronics ; Optoelectronics, Electrical Engineering Impact factor: 1.757, year: 2013

  10. Free electron lasers for transmission of energy in space

    Science.gov (United States)

    Segall, S. B.; Hiddleston, H. R.; Catella, G. C.

    1981-01-01

    A one-dimensional resonant-particle model of a free electron laser (FEL) is used to calculate laser gain and conversion efficiency of electron energy to photon energy. The optical beam profile for a resonant optical cavity is included in the model as an axial variation of laser intensity. The electron beam profile is matched to the optical beam profile and modeled as an axial variation of current density. Effective energy spread due to beam emittance is included. Accelerators appropriate for a space-based FEL oscillator are reviewed. Constraints on the concentric optical resonator and on systems required for space operation are described. An example is given of a space-based FEL that would produce 1.7 MW of average output power at 0.5 micrometer wavelength with over 50% conversion efficiency of electrical energy to laser energy. It would utilize a 10 m-long amplifier centered in a 200 m-long optical cavity. A 3-amp, 65 meV electrostatic accelerator would provide the electron beam and recover the beam after it passes through the amplifier. Three to five shuttle flights would be needed to place the laser in orbit.

  11. Removal of Vesicle Structures from Transmission Electron Microscope Images

    DEFF Research Database (Denmark)

    Jensen, Katrine Hommelhoff; Sigworth, Fred; Brandt, Sami Sebastian

    2015-01-01

    In this paper, we address the problem of imaging membrane proteins for single-particle cryo-electron microscopy reconstruction of the isolated protein structure. More precisely, we propose a method for learning and removing the interfering vesicle signals from the micrograph, prior to reconstruct...

  12. Small round structured viruses (SRSVs) and transmission electron ...

    African Journals Online (AJOL)

    Administrator

    immune-electron microscopy (IEM) from patients' feces. They reported this virus particle as the causative agent of winter vomiting outbreaks in Norwalk (Kapikian et al.,. 1972). This is the remarkable landmark study of non- bacterial gastroenteritis viruses, especially for small round structured viruses (SRSVs). After that, many.

  13. In situ ion etching in a scanning electron microscope

    International Nuclear Information System (INIS)

    Dhariwal, R.S.; Fitch, R.K.

    1977-01-01

    A facility for ion etching in a scanning electron microscope is described which incorporates a new type of electrostatic ion source and viewing of the specimen is possible within about 30 sec after terminating the ion bombardment. Artefacts produced during etching have been studied and cone formation has been followed during its growth. The instrument has provided useful structural information on metals, alloys, and sinters. However, although insulating materials, such as plastics, glass and resins, have been successfully etched, interpretation of the resultant micrographs is more difficult. Ion etching of soft biological tissues, such as the rat duodenum was found to be of considerable interest. The observed structural features arise from the selective intake of the heavy fixation elements by different parts of the tissue. Hard biological materials, such as dental tissues and restorative materials, have also been studied and the prismatic structure of the enamel and the form and distribution of the dentinal tubules have been revealed. (author)

  14. Transmission electron microscopy study of unhydrided,dehydrided and annealed LaNi5

    NARCIS (Netherlands)

    Veirman, de A.E.M.; Staals, A.A.; Notten, P.H.L.

    1994-01-01

    The influence of hydrogen absorption on the microstructure of LaNi5 powders has been investigated by transmission electron microscopy. At the surface of the unhydrided and dehydrided LaNi5 grains a reaction layer is observed. By means of selected area electron diffraction this layer is found to

  15. Charging of carbon thin films in scanning and phase-plate transmission electron microscopy

    DEFF Research Database (Denmark)

    Hettler, Simon; Kano, Emi; Dries, Manuel

    2018-01-01

    A systematic study on charging of carbon thin films under intense electron-beam irradiation was performed in a transmission electron microscope to identify the underlying physics for the functionality of hole-free phase plates. Thin amorphous carbon films fabricated by different deposition techni...

  16. Direct observations of the MOF (UiO-66) structure by transmission electron microscopy

    KAUST Repository

    Zhu, Liangkui

    2013-01-01

    As a demonstration of ab initio structure characterizations of nano metal organic framework (MOF) crystals by high resolution transmission electron microscopy (HRTEM) and electron diffraction tomography methods, a Zr-MOF (UiO-66) structure was determined and further confirmed by Rietveld refinements of powder X-ray diffraction. HRTEM gave direct imaging of the channels. © 2013 The Royal Society of Chemistry.

  17. Analysis of intermetallic particles in Mg-12 wt.%Zn binyry alloy using transmission electron microscopy

    Czech Academy of Sciences Publication Activity Database

    Němec, Martin; Gärtnerová, Viera; Klementová, Mariana; Jäger, Aleš

    2015-01-01

    Roč. 106, Aug (2015), s. 428-436 ISSN 1044-5803 R&D Projects: GA ČR GBP108/12/G043 Institutional support: RVO:68378271 Keywords : biomedical alloy s * heat treatment * microstructure * transmission electron microscopy * electron diffraction Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 2.383, year: 2015

  18. The Design and Construction of a Simple Transmission Electron Microscope for Educational Purposes.

    Science.gov (United States)

    Hearsey, Paul K.

    This document presents a model for a simple transmission electron microscope for educational purposes. This microscope could demonstrate thermonic emission, particle acceleration, electron deflection, and flourescence. It is designed to be used in high school science courses, particularly physics, taking into account the size, weight, complexity…

  19. In situ observation of low temperature growth of Ge on Si(1 1 1) by reflection high energy electron diffraction

    International Nuclear Information System (INIS)

    Grimm, Andreas; Fissel, Andreas; Bugiel, Eberhard; Wietler, Tobias F.

    2016-01-01

    Highlights: • Investigation of the initial stages of epitaxial growth of Ge on Si(1 1 1) in situ by RHEED. • Impact of growth temperature on strain evolution for temperatures between 200 °C and 400 °C. • Epitaxy with a high degree of structural perfection already at growth temperature of 200 °C. • Ordered interfacial dislocation networks already at 200 °C. • Tensile strain contribution of Si(1 1 1) 7 × 7-surface reconstruction to strain relaxation process for epitaxial growth of Ge. - Abstract: In this paper we investigate the initial stages of epitaxial growth of Ge on Si(1 1 1) and the impact of growth temperature on strain evolution in situ by reflection high energy electron diffraction (RHEED) for temperatures between 200 °C and 400 °C. The change in surface morphology from a flat wetting layer to subsequent islanding that is characteristic for Stranski–Krastanov growth is monitored by spot intensity analysis. The corresponding critical layer thickness is determined to 3.1 < d c < 3.4 ML. In situ monitoring of the strain relaxation process reveals a contribution of the Si(1 1 1) 7 × 7-surface reconstruction to the strain relaxation process. High resolution transmission electron microscopy confirms that the Ge islands exhibit a high degree of structural perfection and an ordered interfacial misfit dislocation network already at a growth temperature of 200 °C is established. The temperature dependency of island shape, density and height is characterized by atomic force microscopy and compared to the RHEED investigations.

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

    Science.gov (United States)

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

    2017-08-15

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

  1. First transmission of electrons and ions through the KATRIN beamline

    Czech Academy of Sciences Publication Activity Database

    Arenz, M.; Dragoun, Otokar; Kovalík, Alojz; Lebeda, Ondřej; Ryšavý, Miloš; Sentkerestiová, Jana; Suchopár, Martin; Vénos, Drahoslav

    2018-01-01

    Roč. 13, č. 4 (2018), č. článku P04020. ISSN 1748-0221 R&D Projects: GA MŠk LM2015056; GA MŠk LTT18021 Institutional support: RVO:61389005 Keywords : ion sources * electron beam * detector control systems * beam-line instrumentation * spectrometers Subject RIV: BG - Nuclear, Atomic and Molecular Physics, Colliders OBOR OECD: Nuclear physics Impact factor: 1.220, year: 2016

  2. Transmission of electrons with flat passbands in finite superlattices

    International Nuclear Information System (INIS)

    Barajas-Aguilar, A H; Rodríguez-Magdaleno, K A; Martínez-Orozco, J C; Enciso-Muñoz, A; Contreras-Solorio, D A

    2013-01-01

    Using the transfer matrix method and the Ben Daniel-Duke equation for variable mass electrons propagation, we calculate the transmittance for symmetric finite superlattices where the width and the height of the potential barriers follow a linear dependence. The width and height of the barriers decreases from the center to the ends of the superlattice. The transmittance presents intervals of stopbands and quite flat passbands.

  3. Robust image alignment for cryogenic transmission electron microscopy.

    Science.gov (United States)

    McLeod, Robert A; Kowal, Julia; Ringler, Philippe; Stahlberg, Henning

    2017-03-01

    Cryo-electron microscopy recently experienced great improvements in structure resolution due to direct electron detectors with improved contrast and fast read-out leading to single electron counting. High frames rates enabled dose fractionation, where a long exposure is broken into a movie, permitting specimen drift to be registered and corrected. The typical approach for image registration, with high shot noise and low contrast, is multi-reference (MR) cross-correlation. Here we present the software package Zorro, which provides robust drift correction for dose fractionation by use of an intensity-normalized cross-correlation and logistic noise model to weight each cross-correlation in the MR model and filter each cross-correlation optimally. Frames are reliably registered by Zorro with low dose and defocus. Methods to evaluate performance are presented, by use of independently-evaluated even- and odd-frame stacks by trajectory comparison and Fourier ring correlation. Alignment of tiled sub-frames is also introduced, and demonstrated on an example dataset. Zorro source code is available at github.com/CINA/zorro. Copyright © 2016 Elsevier Inc. All rights reserved.

  4. The influence of Cs/Cc correction in analytical imaging and spectroscopy in scanning and transmission electron microscopy

    International Nuclear Information System (INIS)

    Zaluzec, Nestor J.

    2015-01-01

    Aberration correction in scanning/transmission electron microscopy (S/TEM) owes much to the efforts of a small dedicated group of innovators. Leading that frontier has been Prof. Harald Rose. To date his leadership and dynamic personality has spearheaded our ability to leave behind many of the limitations imposed by spherical aberration (C s ) in high resolution phase contrast imaging. Following shortly behind, has been the development of chromatic aberration correction (C c ) which augments those accomplishments. In this paper we will review and summarize how the combination of C s /C c technology enhances our ability to conduct hyperspectral imaging and spectroscopy in today's and future computationally mediated experiments in both thin as well as realistic specimens in vacuo and during in-situ/environmental experiments

  5. Applications of transmission electron microscopy in the materials and mineral sciences

    International Nuclear Information System (INIS)

    Murr, L.E.

    1975-01-01

    Unique capabilities of transmission electron microscopy in characterizing the structure and properties of metals, minerals, and other crystaline materials are illustrated and compared with observations in the scanning electron and field-ion microscopes. Contrast mechanisms involving both mass-thickness and diffraction processes are illustrated, and examples presented of applications of bright and dark-field techiques. Applications of the electron microscope in the investigation of metallurgical and mineralogical problems are outlined with representative examples [pt

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

    DEFF Research Database (Denmark)

    Canepa, Silvia

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

  7. Big Data Analytics for Scanning Transmission Electron Microscopy Ptychography

    Science.gov (United States)

    Jesse, S.; Chi, M.; Belianinov, A.; Beekman, C.; Kalinin, S. V.; Borisevich, A. Y.; Lupini, A. R.

    2016-05-01

    Electron microscopy is undergoing a transition; from the model of producing only a few micrographs, through the current state where many images and spectra can be digitally recorded, to a new mode where very large volumes of data (movies, ptychographic and multi-dimensional series) can be rapidly obtained. Here, we discuss the application of so-called “big-data” methods to high dimensional microscopy data, using unsupervised multivariate statistical techniques, in order to explore salient image features in a specific example of BiFeO3 domains. Remarkably, k-means clustering reveals domain differentiation despite the fact that the algorithm is purely statistical in nature and does not require any prior information regarding the material, any coexisting phases, or any differentiating structures. While this is a somewhat trivial case, this example signifies the extraction of useful physical and structural information without any prior bias regarding the sample or the instrumental modality. Further interpretation of these types of results may still require human intervention. However, the open nature of this algorithm and its wide availability, enable broad collaborations and exploratory work necessary to enable efficient data analysis in electron microscopy.

  8. Electronic control of a 4-speed automatic transmission with lock-up clutch

    Energy Technology Data Exchange (ETDEWEB)

    Schwab, M.

    1984-01-01

    The paper describes the electronic control of an automatic 4-speed transmission with lock-up clutch. As compared to purely hydraulically controlled transmissions, this control offers a clearly improved quality of shifting and the possibility of achieving improvements in fuel consumption thanks to a special economy program. The electronic control unit is a Bosch MOTRONIC which has been expanded to include the functions of transmission control. A special feature is the engine torque control which is implemented by way of retarding the ignition when shifting. This opens up an additional degree of freedom for optimizing a transmission in terms of shift comfort, life of the friction elements and the power which can be transmitted.

  9. Electron cyclotron waves transmission: new approach for the characterization of electron distribution functions in Tokamak hot plasmas

    International Nuclear Information System (INIS)

    Michelot, Y.

    1995-10-01

    Fast electrons are one of the basic ingredients of plasma operations in many existing thermonuclear fusion research devices. However, the understanding of fast electrons dynamics during creation and sustainment of the superthermal electrons tail is far for being satisfactory. For this reason, the Electron Cyclotron Transmission (ECT) diagnostic was implemented on Tore Supra tokamak. It consists on a microwave transmission system installed on a vertical chord crossing the plasma center and working in the frequency range 77-109 GHz. Variations of the wave amplitude during the propagation across the plasma may be due to refraction and resonant absorption. For the ECT, the most common manifestation of refraction is a reduction of the received power density with respect to the signal detected in vacuum, due to the spreading and deflection of the wave beam. Wave absorption is observed in the vicinity of the electron cyclotron harmonics and may be due both to thermal plasma and to superthermal electron tails. It has a characteristic frequency dependence due to the relativistic mass variation in the wave-electron resonance condition. This thesis presents the first measurements of: the extraordinary mode optical depth at the third harmonics, the electron temperature from the width of a cyclotron absorption line and the relaxation times of the electron distribution during lower hybrid current drive from the ordinary mode spectral superthermal absorption line at the first harmonic. (J.S.). 175 refs., 110 figs., 9 tabs., 3 annexes

  10. A novel and compact nanoindentation device for in situ nanoindentation tests inside the scanning electron microscope

    Directory of Open Access Journals (Sweden)

    Hu Huang

    2012-03-01

    Full Text Available In situ nanomechanical tests provide a unique insight into mechanical behaviors of materials, such as fracture onset and crack propagation, shear band formation and so on. This paper presents a novel in situ nanoindentation device with dimensions of 103mm×74mm×60mm. Integrating the stepper motor, the piezoelectric actuator and the flexure hinge, the device can realize coarse adjustment of the specimen and precision loading and unloading of the indenter automatically. A novel indenter holder was designed to guarantee that the indenter penetrates into and withdraws from the specimen surface vertically. Closed-loop control of the indentation process was established to solve the problem of nonlinearity of the piezoelectric actuator and to enrich the loading modes. The in situ indentation test of Indium Phosphide (InP inside the scanning electron microscope (SEM was carried out and the experimental result indicates the feasibility of the developed device.

  11. Batteryless wireless transmission system for electronic drum uses piezoelectric generator for play signal and power source

    International Nuclear Information System (INIS)

    Nishikawa, H; Yoshimi, A; Takemura, K; Tanaka, A; Douseki, T

    2015-01-01

    A batteryless self-powered wireless transmission system has been developed that sends a signal from a drum pad to a synthesizer. The power generated by a piezoelectric generator functions both as the “Play” signal for the synthesizer and as the power source for the transmitter. An FM transmitter, which theoretically operates with zero latency, and a receiver with quick-response squelch of the received signal were developed for wireless transmission with a minimum system delay. Experimental results for an electronic drum without any connecting wires fully demonstrated the feasibility of self-powered wireless transmission with a latency of 900 μs. (paper)

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

    NARCIS (Netherlands)

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

    2003-01-01

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

  13. Scanning and Transmission Electron Microscopy of High Temperature Materials

    Science.gov (United States)

    1994-01-01

    Software and hardware updates to further extend the capability of the electron microscope were carried out. A range of materials such as intermetallics, metal-matrix composites, ceramic-matrix composites, ceramics and intermetallic compounds, based on refractory elements were examined under this research. Crystal structure, size, shape and volume fraction distribution of various phases which constitute the microstructures were examined. Deformed materials were studied to understand the effect of interfacial microstructure on the deformation and fracture behavior of these materials. Specimens tested for a range of mechanical property requirements, such as stress rupture, creep, low cycle fatigue, high cycle fatigue, thermomechanical fatigue, etc. were examined. Microstructural and microchemical stability of these materials exposed to simulated operating environments were investigated. The EOIM Shuttle post-flight samples were also examined to understand the influence of low gravity processing on microstructure. In addition, fractographic analyses of Nb-Zr-W, titanium aluminide, molybdenum silicide and silicon carbide samples were carried out. Extensive characterization of sapphire fibers in the fiber-reinforced composites made by powder cloth processing was made. Finally, pressure infiltration casting of metal-matrix composites was carried out.

  14. Transmission Electron Microscopy of Bombyx Mori Silk Fibers

    Science.gov (United States)

    Shen, Y.; Martin, D. C.

    1997-03-01

    The microstructure of B. Mori silk fibers before and after degumming was examined by TEM, selected area electron diffraction (SAED), WAXS and low voltage SEM. SEM micrographs of the neat cocoon revealed a network of pairs of twisting filaments. After degumming, there were only individual filaments showing a surface texture consistent with an oriented fibrillar structure in the fiber interior. WAXS patterns confirmed the oriented beta-sheet crystal structure common to silkworm and spider silks. Low dose SAED results were fully consistent with the WAXS data, and revealed that the crystallographic texture did not vary significantly across the fiber diameter. TEM observations of microtomed fiber cross sections indicated a somewhat irregular shape, and also revealed a 0.5-2 micron sericin coating which was removed by the degumming process. TEM observations of the degummed silk fiber showed banded features with a characteristic spacing of nominally 600 nm along the fiber axis. These bands were oriented in a roughly parabolic or V-shape pointing along one axis within a given fiber. We hypothesize that this orientation is induced by the extrusion during the spinning process. Equatorial DF images revealed that axial and lateral sizes of the β-sheet crystallites in silk fibroin ranged from 20 to 170 nm and from 1 to 24 nm, respectively. Crazes developed in the degummed silk fiber parallel to the fiber direction. The formation of these crazes suggests that there are significant lateral interactions between fibrils in silk fibers.

  15. Transmission properties of Dirac electrons through Cantor monolayer graphene superlattices

    Directory of Open Access Journals (Sweden)

    R. Rodríguez-González

    2014-01-01

    Full Text Available En este trabajo usamos el método de la matriz de transferencia para estudiar el tunelamiento de los electrones de Dirac a través de superredes aperiodicas en grafeno. Consideramos una hoja de grafeno depositada encima de bloques de sustratos de Óxido de Silicio (SiO2 y Carburo de Silicio (SiC, en los cuales aplicamos la serie de Cantor. Calculamos la transmitancia para diferentes parámetros fundamentales tales como: ancho de partida, energía de incidencia, ángulo de incidencia y número de generación de la serie de Cantor. En este caso, la transmitancia como función de la energía presenta rasgos autosimilares al variar el número de generación. También computamos la distribución angular de la transmitancia para energías fijas econtrando un patrón autosimilar entre generaciones. Por último, calculamos los factores de escala para algunos espectros de la transmitancia, los cuales efectivamente muestran escalabilidad.

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

    Directory of Open Access Journals (Sweden)

    Liron Issman

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

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

    Science.gov (United States)

    Culnane, Lance F.

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

  18. High definition in-situ electro-optical characterization for Roll to Roll printed electronics

    DEFF Research Database (Denmark)

    Pastorelli, Francesco

    2017-01-01

    Resume: Printed electronics is emerging as a new, large scale and cost effective technology that will be disruptive in fields such as energy harvesting, consumer electronics and medical sensors. The performance of printed organic electronic devices relies principally on the carrier mobility...... and molecular packing of the polymer semiconductor material. Unfortunately, the analysis of such materials is generally performed with destructive techniques, which are hard to make compatible with in situ measurements, and pose a great obstacle for the mass production of printed electronics devices. A rapid......-photon induced photoluminescence (TPPL) and second harmonic response. We anticipate that this non-linear optical method will substantially contribute to the understanding of printed electronic devices and demonstrate it as a promising novel tool for non-destructive and facile testing of materials during printing...

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

    International Nuclear Information System (INIS)

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

    2006-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-12-15

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

  1. Fifty years old, and still going strong: Transmission electron optical studies of materials

    International Nuclear Information System (INIS)

    Brown, L.M.

    2008-01-01

    Highlights in the history of transmission electron microscopy and scanning transmission electron microscopy include the introduction of diffraction contrast, resolution of periodic lattices by phase contrast and incoherent imaging via the high-angle annular dark-field detector. Convergent-beam electron diffraction and analytical electron microscopy, especially the application of energy-dispersive X-ray and electron energy-loss spectrometry, have provided structural and chemical information in addition to strain contrast from lattice defects. From the outset, novel specimen stages and improvements to aid the operator enhanced the electron-optical engineering provided by the instrument makers. The spatial resolution achieved was mainly determined by the way the instrument was used, and not by the basic resolution limit set by the electron optics. However, the application of computer controlled correction of spherical (and higher order) aberration has resulted in a new generation of instruments capable of sub-Angstrom point-to-point resolution. This improved performance, combined with electron energy-loss spectrometry, promises genuine three-dimensional determination of atomic and electronic structure: an indispensable weapon in the battle to fabricate and control useful nanostructures. The uncertainty principle now fundamentally restricts some of the observations one can make, but much more technical development over the next decades must occur before one can say that the techniques of electron-optical imaging of material structure have reached their fundamental limitations. One can expect remarkable progress over the next few years

  2. Structural defects in multiferroic BiMnO3 studied by transmission electron microscopy and electron energy-loss spectroscopy

    International Nuclear Information System (INIS)

    Yang, H.; Chi, Z. H.; Yao, L. D.; Zhang, W.; Li, F. Y.; Jin, C. Q.; Yu, R. C.

    2006-01-01

    The multiferroic material BiMnO 3 synthesized under high pressure has been systematically studied by transmission electron microscopy and electron energy-loss spectroscopy, and some important structural defects are revealed in this multiferroic material. The frequently observed defects are characterized to be Σ3(111) twin boundaries, Ruddlesden-Popper [Acta Crystallogr. 11, 54 (1958)] antiphase boundaries, and a p p superdislocations connected with a small segment of Ruddlesden-Popper defect. These defects are present initially in the as-synthesized sample. In addition, we find that ordered voids (oxygen vacancies) are easily introduced into the multiferroic BiMnO 3 by electron-beam irradiation

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

    Science.gov (United States)

    Chrapoński, J; Rodak, K

    2006-09-01

    The aim of this work was to assess the changes in the microstructure of hot-deformed specimens made of alloys containing 46-50 at.% Al, 2 at.% Cr and 2 at.% Nb (and alloying additions such as carbon and boron) with the aid of scanning electron microscopy and transmission electron microscopy techniques. After homogenization and heat treatment performed in order to make diverse lamellae thickness, the specimens were compressed at 1000 degrees C. Transmission electron microscopy examinations of specimens after the compression test revealed the presence of heavily deformed areas with a high density of dislocation. Deformation twins were also observed. Dynamically recrystallized grains were revealed. For alloys no. 2 and no. 3, the recovery and recrystallization processes were more extensive than for alloy no. 1.

  4. Choice of operating voltage for a transmission electron microscope

    International Nuclear Information System (INIS)

    Egerton, R.F.

    2014-01-01

    An accelerating voltage of 100–300 kV remains a good choice for the majority of TEM or STEM specimens, avoiding the expense of high-voltage microscopy but providing the possibility of atomic resolution even in the absence of lens-aberration correction. For specimens thicker than a few tens of nm, the image intensity and scattering contrast are likely to be higher than at lower voltage, as is the visibility of ionization edges below 1000 eV (as required for EELS elemental analysis). In thick (>100 nm) specimens, higher voltage ensures less beam broadening and better spatial resolution for STEM imaging and EDX spectroscopy. Low-voltage (e.g. 30 kV) TEM or STEM is attractive for a very thin (e.g. 10 nm) specimen, as it provides higher scattering contrast and fewer problems for valence-excitation EELS. Specimens that are immune to radiolysis suffer knock-on damage at high current densities, and this form of radiation damage can be reduced or avoided by choosing a low accelerating voltage. Low-voltage STEM with an aberration-corrected objective lens (together with a high-angle dark-field detector and/or EELS) offers atomic resolution and elemental identification from very thin specimens. Conventional TEM can provide atomic resolution in low-voltage phase-contrast images but requires correction of chromatic aberration and preferably an electron-beam monochromator. Many non-conducting (e.g. organic) specimens damage easily by radiolysis and radiation damage then determines the TEM image resolution. For bright-field scattering contrast, low kV can provide slightly better dose-limited resolution if the specimen is very thin (a few nm) but considerably better resolution is possible from a thicker specimen, for which higher kV is required. Use of a phase plate in a conventional TEM offers the most dose-efficient way of achieving atomic resolution from beam-sensitive specimens. - Highlights: • 100–300 kV accelerating voltage is suitable for TEM specimens of typical

  5. Simulating Neutron Radiation Damage of Graphite by In-situ Electron Irradiation

    International Nuclear Information System (INIS)

    Mironov, Brindusa E; Freeman, H M; Brydson, R M D; Westwood, A V K; Scott, A J

    2014-01-01

    Radiation damage in nuclear grade graphite has been investigated using transmission electron microscopy (TEM) and electron energy loss spectroscopy (EELS). Changes in the structure on the atomic scale and chemical bonding, and the relationship between each were of particular interest. TEM was used to study damage in nuclear grade graphite on the atomic scale following 1.92×10 8 electrons nm −2 of electron beam exposure. During these experiments EELS spectra were also collected periodically to record changes in chemical bonding and structural disorder, by analysing the changes of the carbon K-edge. Image analysis software from the 'PyroMaN' research group provides further information, based on (002) fringe analysis. The software was applied to the micrographs of electron irradiated virgin 'Pile Grade A' (PGA) graphite to quantify the extent of damage from electron beam exposure

  6. The Development of a Hibachi Window for Electron Beam Transmission in a KrF Laser

    International Nuclear Information System (INIS)

    Gentile, C.A.; Parsells, R.; Butler, J.E.; Sethian, J.D.; Ciebiera, L.; Hegeler, F.; Jun, C.; Langish, S.; Myers, M.

    2003-01-01

    In support of Inertial Fusion Energy (IFE), a 150 (micro)m thick silicon (Si) wafer coated on one side with a 1.2 (micro)m nanocrystalline diamond foil is being fabricated as an electron beam transmission (hibachi) window for use in KrF lasers. The hibachi window separates the lasing medium from the electron beam source while allowing the electron beam to pass through. The hibachi window must be capable of withstanding the challenging environment presented in the lasing chamber, which include: fluorine gas, delta pressure >2 atm at 5 Hz, and a high heat flux due to the transmission of electrons passing through the foil. Tests at NRL/Electra and at PPPL have shown that a device employing these novel components in the stated configuration provide for a robust hibachi window with structural integrity

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

    International Nuclear Information System (INIS)

    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

  8. Application of Boltzmann equation to electron transmission and seconary electron emission

    International Nuclear Information System (INIS)

    Lanteri, H.; Bindi, R.; Rostaing, P.

    1979-01-01

    A method is presented for numerical treatment of integro-differential equation, based upon finite difference techniques. This method allows to formulate in a satisfactory manner the Boltzmann's equation applied to backscattering, transmission and secondary emission of metallic targets, avoiding must of the restrictive hypothesis, used until now in these models. For aluminium, the calculated energy spectra, angular distribution, transmission and backscattering coefficients, and secondary emission yield, are found to be in good agreement with experiment [fr

  9. In-situ fabrication of flexible vertically integrated electronic circuits by inkjet printing

    International Nuclear Information System (INIS)

    Wang Zhuo; Wu Wenwen; Yang Qunbao; Li Yongxiang; Noh, Chang-Ho

    2009-01-01

    In this paper, a facile approach for fabricating flexible vertically integrated electronic circuits is demonstrated. A desktop inkjet printer was modified and employed to print silver precursor on a polymer-coated buffer substrates. In-situ reaction was taken place and a conducting line was formed without need of a high temperature treatment. Through this process, several layers of metal integrated circuits were deposited sequentially with polymer buffer layers sandwiched between each layer. Hence, vertically integrated electronic components of diodes, solar cells, flexible flat panel displays, and electrochromic devices can be built with this simple and low-cost technique.

  10. Magnetic imaging with a Zernike-type phase plate in a transmission electron microscope

    DEFF Research Database (Denmark)

    Pollard, Shawn; Malac, Marek; Beleggia, Marco

    2013-01-01

    We demonstrate the use of a hole-free phase plate (HFPP) for magnetic imaging in transmission electron microscopy by mapping the domain structure in PrDyFeB samples. The HFPP, a Zernike-like imaging method, allows for detecting magnetic signals in-focus to correlate the sample crystal structure...... the reference wave distortion from long-range fields affecting electron holography....

  11. Transmission Electron Microscopy of the Gastrointestinal Tract of Nile Perch Lates niloticus

    OpenAIRE

    Namulawa, V. T; Kato, C. D; Nyatia, E; Rutaisire, J; Britz, P. J

    2015-01-01

    The ultrastructure of the gastrointestinal tract of Nile perch was described using Transmission Electron Microscopy standard procedures. Investigations revealed the presence of mucous cells, blood vessels and oil droplets plus several nerve cells and muscle bundles in the oral cavity. Further observations revealed columnar epithelial cells in the oesophagus, with a ragged surface, high electron dense cytoplasm, intercellular spaces, mitochondria and mucus granules. The lamina propria of the o...

  12. Electron dose dependence of signal-to-noise ratio, atom contrast and resolution in transmission electron microscope images

    International Nuclear Information System (INIS)

    Lee, Z.; Rose, H.; Lehtinen, O.; Biskupek, J.; Kaiser, U.

    2014-01-01

    In order to achieve the highest resolution in aberration-corrected (AC) high-resolution transmission electron microscopy (HRTEM) images, high electron doses are required which only a few samples can withstand. In this paper we perform dose-dependent AC-HRTEM image calculations, and study the dependence of the signal-to-noise ratio, atom contrast and resolution on electron dose and sampling. We introduce dose-dependent contrast, which can be used to evaluate the visibility of objects under different dose conditions. Based on our calculations, we determine optimum samplings for high and low electron dose imaging conditions. - Highlights: • The definition of dose-dependent atom contrast is introduced. • The dependence of the signal-to-noise ratio, atom contrast and specimen resolution on electron dose and sampling is explored. • The optimum sampling can be determined according to different dose conditions

  13. Assessing and ameliorating the influence of the electron beam on carbon nanotube oxidation in environmental transmission electron microscopy

    International Nuclear Information System (INIS)

    Koh, Ai Leen; Sinclair, Robert

    2017-01-01

    In this work, we examine how the imaging electron beam can induce damage in carbon nanotubes (CNTs) at varying oxygen gas pressures and electron dose rates using environmental transmission electron microscopy (ETEM). Our studies show that there is a threshold cumulative electron dose which brings about damage in CNTs in oxygen – through removal of their graphitic walls – which is dependent on O_2 pressure, with a 4–5 fold decrease in total electron dose per decade increase at a lower pressure range (10"−"6 to 10"−"5 mbar) and approximately 1.3 –fold decrease per decade increase at a higher pressure range (10"−"3 to 10"0 mbar). However, at a given pressure, damage in CNTs was found to occur even at the lowest dose rate utilized, suggesting the absence of a lower limit for the latter parameter. This study provides guidelines on the cumulative dose required to damage nanotubes in the 10"−"7 mbar to 10"0 mbar pressure regimes, and discusses the role of electron dose rate and total electron dose on beam-induced CNT degradation experiments. - Highlights: • The electron beam ionizes gas molecules in ETEM and affects experimental outcomes. • Beam-induced damage in CNTs occurs at varying O_2 pressures and electron dose rates. • There is a threshold cumulative dose to damage CNTs which depends on O_2 pressure. • At a given pressure, CNT damage occurs even at the electron dose rate utilized.

  14. Transmission electron microscopy: direct observation of crystal structure in refractory ceramics.

    Science.gov (United States)

    Shaw, T M; Thomas, G

    1978-11-10

    Using high-resolution multibeam interference techniques in the transmission electron microscope, images have been obtained that make possible a real-space structure analysis of a beryllium-silicon-nitrogen compound. The results illustrate the usefulness of lattice imaging in the analysis of local crystal structure in these technologically promising ceramic materials.

  15. Transmission electron microscopy investigation of colloids and particles from landfill leachates

    Czech Academy of Sciences Publication Activity Database

    Matura, M.; Ettler, V.; Klementová, Mariana

    2012-01-01

    Roč. 30, č. 5 (2012), s. 530-541 ISSN 0734-242X Institutional research plan: CEZ:AV0Z40320502 Keywords : colloids * landfill leachates * transmission electron microscopy * calcite * contaminant mobility Subject RIV: CA - Inorganic Chemistry Impact factor: 1.047, year: 2012

  16. Preparation of ZiO2 specimens for transmission electron microscopy

    International Nuclear Information System (INIS)

    Bressiani, A.H.A.

    1987-01-01

    The determination of average grain size, of the presence of monoclinic, tetragonal and cubic phases, as well as their relative distributions are necessary for the study of several partially stabilized zirconia properties. However, the phase distributions can be changed during the preparation of specimens for transmission electron microscopy, yielding misleading results. In this work suitable preparation method is reported. (Author) [pt

  17. Gas-phase synthesis of magnesium nanoparticles : A high-resolution transmission electron microscopy study

    NARCIS (Netherlands)

    Kooi, B.J.; Palasantzas, G.; de Hosson, J.T.M.

    2006-01-01

    Magnesium nanoparticles with size above 10 nm, prepared by gas-phase syntheses, were investigated by high-resolution transmission electron microscopy. The dominant particle shape is a hexagonal prism terminated by Mg(0002) and Mg{1010} facets. Oxidation of Mg yields a MgO shell (similar to 3 nm

  18. Preparation of transmission electron microscopy cross-section specimens using focused ion beam milling

    International Nuclear Information System (INIS)

    Langford, R.M.; Petford-Long, A.K.

    2001-01-01

    The preparation of transmission electron microscopy cross-section specimens using focused ion beam milling is outlined. The 'liftout' and 'trench' techniques are both described in detail, and their relative advantages and disadvantages are discussed. Artifacts such as ion damage to the top surface and sidewalls of the cross-section specimens, and methods of reducing them, are addressed

  19. Quantitative analysis of structural inhomogeneity in nanomaterials using transmission electron microscopy

    Czech Academy of Sciences Publication Activity Database

    Klinger, Miloslav; Polívka, Leoš; Jäger, Aleš; Tyunina, Marina

    2016-01-01

    Roč. 49, Jun (2016), 762-770 ISSN 1600-5767 R&D Projects: GA ČR GBP108/12/G043; GA ČR GA15-15123S Institutional support: RVO:68378271 Keywords : transmission electron microscopy * structural inhomogeneity * lattice parameters * image processing Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 2.495, year: 2016

  20. Transmission electron microscope examination of rare-gas bubbles in metals: analysis of observed contrast effects

    International Nuclear Information System (INIS)

    Levy, V.

    1964-01-01

    Metallic samples containing rare gas bubbles have been examined by transmission electron microscopy. The different features of the contrast patterns of the bubbles have been explained by the dynamical theory of contrast, assuming that the bubble behaves as a hole in the metal. Experimental results are in good agreement with the theory. (author) [fr

  1. Three-dimensional visualization and characterization of polymeric self-assemblies by Transmission Electron Microtomography

    NARCIS (Netherlands)

    H. Jinnai (Hiroshi); T. Higuchi (Takeshi); X. Zhuge (Jason); A. Kumamoto (Akihito); K.J. Batenburg (Joost); Y. Ikuhara (Yuichi)

    2017-01-01

    textabstractSelf-assembling structures and their dynamical processes in polymeric systems have been investigated using three-dimensional transmission electron microscopy (3D-TEM). Block copolymers (BCPs) self-assemble into nanoscale periodic structures called microphase-separated structures, a deep

  2. Simulations of the electron cloud buildup and its influence on the microwave transmission measurement

    Energy Technology Data Exchange (ETDEWEB)

    Haas, Oliver Sebastian, E-mail: o.haas@gsi.de [GSI Helmholtzzentrum für Schwerionenforschung GmbH, Planckstraße 1, 64291 Darmstadt (Germany); Boine-Frankenheim, Oliver [GSI Helmholtzzentrum für Schwerionenforschung GmbH, Planckstraße 1, 64291 Darmstadt (Germany); Technische Universität Darmstadt, Institut für Theorie Elektromagnetischer Felder, Schlossgartenstraße 8, 64289 Darmstadt (Germany); Petrov, Fedor [Technische Universität Darmstadt, Institut für Theorie Elektromagnetischer Felder, Schlossgartenstraße 8, 64289 Darmstadt (Germany)

    2013-11-21

    An electron cloud density in an accelerator can be measured using the Microwave Transmission (MWT) method. The aim of our study is to evaluate the influence of a realistic, nonuniform electron cloud on the MWT. We conduct electron cloud buildup simulations for beam pipe geometries and bunch parameters resembling roughly the conditions in the CERN SPS. For different microwave waveguide modes the phase shift induced by a known electron cloud density is obtained from three different approaches: 3D Particle-In-Cell (PIC) simulation of the electron response, a 2D eigenvalue solver for waveguide modes assuming a dielectric response function for cold electrons, a perturbative method assuming a sufficiently smooth density profile. While several electron cloud parameters, such as temperature, result in minor errors in the determined density, the transversely inhomogeneous density can introduce a large error in the measured electron density. We show that the perturbative approach is sufficient to describe the phase shift under realistic electron cloud conditions. Depending on the geometry of the beam pipe, the external magnetic field configuration and the used waveguide mode, the electron cloud density can be concentrated at the beam pipe or near the beam pipe center, leading to a severe over- or underestimation of the electron density. -- Author-Highlights: •Electron cloud distributions are very inhomogeneous, especially in dipoles. •These inhomogeneities affect the microwave transmission measurement results. •Electron density might be over- or underestimated, depending on setup. •This can be quantified with several models, e.g. a perturbative approach.

  3. The Investigation of New Magnetic Materials and Their Phenomena Using Ultrafast Fresnel Transmission Electron Microscopy

    Science.gov (United States)

    Schliep, Karl B.

    State-of-the-art technology drives scientific progress, pushing the boundaries of our current understanding of fundamental processes and mechanisms. Our continual scientific advancement is hindered only by what we can observe and experimentally verify; thus, it is reasonable to assert that instrument development and improvement is the cornerstone for technological and intellectual growth. For example, the invention of transmission electron microscopy (TEM) allowed us to observe nanoscale phenomena for the first time in the 1930s and even now it is invaluable in the development of smaller, faster electronics. As we uncover more about the fundamentals of nanoscale phenomena, we have realized that images alone reveal only a snapshot of the story; to continue progressing we need a way to observe the entire scene unfold (e.g. how defects affect the flow of current across a transistor or how thermal energy propagates in nanoscale systems like graphene). Recently, by combining the spatial resolution of a TEM with the temporal resolution of ultrafast lasers, ultrafast electron microscopy ? or microscope ? (UEM) has allowed us to simultaneously observe transient nanoscale phenomena at ultrafast timescales. Ultrafast characterization techniques allow for the investigation of a new realm of previously unseen phenomenon inherent to the transient electronic, magnetic, and structural properties of materials. However, despite the progress made in ultrafast techniques, capturing the nanoscale spatial sub-ns temporal mechanisms and phenomenon at play in magnetic materials (especially during the operation of magnetic devices) has only recently become possible using UEM. With only a handful of instruments available, magnetic characterization using UEM is far from commonplace and any advances made are sparsely reported, and further, specific to the individual instrument. In this dissertation, I outline the development of novel magnetic materials and the establishment of a UEM lab at

  4. Transmission Electron Microscopy of a CMSX-4 Ni-Base Superalloy Produced by Selective Electron Beam Melting

    Directory of Open Access Journals (Sweden)

    Alireza B. Parsa

    2016-10-01

    Full Text Available In this work, the microstructures of superalloy specimens produced using selective electron beam melting additive manufacturing were characterized. The materials were produced using a CMSX-4 powder. Two selective electron beam melting processing strategies, which result in higher and lower effective cooling rates, are described. Orientation imaging microscopy, scanning transmission electron microscopy and conventional high resolution transmission electron microscopy are used to investigate the microstructures. Our results suggest that selective electron beam melting processing results in near equilibrium microstructures, as far as γ′ volume fractions, the formation of small amounts of TCP phases and the partitioning behavior of the alloy elements are concerned. As expected, higher cooling rates result in smaller dendrite spacings, which are two orders of magnitude smaller than observed during conventional single crystal casting. During processing, columnar grains grow in <100> directions, which are rotated with respect to each other. There are coarse γ/γ′ microstructures in high angle boundary regions. Dislocation networks form low angle boundaries. A striking feature of the as processed selective electron beam melting specimens is their high dislocation density. From a fundamental point of view, this opens new possibilities for the investigation of elementary dislocation processes which accompany solidification.

  5. Bragg-edge neutron transmission strain tomography for in situ loadings

    Energy Technology Data Exchange (ETDEWEB)

    Wensrich, C.M., E-mail: christopher.wensrich@newcastle.edu.au [School of Engineering, The University of Newcastle, Callaghan, NSW 2308 (Australia); Hendriks, J.N.; Gregg, A. [School of Engineering, The University of Newcastle, Callaghan, NSW 2308 (Australia); Meylan, M.H. [School of Mathematical and Physical Sciences, The University of Newcastle, Callaghan, NSW 2308 (Australia); Luzin, V. [Bragg Institute, Australian Nuclear Science and Technology Organisation (ANSTO), Kirrawee, NSW 2232 (Australia); Tremsin, A.S. [Space Sciences Laboratory, University of California, Berkeley, CA 94720 (United States)

    2016-09-15

    An approach for tomographic reconstruction of three-dimensional strain distributions from Bragg-edge neutron transmission strain images is outlined and investigated. This algorithm is based on the link between Bragg-edge strain measurements and the Longitudinal Ray Transform, which has been shown to be sensitive only to boundary displacement. By exploiting this observation we provide a method for reconstructing boundary displacement from sets of Bragg-edge strain images. In the case where these displacements are strictly the result of externally applied tractions, corresponding internal strain fields can then be found through traditional linear-static finite element methods. This approach is tested on synthetic data in two-dimensions, where the rate of convergence in the presence of measurement noise and beam attenuation is examined.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-09-15

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

  7. In situ electron backscatter diffraction (EBSD) during the compression of micropillars

    International Nuclear Information System (INIS)

    Niederberger, C.; Mook, W.M.; Maeder, X.; Michler, J.

    2010-01-01

    For the first time, in situ electron backscatter diffraction (EBSD) measurements during compression experiments by a modified nanoindenter on micron-sized single crystal pillars are demonstrated here. The experimental setup and the requirements concerning the compression sample are described in detail. EBSD mappings have been acquired before loading, under load and after unloading for consecutive compression cycles on a focused ion beam (FIB) milled GaAs micropillar. In situ EBSD allows for the determination of crystallographic orientation with sub-100 nm spatial resolution. Thereby, it provides highly localized information pertaining to the deformation phenomena such as elastic bending of the micropillar or the formation of deformation twins and plastic orientation gradients due to geometrically necessary dislocations. The most striking features revealed by in situ EBSD are the non-negligible amount of reversible (elastic) bending of the micropillar and the fact that deformation twinning and dislocation glide initiate where the bending is strongest. Due to this high spatial and orientation resolution, in situ EBSD measurements during micromechanical testing are demonstrated to be a promising technique for the investigation of deformation phenomena at the nano- to micro-scale.

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

    Science.gov (United States)

    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.

  9. Portable spectroscopic scanning electron microscope on ISS: in situ nanostructural/chemical analysis for critical vehicle systems, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — We will construct a novel field-portable miniature analytical electron microscope (EM+EDS) called Mochii "S" for in situ sensing in harsh/remote environments such as...

  10. Miniature Variable Pressure Scanning Electron Microscope for In-Situ Imaging and Chemical Analysis

    Science.gov (United States)

    Gaskin, Jessica A.; Jerman, Gregory; Gregory, Don; Sampson, Allen R.

    2012-01-01

    NASA Marshall Space Flight Center (MSFC) is leading an effort to develop a Miniaturized Variable Pressure Scanning Electron Microscope (MVP-SEM) for in-situ imaging and chemical analysis of uncoated samples. This instrument development will be geared towards operation on Mars and builds on a previous MSFC design of a mini-SEM for the moon (funded through the NASA Planetary Instrument Definition and Development Program). Because Mars has a dramatically different environment than the moon, modifications to the MSFC lunar mini-SEM are necessary. Mainly, the higher atmospheric pressure calls for the use of an electron gun that can operate at High Vacuum, rather than Ultra-High Vacuum. The presence of a CO2-rich atmosphere also allows for the incorporation of a variable pressure system that enables the in-situ analysis of nonconductive geological specimens. Preliminary testing of Mars meteorites in a commercial Environmental SEM(Tradmark) (FEI) confirms the usefulness of lowcurrent/low-accelerating voltage imaging and highlights the advantages of using the Mars atmosphere for environmental imaging. The unique capabilities of the MVP-SEM make it an ideal tool for pursuing key scientific goals of NASA's Flagship Mission Max-C; to perform in-situ science and collect and cache samples in preparation for sample return from Mars.

  11. In situ electrical and thermal monitoring of printed electronics by two-photon mapping.

    Science.gov (United States)

    Pastorelli, Francesco; Accanto, Nicolò; Jørgensen, Mikkel; van Hulst, Niek F; Krebs, Frederik C

    2017-06-19

    Printed electronics is emerging as a new, large scale and cost effective technology that will be disruptive in fields such as energy harvesting, consumer electronics and medical sensors. The performance of printed electronic devices relies principally on the carrier mobility and molecular packing of the polymer semiconductor material. Unfortunately, the analysis of such materials is generally performed with destructive techniques, which are hard to make compatible with in situ measurements, and pose a great obstacle for the mass production of printed electronics devices. A rapid, in situ, non-destructive and low-cost testing method is needed. In this study, we demonstrate that nonlinear optical microscopy is a promising technique to achieve this goal. Using ultrashort laser pulses we stimulate two-photon absorption in a roll coated polymer semiconductor and map the resulting two-photon induced photoluminescence and second harmonic response. We show that, in our experimental conditions, it is possible to relate the total amount of photoluminescence detected to important material properties such as the charge carrier density and the molecular packing of the printed polymer material, all with a spatial resolution of 400 nm. Importantly, this technique can be extended to the real time mapping of the polymer semiconductor film, even during the printing process, in which the high printing speed poses the need for equally high acquisition rates.

  12. Numerical study of electron-leakage power loss in a tri-plate transmission line

    International Nuclear Information System (INIS)

    Barker, R.J.; Goldstein, S.A.

    1982-01-01

    Numerical simulations have been conducted using NRL's DIODE2D computer code to model the steady-state behavior of electron flow in a radial diode and in its adjacent tri-plate transmission line (TTL). Particular attention was paid to the magnitude of the electron current flowing from the cathode to the anode surface in the TTL. A quantitative value for this effective power loss is given. The electron current is restricted mainly to the transition region in the TTL into which there is seepage of the B/sub z/ that is imposed in the diode gap. This finding highlights the importance of that region to diode designers

  13. Achromatic elemental mapping beyond the nanoscale in the transmission electron microscope.

    Science.gov (United States)

    Urban, K W; Mayer, J; Jinschek, J R; Neish, M J; Lugg, N R; Allen, L J

    2013-05-03

    Newly developed achromatic electron optics allows the use of wide energy windows and makes feasible energy-filtered transmission electron microscopy (EFTEM) at atomic resolution. In this Letter we present EFTEM images formed using electrons that have undergone a silicon L(2,3) core-shell energy loss, exhibiting a resolution in EFTEM of 1.35 Å. This permits elemental mapping beyond the nanoscale provided that quantum mechanical calculations from first principles are done in tandem with the experiment to understand the physical information encoded in the images.

  14. Simulation and Analysis of Microwave Transmission through an Electron Cloud, a Comparison of Results

    International Nuclear Information System (INIS)

    Sonnad, Kiran; Sonnad, Kiran; Furman, Miguel; Veitzer, Seth; Stoltz, Peter; Cary, John

    2007-01-01

    Simulation studies for transmission of microwaves through electron clouds show good agreement with analytic results. The electron cloud produces a shift in phase of the microwave. Experimental observation of this phenomena would lead to a useful diagnostic tool for accessing the local density of electron clouds in an accelerator. These experiments are being carried out at the CERN SPS and the PEP-II LER at SLAC and is proposed to be done at the Fermilab main injector. In this study, a brief analysis of the phase shift is provided and the results are compared with that obtained from simulations

  15. Investigating the mesostructure of ordered porous silica nanocomposites by transmission electron microscopy techniques

    Energy Technology Data Exchange (ETDEWEB)

    Bullita, S.; Casula, M. F., E-mail: casulaf@unica.it [INSTM and Department of Chemical and Geological Science, University of Cagliari, Monserrato (Canada) (Italy); Piludu, M. [Department of Biomedical Sciences, University of Cagliari, Monserrato (Canada) (Italy); Falqui, A. [INSTM and Department of Chemical and Geological Science, University of Cagliari, Monserrato (Canada) Italy and KAUST-King Abdullah University of Science and Technology, Jeddah (Saudi Arabia); Carta, D. [INSTM and Department of Chemical and Geological Science, University of Cagliari, Monserrato (Canada), Italy and Faculty of Physical Sciences and Engineering, University of Southampton, Southampton (United Kingdom); Corrias, A. [INSTM and Department of Chemical and Geological Science, University of Cagliari, Monserrato (Canada) Italy and School of Physical Sciences, Ingram Building, University of Kent, Canterbury (United Kingdom)

    2014-10-21

    Nanocomposites made out of FeCo alloy nanocrystals supported onto pre-formed mesoporous ordered silica which features a cubic arrangement of pores (SBA-16) were investigated. Information on the effect of the nanocrystals on the mesostructure (i.e. pore arrangement symmetry, pore size, and shape) were deduced by a multitechnique approach including N2 physisorption, low angle X-ray diffraction, and Transmission electron microscopy. It is shown that advanced transmission electron microscopy techniques are required, however, to gain direct evidence on key compositional and textural features of the nanocomposites. In particular, electron tomography and microtomy techniques make clear that the FeCo nanocrystals are located within the pores of the SBA-16 silica, and that the ordered mesostructure of the nanocomposite is retained throughout the observed specimen.

  16. Three-dimensional optical transfer functions in the aberration-corrected scanning transmission electron microscope.

    Science.gov (United States)

    Jones, L; Nellist, P D

    2014-05-01

    In the scanning transmission electron microscope, hardware aberration correctors can now correct for the positive spherical aberration of round electron lenses. These correctors make use of nonround optics such as hexapoles or octupoles, leading to the limiting aberrations often being of a nonround type. Here we explore the effect of a number of potential limiting aberrations on the imaging performance of the scanning transmission electron microscope through their resulting optical transfer functions. In particular, the response of the optical transfer function to changes in defocus are examined, given that this is the final aberration to be tuned just before image acquisition. The resulting three-dimensional optical transfer functions also allow an assessment of the performance of a system for focal-series experiments or optical sectioning applications. © 2014 The Authors Journal of Microscopy © 2014 Royal Microscopical Society.

  17. Attosecond electron pulse trains and quantum state reconstruction in ultrafast transmission electron microscopy

    Science.gov (United States)

    Priebe, Katharina E.; Rathje, Christopher; Yalunin, Sergey V.; Hohage, Thorsten; Feist, Armin; Schäfer, Sascha; Ropers, Claus

    2017-12-01

    Ultrafast electron and X-ray imaging and spectroscopy are the basis for an ongoing revolution in the understanding of dynamical atomic-scale processes in matter. The underlying technology relies heavily on laser science for the generation and characterization of ever shorter pulses. Recent findings suggest that ultrafast electron microscopy with attosecond-structured wavefunctions may be feasible. However, such future technologies call for means to both prepare and fully analyse the corresponding free-electron quantum states. Here, we introduce a framework for the preparation, coherent manipulation and characterization of free-electron quantum states, experimentally demonstrating attosecond electron pulse trains. Phase-locked optical fields coherently control the electron wavefunction along the beam direction. We establish a new variant of quantum state tomography—`SQUIRRELS'—for free-electron ensembles. The ability to tailor and quantitatively map electron quantum states will promote the nanoscale study of electron-matter entanglement and new forms of ultrafast electron microscopy down to the attosecond regime.

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

    International Nuclear Information System (INIS)

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

    2010-01-01

    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.

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

    International Nuclear Information System (INIS)

    Dey, G. K.

    2011-01-01

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

  20. Electron magnetic chiral dichroism in CrO2 thin films using monochromatic probe illumination in a transmission electron microscope

    International Nuclear Information System (INIS)

    Loukya, B.; Zhang, X.; Gupta, A.; Datta, R.

    2012-01-01

    Electron magnetic chiral dichroism (EMCD) has been studied in CrO 2 thin films (with (100) and (110) growth orientations on TiO 2 substrates) using a gun monochromator in an aberration corrected transmission electron microscope operating at 300 kV. Excellent signal-to-noise ratio is obtained at spatial resolution ∼10 nm using a monochromatic probe as compared to conventional parallel illumination, large area convergent beam electron diffraction and scanning transmission electron microscopy techniques of EMCD. Relatively rapid exposure using mono probe illumination enables collection of EMCD spectra in total of 8–9 min in energy filtered imaging mode for a given Cr L 2,3 energy scan (energy range ∼35 eV). We compared the EMCD signal obtained by extracting the Cr L 2,3 spectra under three beam diffraction geometry of two different reciprocal vectors (namely g=110 and 200) and found that the g=200 vector enables acquisition of excellent EMCD signal from relatively thicker specimen area due to the associated larger extinction distance. Orbital to spin moment ratio has been calculated using EMCD sum rules for 3d elements and dichroic spectral features associated with CrO 2 are compared and discussed with XMCD theoretical spectra. - Highlights: ► Electron magnetic circular dichroism (EMCD) of CrO 2 thin film with two different orientations. ► Improved EMCD signal with Gun monochromator illumination. ► Improved EMCD signal with higher g vector.

  1. Dose-rate-dependent damage of cerium dioxide in the scanning transmission electron microscope.

    Science.gov (United States)

    Johnston-Peck, Aaron C; DuChene, Joseph S; Roberts, Alan D; Wei, Wei David; Herzing, Andrew A

    2016-11-01

    Beam damage caused by energetic electrons in the transmission electron microscope is a fundamental constraint limiting the collection of artifact-free information. Through understanding the influence of the electron beam, experimental routines may be adjusted to improve the data collection process. Investigations of CeO 2 indicate that there is not a critical dose required for the accumulation of electron beam damage. Instead, measurements using annular dark field scanning transmission electron microscopy and electron energy loss spectroscopy demonstrate that the onset of measurable damage occurs when a critical dose rate is exceeded. The mechanism behind this phenomenon is that oxygen vacancies created by exposure to a 300keV electron beam are actively annihilated as the sample re-oxidizes in the microscope environment. As a result, only when the rate of vacancy creation exceeds the recovery rate will beam damage begin to accumulate. This observation suggests that dose-intensive experiments can be accomplished without disrupting the native structure of the sample when executed using dose rates below the appropriate threshold. Furthermore, the presence of an encapsulating carbonaceous layer inhibits processes that cause beam damage, markedly increasing the dose rate threshold for the accumulation of damage. Published by Elsevier B.V.

  2. Ultrafast transmission electron microscopy using a laser-driven field emitter: Femtosecond resolution with a high coherence electron beam

    Energy Technology Data Exchange (ETDEWEB)

    Feist, Armin; Bach, Nora; Rubiano da Silva, Nara; Danz, Thomas; Möller, Marcel; Priebe, Katharina E.; Domröse, Till; Gatzmann, J. Gregor; Rost, Stefan; Schauss, Jakob; Strauch, Stefanie; Bormann, Reiner; Sivis, Murat; Schäfer, Sascha, E-mail: sascha.schaefer@phys.uni-goettingen.de; Ropers, Claus, E-mail: claus.ropers@uni-goettingen.de

    2017-05-15

    We present the development of the first ultrafast transmission electron microscope (UTEM) driven by localized photoemission from a field emitter cathode. We describe the implementation of the instrument, the photoemitter concept and the quantitative electron beam parameters achieved. Establishing a new source for ultrafast TEM, the Göttingen UTEM employs nano-localized linear photoemission from a Schottky emitter, which enables operation with freely tunable temporal structure, from continuous wave to femtosecond pulsed mode. Using this emission mechanism, we achieve record pulse properties in ultrafast electron microscopy of 9 Å focused beam diameter, 200 fs pulse duration and 0.6 eV energy width. We illustrate the possibility to conduct ultrafast imaging, diffraction, holography and spectroscopy with this instrument and also discuss opportunities to harness quantum coherent interactions between intense laser fields and free-electron beams. - Highlights: • First implementation of an ultrafast TEM employing a nanoscale photocathode. • Localized single photon-photoemission from nanoscopic field emitter yields low emittance ultrashort electron pulses. • Electron pulses focused down to ~9 Å, with a duration of 200 fs and an energy width of 0.6 eV are demonstrated. • Quantitative characterization of ultrafast electron gun emittance and brightness. • A range of applications of high coherence ultrashort electron pulses is shown.

  3. In situ electromagnetic field diagnostics with an electron plasma in a Penning-Malmberg trap

    CERN Document Server

    Amole, C; Baquero-Ruiz, M.; Bertsche, W.; Butler, E.; Capra, A.; Cesar, C.L.; Charlton, M.; Deller, A.; Evetts, N.; Eriksson, S.; Fajans, J.; Friesen, T.; Fujiwara, M.C.; Gill, D.R.; Gutierrez, A.; Hangst, J.S.; Hardy, W.N.; Hayden, M.E.; Isaac, C.A.; Jonsell, S.; Kurchaninov, L.; Little, A.; Madsen, N.; McKenna, J.T.K.; Menary, S.; Napoli, S.C.; Olchanski, K.; Olin, A.; Pusa, P.; Rasmussen, C.; Robicheaux, F.; Sarid, E.; Silveira, D.M.; So, C.; Stracka, S.; Tharp, T.; Thompson, R.I.; van der Werf, D.P.; Wurtele, J.S.

    2014-01-01

    We demonstrate a novel detection method for the cyclotron resonance frequency of an electron plasma in a Penning-Malmberg trap. With this technique, the electron plasma is used as an in situ diagnostic tool for measurement of the static magnetic field and the microwave electric field in the trap. The cyclotron motion of the electron plasma is excited by microwave radiation and the temperature change of the plasma is measured non-destructively by monitoring the plasma's quadrupole mode frequency. The spatially-resolved microwave electric field strength can be inferred from the plasma temperature change and the magnetic field is found through the cyclotron resonance frequency. These measurements were used extensively in the recently reported demonstration of resonant quantum interactions with antihydrogen.

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

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, C.; Golberg, D., E-mail: xuzhi@iphy.ac.cn, E-mail: golberg.dmitri@nims.go.jp [International Center for Materials Nanoarchitectonics (MANA), National Institute for Materials Science (NIMS), Namiki 1-1, Tsukuba, Ibaraki 3050044 (Japan); Graduate School of Pure and Applied Sciences, University of Tsukuba, Tennodai 1, Tsukuba, Ibaraki 3058577 (Japan); Xu, Z., E-mail: xuzhi@iphy.ac.cn, E-mail: golberg.dmitri@nims.go.jp [Beijing National Laboratory for Condensed Matter Physics, Institute of Physics, Chinese Academy of Sciences, Beijing 100190 (China); Kvashnin, D. G. [National University of Science and Technology, MISIS, Leninskiy Prospect 4, Moscow 119049 (Russian Federation); Tang, D.-M.; Xue, Y. M.; Bando, Y. [International Center for Materials Nanoarchitectonics (MANA), National Institute for Materials Science (NIMS), Namiki 1-1, Tsukuba, Ibaraki 3050044 (Japan); Sorokin, P. B. [National University of Science and Technology, MISIS, Leninskiy Prospect 4, Moscow 119049 (Russian Federation); Moscow Institute of Physics and Technology, Institutsky Lane 9, Dolgoprudny 141700 (Russian Federation)

    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.

  5. Spherical aberration correction in a scanning transmission electron microscope using a sculpted thin film.

    Science.gov (United States)

    Shiloh, Roy; Remez, Roei; Lu, Peng-Han; Jin, Lei; Lereah, Yossi; Tavabi, Amir H; Dunin-Borkowski, Rafal E; Arie, Ady

    2018-06-01

    Nearly eighty years ago, Scherzer showed that rotationally symmetric, charge-free, static electron lenses are limited by an unavoidable, positive spherical aberration. Following a long struggle, a major breakthrough in the spatial resolution of electron microscopes was reached two decades ago by abandoning the first of these conditions, with the successful development of multipole aberration correctors. Here, we use a refractive silicon nitride thin film to tackle the second of Scherzer's constraints and demonstrate an alternative method for correcting spherical aberration in a scanning transmission electron microscope. We reveal features in Si and Cu samples that cannot be resolved in an uncorrected microscope. Our thin film corrector can be implemented as an immediate low cost upgrade to existing electron microscopes without re-engineering of the electron column or complicated operation protocols and can be extended to the correction of additional aberrations. Copyright © 2018 The Authors. Published by Elsevier B.V. All rights reserved.

  6. An in situ Comparison of Electron Acceleration at Collisionless Shocks under Differing Upstream Magnetic Field Orientations

    Energy Technology Data Exchange (ETDEWEB)

    Masters, A.; Dougherty, M. K. [The Blackett Laboratory, Imperial College London, Prince Consort Road, London, SW7 2AZ (United Kingdom); Sulaiman, A. H. [Department of Physics and Astronomy, University of Iowa, Iowa City, IA 52242 (United States); Stawarz, Ł. [Astronomical Observatory, Jagiellonian University, ul. Orla 171, 30-244 Krakow (Poland); Reville, B. [School of Mathematics and Physics, Queens University Belfast, Belfast BT7 1NN (United Kingdom); Sergis, N. [Office of Space Research and Technology, Academy of Athens, Soranou Efesiou 4, 11527 Athens (Greece); Fujimoto, M. [Institute of Space and Astronautical Science, Japan Aerospace Exploration Agency, 3-1-1 Yoshinodai, Chuo-ku, Sagamihara, Kanagawa 252-5210 (Japan); Burgess, D. [School of Physics and Astronomy, Queen Mary University of London, London E1 4NS (United Kingdom); Coates, A. J., E-mail: a.masters@imperial.ac.uk [Mullard Space Science Laboratory, Department of Space and Climate Physics, University College London, Holmbury St. Mary, Dorking RH5 6NT (United Kingdom)

    2017-07-10

    A leading explanation for the origin of Galactic cosmic rays is acceleration at high-Mach number shock waves in the collisionless plasma surrounding young supernova remnants. Evidence for this is provided by multi-wavelength non-thermal emission thought to be associated with ultrarelativistic electrons at these shocks. However, the dependence of the electron acceleration process on the orientation of the upstream magnetic field with respect to the local normal to the shock front (quasi-parallel/quasi-perpendicular) is debated. Cassini spacecraft observations at Saturn’s bow shock have revealed examples of electron acceleration under quasi-perpendicular conditions, and the first in situ evidence of electron acceleration at a quasi-parallel shock. Here we use Cassini data to make the first comparison between energy spectra of locally accelerated electrons under these differing upstream magnetic field regimes. We present data taken during a quasi-perpendicular shock crossing on 2008 March 8 and during a quasi-parallel shock crossing on 2007 February 3, highlighting that both were associated with electron acceleration to at least MeV energies. The magnetic signature of the quasi-perpendicular crossing has a relatively sharp upstream–downstream transition, and energetic electrons were detected close to the transition and immediately downstream. The magnetic transition at the quasi-parallel crossing is less clear, energetic electrons were encountered upstream and downstream, and the electron energy spectrum is harder above ∼100 keV. We discuss whether the acceleration is consistent with diffusive shock acceleration theory in each case, and suggest that the quasi-parallel spectral break is due to an energy-dependent interaction between the electrons and short, large-amplitude magnetic structures.

  7. Characterization of Li-rich layered oxides by using transmission electron microscope

    Directory of Open Access Journals (Sweden)

    Hu Zhao

    2017-07-01

    Full Text Available Lithium-rich layered oxides (LrLOs deliver extremely high specific capacities and are considered to be promising candidates for electric vehicle and smart grid applications. However, the application of LrLOs needs further understanding of the structural complexity and dynamic evolution of monoclinic and rhombohedral phases, in order to overcome the issues including voltage decay, poor rate capability, initial irreversible capacity loss and etc. The development of aberration correction for the transmission electron microscope and concurrent progress in electron spectroscopy, have fueled rapid progress in the understanding of the mechanism of such issues. New techniques based on the transmission electron microscope are first surveyed, and the applications of these techniques for the study of the structure, migration of transition metal, and the activation of oxygen of LrLOs are then explored in detail, with a particular focus on the mechanism of voltage decay. Keywords: Lithium-ion battery, Transmission electron microscope, Lithium-rich layered oxide, Cathode material

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

    Energy Technology Data Exchange (ETDEWEB)

    Brown, H.G.; D' Alfonso, A.J.; Forbes, B.D.; Allen, L.J., E-mail: lja@unimelb.edu.au

    2016-01-15

    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. - Highlights: • Interpretation of EFTEM images is complicated by preservation of elastic contrast. • More direct images obtained by scanning with a focused coherent probe and averaging. • This is equivalent to precession EFTEM through the solid angle defined by the probe. • Also yields similar results to energy-loss scanning transmission electron microscopy. • Scanning approach immune to probe aberrations and resilient to scan distortions.

  9. Ohmic contact junction of carbon nanotubes fabricated by in situ electron beam deposition

    International Nuclear Information System (INIS)

    Wang, Y G; Wang, T H; Lin, X W; Dravid, V P

    2006-01-01

    We present experimental evidence of in situ fabrication of multi-walled carbon nanotube junctions via electron beam induced deposition. The tip-to-tip interconnection of the nanotubes involves the alignment of two nanotubes via a piezodriven nanomanipulator and nano-welding by electron beam deposition. Hydrocarbon contamination from the pump oil vapour of the vacuum system of the TEM chamber was used as the solder; this is superior to the already available metallic solders because its composition is identical to the carbon nanotube. The hydrocarbon deposition, with perfect wettability, on the nanotubes establishes strong mechanical binding between the two nanotubes to form an integrated structure. Consequently, the nanotubes cross-linked by the hydrocarbon solder produce good electrical and mechanical connections. The joint dimension was determined by the size of the electron beam, which results in a sound junction with well-defined geometry and the smallest junction size obtained so far. In situ electric measurement showed a linear current-voltage property for the multi-walled nanotube junction

  10. Multiphoton electronic-spin generation and transmission spectroscopy in n-type GaAs

    Energy Technology Data Exchange (ETDEWEB)

    Idrish Miah, M., E-mail: m.miah@griffith.edu.a [Department of Physics, University of Chittagong, Chittagong 4331 (Bangladesh)

    2011-01-17

    Multiphoton electronic-spin generation in semiconductors was investigated using differential transmission spectroscopy. The generation of the electronic spins in the semiconductor samples were achieved by multiphoton pumping with circularly polarized light beam and was probed by the spin-resolved transmission of the samples. The electronic spin-polarization of conduction band was estimated and was found to depend on the delay of the probe beam, temperature as well as on the multiphoton pumping energy. The temperature dependence showed a decrease of the spin-polarization with increasing temperature. The electronic spin-polarization was found to depolarize rapidly for multiphoton pumping energy larger than the energy gap of the split-off band to the conduction band. The results were compared with those obtained in one-photon pumping, which shows that an enhancement of the electronic spin-polarization was achieved in multiphoton pumping. The findings resulting from this investigation might have potential applications in opto-spintronics, where the generation of highly polarized electronic spins is required.

  11. Multiphoton electronic-spin generation and transmission spectroscopy in n-type GaAs

    International Nuclear Information System (INIS)

    Idrish Miah, M.

    2011-01-01

    Multiphoton electronic-spin generation in semiconductors was investigated using differential transmission spectroscopy. The generation of the electronic spins in the semiconductor samples were achieved by multiphoton pumping with circularly polarized light beam and was probed by the spin-resolved transmission of the samples. The electronic spin-polarization of conduction band was estimated and was found to depend on the delay of the probe beam, temperature as well as on the multiphoton pumping energy. The temperature dependence showed a decrease of the spin-polarization with increasing temperature. The electronic spin-polarization was found to depolarize rapidly for multiphoton pumping energy larger than the energy gap of the split-off band to the conduction band. The results were compared with those obtained in one-photon pumping, which shows that an enhancement of the electronic spin-polarization was achieved in multiphoton pumping. The findings resulting from this investigation might have potential applications in opto-spintronics, where the generation of highly polarized electronic spins is required.

  12. Effects of Electron Flow Current Density on Flow Impedance of Magnetically Insulated Transmission Lines

    International Nuclear Information System (INIS)

    He Yong; Zou Wen-Kang; Song Sheng-Yi

    2011-01-01

    In modern pulsed power systems, magnetically insulated transmission lines (MITLs) are used to couple power between the driver and the load. The circuit parameters of MITLs are well understood by employing the concept of flow impedance derived from Maxwell's equations and pressure balance across the flow. However, the electron density in an MITL is always taken as constant in the application of flow impedance. Thus effects of electron flow current density (product of electron density and drift velocity) in an MITL are neglected. We calculate the flow impedances of an MITL and compare them under three classical MITL theories, in which the electron density profile and electron flow current density are different from each other. It is found that the assumption of constant electron density profile in the calculation of the flow impedance is not always valid. The electron density profile and the electron flow current density have significant effects on flow impedance of the MITL. The details of the electron flow current density and its effects on the operation impedance of the MITL should be addressed more explicitly by experiments and theories in the future. (nuclear physics)

  13. Assessing and ameliorating the influence of the electron beam on carbon nanotube oxidation in environmental transmission electron microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Koh, Ai Leen, E-mail: alkoh@stanford.edu [Stanford Nano Shared Facilities, Stanford University, Stanford, CA 94305 (United States); Sinclair, Robert [Department of Materials Science and Engineering, Stanford University, Stanford, CA 94305 (United States)

    2017-05-15

    In this work, we examine how the imaging electron beam can induce damage in carbon nanotubes (CNTs) at varying oxygen gas pressures and electron dose rates using environmental transmission electron microscopy (ETEM). Our studies show that there is a threshold cumulative electron dose which brings about damage in CNTs in oxygen – through removal of their graphitic walls – which is dependent on O{sub 2} pressure, with a 4–5 fold decrease in total electron dose per decade increase at a lower pressure range (10{sup −6} to 10{sup −5} mbar) and approximately 1.3 –fold decrease per decade increase at a higher pressure range (10{sup −3} to 10{sup 0} mbar). However, at a given pressure, damage in CNTs was found to occur even at the lowest dose rate utilized, suggesting the absence of a lower limit for the latter parameter. This study provides guidelines on the cumulative dose required to damage nanotubes in the 10{sup −7} mbar to 10{sup 0} mbar pressure regimes, and discusses the role of electron dose rate and total electron dose on beam-induced CNT degradation experiments. - Highlights: • The electron beam ionizes gas molecules in ETEM and affects experimental outcomes. • Beam-induced damage in CNTs occurs at varying O{sub 2} pressures and electron dose rates. • There is a threshold cumulative dose to damage CNTs which depends on O{sub 2} pressure. • At a given pressure, CNT damage occurs even at the electron dose rate utilized.

  14. Investigation of the martensitic phase transformations in CoFe single crystals using high-resolution transmission electron microscopy

    International Nuclear Information System (INIS)

    Waitz, T.

    1999-06-01

    In CoFe crystals containing 0.85, 1.5, 5.75 and 6.0at.% Fe the thermally induced martensitic phase transformations between the close packed lattices face centered cubic (fcc), double hexagonal close packed (dhcp) and hexagonal close packed (hcp) were studied. Transmission electron microscopy methods were applied including in-situ experiments; both high-resolution transmission electron microscopy (HRTEM) images and lattice fringe images were used to analyze the transformations at an atomic scale. Based on the results of both the transformations in the bulk and the in-situ transformations it is concluded that the phase transitions occur by the formation of lamellae on the close packed habit planes. The lamellae have a minimum thickness of 10 to 15 close packed planes; therefore transformation models that are based on random overlap of stacking faults can be excluded. The glissile transformation fronts of the lamellae contain transformation dislocations (partials) that are correlated on an atomic scale. In the HRTEM images partials that are only about 0.2 nm apart were resolved and analyzed in detail by circuits that are similar to Burgers circuits. Two attracting partials on adjacent close packed planes are the structural units of the transformation fronts; they are dipoles and paired partials (with a total Burgers vector of a single partial) in the case of the transformations hcp dhcp and fcc dhcp, respectively. Different arrangements of the partials at the transformation fronts lead to two different modes A and B of the phase transition. These two modes seem to be competitive processes that can be favored by different parameters of the material (as chemical composition and microstructure). Partials of mode A transformations have the same Burgers vectors; therefore the partials repel each other causing long range internal stresses and large transformation shear strains that can lead to a surface relief. Whereas, partials of mode B transformations have different

  15. Characterisation of nano-structured titanium and aluminium nitride coatings by indentation, transmission electron microscopy and electron energy loss spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Girleanu, M., E-mail: maria.girleanu@uha.fr [Mecanique, Materiaux et Procedes de Fabrication, LPMT (EA CNRS 4365), Universite de Haute Alsace, 61 rue Albert Camus, F-68093 Mulhouse (France); Pac, M.-J.; Louis, P. [Mecanique, Materiaux et Procedes de Fabrication, LPMT (EA CNRS 4365), Universite de Haute Alsace, 61 rue Albert Camus, F-68093 Mulhouse (France); Ersen, O.; Werckmann, J. [Departement Structures et Interfaces, IPCMS (UMR CNRS 7504), Universite de Strasbourg, 23 rue du Loess, F-67087 Strasbourg (France); Rousselot, C. [Departement Micro Nano Sciences et Systemes, FEMTO-ST (UMR CNRS 6174), Universite de Franche-Comte, BP 71427, F-25211 Montbeliard (France); Tuilier, M.-H. [Mecanique, Materiaux et Procedes de Fabrication, LPMT (EA CNRS 4365), Universite de Haute Alsace, 61 rue Albert Camus, F-68093 Mulhouse (France)

    2011-07-01

    Titanium and aluminium nitride Ti{sub 1-x}Al{sub x}N films deposited by radiofrequency magnetron reactive sputtering onto steel substrate are examined by transmission electron microscopy over all the range of composition (x = 0, 0.5, 0.68, 0.86, 1). The deposition parameters are optimised in order to grow nitride films with low stress over all the composition range. Transmission electron microscopy cross-section images of Vickers indentation prints performed on that set of coatings show the evolution of their damage behaviour as increasing x Al content. Cubic Ti-rich nitrides consist of small grains clustered in rather large columns sliding along each other during indentation. Hexagonal Al-rich films grow in thinner columns which can be bent under the Vickers tip. Indentation tests carried out on TiN and AlN films are simulated using finite element modelling. Particular aspects of shear stresses and displacements in the coating/substrate are investigated. The growth mode and the nanostructure of two typical films, TiN and Ti{sub 0.14}Al{sub 0.86}N, are studied in detail by combining transmission electron microscopy cross-sections and plan views. Electron energy loss spectrum taken across Ti{sub 0.14}Al{sub 0.86}N film suggests that a part of nitrogen atoms is in cubic-like local environment though the lattice symmetry of Al-rich coatings is hexagonal. The poorly crystallised domains containing Ti and N atoms in cubic-like environment are obviously located in grain boundaries and afford protection of the coating against cracking.

  16. Characterisation of nano-structured titanium and aluminium nitride coatings by indentation, transmission electron microscopy and electron energy loss spectroscopy

    International Nuclear Information System (INIS)

    Girleanu, M.; Pac, M.-J.; Louis, P.; Ersen, O.; Werckmann, J.; Rousselot, C.; Tuilier, M.-H.

    2011-01-01

    Titanium and aluminium nitride Ti 1-x Al x N films deposited by radiofrequency magnetron reactive sputtering onto steel substrate are examined by transmission electron microscopy over all the range of composition (x = 0, 0.5, 0.68, 0.86, 1). The deposition parameters are optimised in order to grow nitride films with low stress over all the composition range. Transmission electron microscopy cross-section images of Vickers indentation prints performed on that set of coatings show the evolution of their damage behaviour as increasing x Al content. Cubic Ti-rich nitrides consist of small grains clustered in rather large columns sliding along each other during indentation. Hexagonal Al-rich films grow in thinner columns which can be bent under the Vickers tip. Indentation tests carried out on TiN and AlN films are simulated using finite element modelling. Particular aspects of shear stresses and displacements in the coating/substrate are investigated. The growth mode and the nanostructure of two typical films, TiN and Ti 0.14 Al 0.86 N, are studied in detail by combining transmission electron microscopy cross-sections and plan views. Electron energy loss spectrum taken across Ti 0.14 Al 0.86 N film suggests that a part of nitrogen atoms is in cubic-like local environment though the lattice symmetry of Al-rich coatings is hexagonal. The poorly crystallised domains containing Ti and N atoms in cubic-like environment are obviously located in grain boundaries and afford protection of the coating against cracking.

  17. Magnetically insulated transmission line used for relativistic electron beam injection into SPAC-VI

    International Nuclear Information System (INIS)

    Tsuzuki, Tetsuya; Narihara, Kazumichi; Tomita, Yukihiro; Mohri, Akihiro.

    1980-10-01

    For the purpose to inject the electron beam with energy of about 1.5 MeV and current of about 100 kA into the SPAC-6 (torus device), a magnetically insulated transmission line was designed and constructed. The motion of electrons in the line was theoretically analyzed. The requirements for the design of the transmission line were as follows-: (a) condition of magnetic insulation, (b) suppression against reverse gas flow from the beam source to the torus, (c) care to minimize the influence of strong torus magnetic field, (d) reduction of inductance and (e) safety engineering measures, e.g., separation valve in the MITL between the beam source and the SPAC-6. The transmission line of 2.4 m long was designed and constructed. The wave forms of electric potential and current were measured. The transmission efficiency of current along the axis and the efficiency as a function of current at the end of the line were also measured. The reason of the loss of current is discussed. (J.P.N.)

  18. A graphene oxide-carbon nanotube grid for high-resolution transmission electron microscopy of nanomaterials

    International Nuclear Information System (INIS)

    Zhang Lina; Zhang Haoxu; Zhou Ruifeng; Chen Zhuo; Li Qunqing; Fan Shoushan; Jiang Kaili; Ge Guanglu; Liu Renxiao

    2011-01-01

    A novel grid for use in transmission electron microscopy is developed. The supporting film of the grid is composed of thin graphene oxide films overlying a super-aligned carbon nanotube network. The composite film combines the advantages of graphene oxide and carbon nanotube networks and has the following properties: it is ultra-thin, it has a large flat and smooth effective supporting area with a homogeneous amorphous appearance, high stability, and good conductivity. The graphene oxide-carbon nanotube grid has a distinct advantage when characterizing the fine structure of a mass of nanomaterials over conventional amorphous carbon grids. Clear high-resolution transmission electron microscopy images of various nanomaterials are obtained easily using the new grids.

  19. Electronic transmission through p-n and n-p-n junctions of graphene

    Energy Technology Data Exchange (ETDEWEB)

    Setare, M R [Department of Science of Bijar, University of Kurdistan, Bijar (Iran, Islamic Republic of); Jahani, D, E-mail: rezakord@ipm.co, E-mail: Dariush110@gmail.co [Department of Physics, Razi University, Kermanshah (Iran, Islamic Republic of)

    2010-06-23

    In this paper, we first evaluate the electronic transmission of Dirac fermions into a p-n junction of gapped graphene and show that the final result depends on the sign of the refractive index, n. We also, by considering the appropriate wavefunctions in the region of the electrostatic potential, show that both transmission and the reflection probability turn out to be positive and less than unity instead of the negative transmission and higher than unity reflection coefficient commonly referred to as the Klein paradox. We then obtain the transmission probability corresponding to a special p-n junction for which there exists a region in which the low energy excitations of graphene acquire a finite mass and, interestingly, find that in this case the transmission is independent of the index of refraction, in contrast with the corresponding result for gapped graphene. We then discuss the validity of the solutions reported in some of the papers cited in this work which, considering the Buettiker formula, turn out to lead to the wrong results for conductivity.

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

    Czech Academy of Sciences Publication Activity Database

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

    2012-01-01

    Roč. 122, NOV (2012), s. 48-59 ISSN 0304-3991 R&D Projects: GA ČR GA202/09/2073 Institutional research plan: CEZ:AV0Z20410507 Keywords : stereoscopy * scanning transmission electron microscopy * single crystal Ni-base superalloys * Dislocation substructures * Foil thickness measurement Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 2.470, year: 2012

  1. Principle of energy-filtering transmission electron microscopy and its applications

    International Nuclear Information System (INIS)

    Kurata, Hiroki

    1997-01-01

    Energy-filtering transmission electron microscopy (EFTEM) is widely used to make images and diffraction patterns more quantitative by removing the inelastic background, and to perform elemental and chemical mapping at high spatial resolution. The principal factors restricting the spatial resolution in elemental maps are discussed. The relativistic effect on inelastic scattering cross-section, which becomes significant for high-voltage EFTEM analysis, is also discussed in relation to the detection efficiency of core-loss signals. (author)

  2. Electronic excitation in transmission of relativistic H- ions through thin foils

    International Nuclear Information System (INIS)

    Reinhold, C.O.; Kuerpick, P.; Burgdoerfer, J.; Yoshida, S.

    1998-01-01

    The authors describe a theoretical model to study the transmission of relativistic H - ions through thin carbon foils. The approach is based on a Monte Carlo solution of the Langevin equation describing electronic excitations of the atoms during the transport through the foil. Calculations for the subshell populations of outgoing hydrogen atoms are found to be in good agreement with recent experimental data on an absolute scale and show that there exists a propensity for populating extreme Stark states

  3. Light-Induced Reduction of Cuprous Oxide in an Environmental Transmission Electron Microscope

    DEFF Research Database (Denmark)

    Cavalca, Filippo Carlo; Laursen, Anders Bo; Wagner, Jakob Birkedal

    2013-01-01

    Photocatalysts for solar fuel production are subject to intensive investigation as they constitute one viable route for solar energy harvesting. Cuprous oxide (Cu2O) is a working photocatalyst for hydrogen evolution but it photocorrodes upon light illumination in an aqueous environment....... Environmental transmission electron microscopy (ETEM) makes it possible to obtain insight into the local structure, composition and reactivity of catalysts in their working environment, which is of fundamental interest for sustainable energy research and is essential for further material optimization. Herein...

  4. Graphene as a transparent conductive support for studying biological molecules by transmission electron microscopy

    International Nuclear Information System (INIS)

    Nair, R. R.; Anissimova, S.; Novoselov, K. S.; Blake, P.; Blake, J. R.; Geim, A. K.; Zan, R.; Bangert, U.; Golovanov, A. P.; Morozov, S. V.; Latychevskaia, T.

    2010-01-01

    We demonstrate the application of graphene as a support for imaging individual biological molecules in transmission electron microscope (TEM). A simple procedure to produce free-standing graphene membranes has been designed. Such membranes are extremely robust and can support practically any submicrometer object. Tobacco mosaic virus has been deposited on graphene samples and observed in a TEM. High contrast has been achieved even though no staining has been applied.

  5. A Transmission Electron Microscope Investigation of Space Weathering Effects in Hayabusa Samples

    Science.gov (United States)

    Keller, Lindsay P.; Berger, Eve L.

    2014-01-01

    The Hayabusa mission to asteroid 25143 Itokawa successfully returned the first direct samples of the regolith from the surface of an asteroid. The Hayabusa samples thus present a special opportunity to directly investigate the evolution of asteroidal surfaces, from the development of the regolith to the study of the more complex effects of space weathering. Here we describe the mineralogy, microstructure and composition of three Hayabusa mission particles using transmission electron microscope (TEM) techniques

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

    International Nuclear Information System (INIS)

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

    2001-01-01

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

  7. The Physical Characterization of Liposome Salicylic Acid Using Transmission Electron Microscope

    International Nuclear Information System (INIS)

    Elman Panjaitan

    2008-01-01

    The physical characterization of liposome, formulated from salicylic acid using thin film hydration methods with cholesterol and soybean lecithin, has been done. The formula was characterized by optical microscopes and Transmission Electron Microscope (TEM). The observation result shows that the salicylic acid can be formulated to liposomes. Soybean lecithin combined with cholesterol (600 mg : 20 mg) was the best formula and the liposome was spherical vesicle like with dimension about 70 nm unit 800 nm. (author)

  8. Microstructure of NiTi orthodontic wires observations using transmission electron microscopy

    OpenAIRE

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

    2014-01-01

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

  9. Transmission dosimetry with a liquid-filled electronic portal imaging device

    International Nuclear Information System (INIS)

    Boellaard, R.; Van Herk, M.; Mijnheer, B.J.

    1995-01-01

    The aim of transmission dosimetry is to correlate transmission dose values with patient dose values. A liquid-filled electronic portal imaging device (EPID) has been developed. After determination of the dose response relationship, i.e. the relation between pixel value and dose rate, for clinical situations it was found that the EPID is applicable for two-dimensional dosimetry with an accuracy of about 1%. The aim of this study was to investigate transmission dose distributions at different phantom-detector distances to predict exit dose distributions from transmission dose images. An extensive set of transmission dose measurements below homogeneous phantoms were performed with the EPID. The influence of several parameters such as field size, phantom thickness, phantom-detector distance and phantom-source distance on the transmission dose and its distribution were investigated. The two-dimensional transmission dose images were separated into two components: a primary dose and a scattered dose distribution. It was found that the scattered dose is maximal at a phantom thickness of about 10 cm. The scattered dose distribution below a homogeneous phantom has a Gaussian shape. The width of the Gaussian is small at small phantom-detector distances and increases for larger phantom-detector distances. The dependence of the scattered dose distribution on the field size at various phantom-detector distances has been used to estimate the dose distribution at the exit site of the phantom. More work is underway to determine the exit dose distributions for clinical situations, including the presence of inhomogeneities

  10. Transmission dosimetry with a liquid-filled electronic portal imaging device

    Energy Technology Data Exchange (ETDEWEB)

    Boellaard, R; Van Herk, M; Mijnheer, B J [Nederlands Kanker Inst. ` Antoni van Leeuwenhoekhuis` , Amsterdam (Netherlands)

    1995-12-01

    The aim of transmission dosimetry is to correlate transmission dose values with patient dose values. A liquid-filled electronic portal imaging device (EPID) has been developed. After determination of the dose response relationship, i.e. the relation between pixel value and dose rate, for clinical situations it was found that the EPID is applicable for two-dimensional dosimetry with an accuracy of about 1%. The aim of this study was to investigate transmission dose distributions at different phantom-detector distances to predict exit dose distributions from transmission dose images. An extensive set of transmission dose measurements below homogeneous phantoms were performed with the EPID. The influence of several parameters such as field size, phantom thickness, phantom-detector distance and phantom-source distance on the transmission dose and its distribution were investigated. The two-dimensional transmission dose images were separated into two components: a primary dose and a scattered dose distribution. It was found that the scattered dose is maximal at a phantom thickness of about 10 cm. The scattered dose distribution below a homogeneous phantom has a Gaussian shape. The width of the Gaussian is small at small phantom-detector distances and increases for larger phantom-detector distances. The dependence of the scattered dose distribution on the field size at various phantom-detector distances has been used to estimate the dose distribution at the exit site of the phantom. More work is underway to determine the exit dose distributions for clinical situations, including the presence of inhomogeneities.

  11. A Monte Carlo investigation of contaminant electrons due to a novel in vivo transmission detector

    International Nuclear Information System (INIS)

    Asuni, G; Jensen, J M; McCurdy, B M C

    2011-01-01

    A novel transmission detector (IBA Dosimetry, Germany) developed as an IMRT quality assurance tool, intended for in vivo patient dose measurements, is studied here. The goal of this investigation is to use Monte Carlo techniques to characterize treatment beam parameters in the presence of the detector and to compare to those of a plastic block tray (a frequently used clinical device). Particular attention is paid to the impact of the detector on electron contamination model parameters of two commercial dose calculation algorithms. The linac head together with the COMPASS transmission detector (TRD) was modeled using BEAMnrc code. To understand the effect of the TRD on treatment beams, the contaminant electron fluence, energy spectra, and angular distributions at different SSDs were analyzed for open and non-open (i.e. TRD and block tray) fields. Contaminant electrons in the BEAMnrc simulations were separated according to where they were created. Calculation of surface dose and the evaluation of contributions from contaminant electrons were performed using the DOSXYZnrc user code. The effect of the TRD on contaminant electrons model parameters in Eclipse AAA and Pinnacle 3 dose calculation algorithms was investigated. Comparisons of the fluence of contaminant electrons produced in the non-open fields versus open field show that electrons created in the non-open fields increase at shorter SSD, but most of the electrons at shorter SSD are of low energy with large angular spread. These electrons are out-scattered or absorbed in air and contribute less to surface dose at larger SSD. Calculated surface doses with the block tray are higher than those with the TRD. Contribution of contaminant electrons to dose in the buildup region increases with increasing field size. The additional contribution of electrons to surface dose increases with field size for TRD and block tray. The introduction of the TRD results in a 12% and 15% increase in the Gaussian widths used in the

  12. Characterization of a direct detection device imaging camera for transmission electron microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Milazzo, Anna-Clare, E-mail: amilazzo@ncmir.ucsd.edu [University of California at San Diego, 9500 Gilman Dr., La Jolla, CA 92093 (United States); Moldovan, Grigore [Department of Materials, University of Oxford, Parks Road, Oxford OX1 3PH (United Kingdom); Lanman, Jason [Department of Molecular Biology, The Scripps Research Institute, La Jolla, CA 92037 (United States); Jin, Liang; Bouwer, James C. [University of California at San Diego, 9500 Gilman Dr., La Jolla, CA 92093 (United States); Klienfelder, Stuart [University of California at Irvine, Irvine, CA 92697 (United States); Peltier, Steven T.; Ellisman, Mark H. [University of California at San Diego, 9500 Gilman Dr., La Jolla, CA 92093 (United States); Kirkland, Angus I. [Department of Materials, University of Oxford, Parks Road, Oxford OX1 3PH (United Kingdom); Xuong, Nguyen-Huu [University of California at San Diego, 9500 Gilman Dr., La Jolla, CA 92093 (United States)

    2010-06-15

    The complete characterization of a novel direct detection device (DDD) camera for transmission electron microscopy is reported, for the first time at primary electron energies of 120 and 200 keV. Unlike a standard charge coupled device (CCD) camera, this device does not require a scintillator. The DDD transfers signal up to 65 lines/mm providing the basis for a high-performance platform for a new generation of wide field-of-view high-resolution cameras. An image of a thin section of virus particles is presented to illustrate the substantially improved performance of this sensor over current indirectly coupled CCD cameras.

  13. Characterization of a direct detection device imaging camera for transmission electron microscopy

    International Nuclear Information System (INIS)

    Milazzo, Anna-Clare; Moldovan, Grigore; Lanman, Jason; Jin, Liang; Bouwer, James C.; Klienfelder, Stuart; Peltier, Steven T.; Ellisman, Mark H.; Kirkland, Angus I.; Xuong, Nguyen-Huu

    2010-01-01

    The complete characterization of a novel direct detection device (DDD) camera for transmission electron microscopy is reported, for the first time at primary electron energies of 120 and 200 keV. Unlike a standard charge coupled device (CCD) camera, this device does not require a scintillator. The DDD transfers signal up to 65 lines/mm providing the basis for a high-performance platform for a new generation of wide field-of-view high-resolution cameras. An image of a thin section of virus particles is presented to illustrate the substantially improved performance of this sensor over current indirectly coupled CCD cameras.

  14. A video-amplifier device for the transmission-type electron microscope ELMISCOP I of Siemens

    International Nuclear Information System (INIS)

    Groboth, G.; Hoerl, E.M.

    1975-01-01

    In order to get a visual image of the sample at the final screen of a transmission-type electron microscope and to keep at the same time the sample at low temperature a video-amplifier device has been developed by the authors. Details about its design and the necessary reconstruction of the electron microscope equipment are given. The beam current density at the transparent screen is reduced to 10 -12 -10 -13 A.cm -2 . Moreover the costs of this video-amplifier device are lower than those available. (CR)

  15. Transmission electron microscopy analysis of skin lesions from sporotrichosis epidemic in Rio de Janeiro, Brazil.

    Science.gov (United States)

    Ferreira, Cassio Porto; Oliveira de Almeida, Ana Cristina; Corte-Real, Suzana

    2015-02-01

    Transmission electron microscopy can yield useful information in a range of scientific fields; it is capable of imaging at a significantly higher resolution than light microscopes and has been a very useful tool in the identification of morphological changes of the dermis as well as assessment of changes in the extracellular matrix. Our aim is to characterize by electron microscopy the cellular profile of lesions caused by Sporothrix schenckii from the sporotrichosis epidemic in its zoonotic form that occurs in Rio de Janeiro, Brazil. © The American Society of Tropical Medicine and Hygiene.

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

    Science.gov (United States)

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

    2016-01-01

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

  17. Gas-phase synthesis of magnesium nanoparticles: A high-resolution transmission electron microscopy study

    International Nuclear Information System (INIS)

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

    2006-01-01

    Magnesium nanoparticles with size above 10 nm, prepared by gas-phase syntheses, were investigated by high-resolution transmission electron microscopy. The dominant particle shape is a hexagonal prism terminated by Mg(0002) and Mg(1010) facets. Oxidation of Mg yields a MgO shell (∼3 nm thick), which has an orientation relation with the Mg. Inhomogeneous facet oxidation influences their growth kinetics resulting in a relatively broad size and shape distribution. Faceted voids between Mg and MgO shells indicate a fast outward diffusion of Mg and vacancy rearrangement into voids. The faceting of polar (220) planes is assisted by electron irradiation

  18. The Fresnel mode of Lorentz microscopy using a scanning transmission electron microscope

    International Nuclear Information System (INIS)

    Chapman, J.N.; Waddell, E.M.; Batson, P.E.; Ferrier, R.P.

    1979-01-01

    The most widely used method of investigating ferromagnetic films in the transmission electron microscope is the Fresnel or defocus mode of Lorentz microscopy. This may be implemented either in a fixed beam or a scanning instrument. Despite a rather inefficient utilization of electrons, several advantages accrue if the latter is used, and provided it is equipped with a field emission gun, low noise images may be obtained in acceptable recording times. To extract quantitative estimates of domain wall widths from such images it is necessary to measure accurately both instrumental and specimen parameters. Methods for this are discussed and an example of an analysis using a polycrystalline permalloy film is given. (Auth.)

  19. Transmission electron-microscopic studies of structural changes in polycrystalline graphite after high temperature irradiation

    International Nuclear Information System (INIS)

    Platonov, P.A.; Gurovich, B.A.; Shtrombakh, Ya.I.; Karpukhin, V.I.

    1985-01-01

    Transmission electron-microscopic investigation of polycrystalline graphite before and after irradiation is carried out. The direct use of graphite samples after ion thinning, as an inquiry subject is the basic peculiarity of the work. Main structural components of MPG-6 graphite before and after irradiation are revealed, the structural mechanism of the reactor graphite destruction under irradiation is demonstrated. The mean values of L αm and L cm crystallite dimensions are determined. Radiation defects, occuring in some crystallites after irradiation are revealed by the dark-field electron microscopy method

  20. Three-dimensional nanofabrication by electron-beam-induced deposition using 200-keV electrons in scanning transmission electron microscope

    International Nuclear Information System (INIS)

    Liu, Z.Q.; Mitsuishi, K.; Furuya, K.

    2005-01-01

    Attempts were made to fabricate three-dimensional nanostructures on and out of a substrate by electron-beam-induced deposition in a 200-kV scanning transmission electron microscope. Structures with parallel wires over the substrate surface were difficult to fabricate due to the direct deposition of wires on both top and bottom surfaces of the substrate. Within the penetration depth of the incident electron beam, nanotweezers were fabricated by moving the electron beam beyond different substrate layers. Combining the deposition of self-supporting wires and self-standing tips, complicated three-dimensional doll-like, flag-like, and gate-like nanostructures that extend out of the substrate were successfully fabricated with one-step or multi-step scans of the electron beam. Effects of coarsening, nucleation, and distortion during electron-beam-induced deposition are discussed. (orig.)

  1. In situ ETEM synthesis of NiGa alloy nanoparticles from nitrate salt solution

    DEFF Research Database (Denmark)

    Damsgaard, Christian Danvad; Duchstein, Linus Daniel Leonhard; Sharafutdinov, Irek

    2014-01-01

    Metallic alloy nanoparticles (NPs) are synthesized in situ in an environmental transmission electron microscope. Atomic level characterization of the formed alloy NPs is carried out at synthesis conditions by use of high-resolution transmission electron microscopy, electron diffraction and electron...

  2. Nanostructured PLD-grown gadolinia doped ceria: Chemical and structural characterization by transmission electron microscopy techniques

    DEFF Research Database (Denmark)

    Rodrigo, Katarzyna Agnieszka; Wang, Hsiang-Jen; Heiroth, Sebastian

    2011-01-01

    The morphology as well as the spatially resolved elemental and chemical characterization of 10 mol% gadolinia doped ceria (CGO10) structures prepared by pulsed laser deposition (PLD) technique are investigated by scanning transmission electron microscopy accompanied with electron energy loss spec......, indicate apparent variation of the ceria valence state across and along the film. No element segregation to the grain boundaries is detected. These results are discussed in the context of solid oxide fuel cell applications.......The morphology as well as the spatially resolved elemental and chemical characterization of 10 mol% gadolinia doped ceria (CGO10) structures prepared by pulsed laser deposition (PLD) technique are investigated by scanning transmission electron microscopy accompanied with electron energy loss...... spectroscopy and energy dispersive X-ray spectroscopy. A dense, columnar and structurally inhomogeneous CGO10 film, i.e. exhibiting grain size refinement across the film thickness, is obtained in the deposition process. The cerium M4,5 edges, used to monitor the local electronic structure of the grains...

  3. Design and implementation of a fs-resolved transmission electron microscope based on thermionic gun technology

    Energy Technology Data Exchange (ETDEWEB)

    Piazza, L., E-mail: luca.piazza@epfl.ch [Laboratory for Ultrafast Microscopy and Electron Scattering (LUMES), ICMP, Ecole Polytechnique Fédérale de Lausanne, CH-1015 Lausanne (Switzerland); Masiel, D.J. [Integrated Dynamic Electron Solutions, Inc., 455 Bolero Drive, Danville, CA 94526 (United States); LaGrange, T.; Reed, B.W. [Condensed Matter and Materials Division Physical and Life Sciences Directorate, Lawrence Livermore National Laboratory, P.O. Box 808, L-356, Livermore, CA 94550 (United States); Barwick, B. [Department of Physics, Trinity College, 300 Summit St., Hartford, CT 06106 (United States); Carbone, Fabrizio [Laboratory for Ultrafast Microscopy and Electron Scattering (LUMES), ICMP, Ecole Polytechnique Fédérale de Lausanne, CH-1015 Lausanne (Switzerland)

    2013-09-23

    Highlights: • We present the implementation of a femtosecond-resolved ultrafast TEM. • This is the first ultrafast TEM based on a thermionic gun geometry. • An additional condenser lens has been used to maximize the electron count. • We achieved a time resolution of about 300 fs and an energy resolution of 1 eV. - Abstract: In this paper, the design and implementation of a femtosecond-resolved ultrafast transmission electron microscope is presented, based on a thermionic gun geometry. Utilizing an additional magnetic lens between the electron acceleration and the nominal condenser lens system, a larger percentage of the electrons created at the cathode are delivered to the specimen without degrading temporal, spatial and energy resolution significantly, while at the same time maintaining the femtosecond temporal resolution. Using the photon-induced near field electron microscopy effect (PINEM) on silver nanowires the cross-correlation between the light and electron pulses was measured, showing the impact of the gun settings and initiating laser pulse duration on the electron bunch properties. Tuneable electron pulses between 300 fs and several ps can be obtained, and an overall energy resolution around 1 eV was achieved.

  4. Micro-four-point probes in a UHV scanning electron microscope for in-situ surface-conductivity measurements

    DEFF Research Database (Denmark)

    Shiraki, I.; Nagao, T.; Hasegawa, S.

    2000-01-01

    For in-situ measurements of surface conductivity in ultrahigh vacuum (UHV), we have installed micro-four-point probes (probe spacings down to 4 mum) in a UHV scanning electron microscope (SEM) combined with scanning reflection-high-energy electron diffraction (RHEED). With the aid of piezoactuators...

  5. Advantages of a monochromated transmission electron microscope for solid state physics

    International Nuclear Information System (INIS)

    Grogger, W.; Kothleitner, G.; Hofer, F.

    2006-01-01

    Full text: The characterization of nanostructured devices and functional materials at a nanometer scale is paramount for the understanding of their physical and chemical properties. Transmission electron microscopy (TEM) plays a central role, especially in terms of structural and chemical analysis on a nearly atomic scale. In particular, electron energy-loss spectrometry (EELS) can obtain information not only about the chemical composition of a thin sample, but also about chemical bonding and electronic structure (ionization edge fine structures) and optical properties (through valence loss EELS). Recent instrumental advances like monochromators for the electron gun in the TEM have made it possible to reduce the energy resolution to 0.15 eV at an acceleration voltage of 200 kV. Another strong point of the method lies in the combination with a fine electron probe (0.2 nm) which allows to record EELS spectra with high energy resolution and spatial resolution in the range of 1 nm. The improved energy resolution opens new possibilities for studying detailed electronic structure and bonding effects in solids such as transmission metal oxides. The experimental results will be compared with x-ray absorption spectroscopy and band structure calculations. A better energy-resolution is particularly important for measurements in the low loss region of the EELS spectrum which provides the information about the band gap and the dielectric function. We will highlight the potential of the method for studying metallic nanoparticles and semiconducting devices. Additionally, the influence of the intrinsic effects like core-hole and excited lifetime broadening and delocalization of the inelastically scattered electrons will be discussed. (author)

  6. Selected Energy Epitaxial Deposition and Low Energy Electron Microscopy of AlN, GaN and SiC Thin Films

    National Research Council Canada - National Science Library

    Davis, R

    1999-01-01

    The homoepitaxial growth of GaN(0001) layers was studied in situ and in real time using the low-energy electron microscope and ex situ using atomic force microscopy and transmission electron microscopy...

  7. On the threshold conditions for electron beam damage of asbestos amosite fibers in the transmission electron microscope (TEM).

    Science.gov (United States)

    Martin, Joannie; Beauparlant, Martin; Sauvé, Sébastien; L'Espérance, Gilles

    2016-12-01

    Asbestos amosite fibers were investigated to evaluate the damage caused by a transmission electron microscope (TEM) electron beam. Since elemental x-ray intensity ratios obtained by energy dispersive x-ray spectroscopy (EDS) are commonly used for asbestos identification, the impact of beam damage on these ratios was evaluated. It was determined that the magnesium/silicon ratio best represented the damage caused to the fiber. Various tests showed that most fibers have a current density threshold above which the chemical composition of the fiber is modified. The value of this threshold current density varied depending on the fiber, regardless of fiber diameter, and in some cases could not be determined. The existence of a threshold electron dose was also demonstrated. This value was dependent on the current density used and can be increased by providing a recovery period between exposures to the electron beam. This study also established that the electron beam current is directly related to the damage rate above a current density of 165 A/cm 2 . The large number of different results obtained suggest, that in order to ensure that the amosite fibers are not damaged, analysis should be conducted below a current density of 100 A/cm 2 .

  8. Electron holography study of magnetization behavior in the writer pole of a perpendicular magnetic recording head by a 1 MV transmission electron microscope.

    Science.gov (United States)

    Hirata, Kei; Ishida, Yoichi; Akashi, Tetsuya; Shindo, Daisuke; Tonomura, Akira

    2012-01-01

    The magnetic domain structure of the writer poles of perpendicular magnetic recording heads was studied using electron holography. Although the domain structure of a 100-nm-thick writer pole could be observed with a 300 kV transmission electron microscope, that of the 250-nm-thick writer pole could not be analyzed due to the limited transmission capability of the instrument. On the other hand, the detailed domain structure of the 250-nm-thick writer pole was successfully analyzed by a 1 MV electron microscope using its high transmission capability. The thickness and material dependency of the domain structure of a writer pole were discussed.

  9. Dual ion beam irradiation system for in situ observation with electron microscope

    International Nuclear Information System (INIS)

    Tsukamoto, Tetuo; Hojou, Kiiti; Furuno, Sigemi; Otsu, Hitosi; Izui, Kazuhiko.

    1993-01-01

    We have developed a new in situ observation system for dynamic processes under dual ion beam irradiation. The system consists of a modified 400 keV analytical electron microscope (JEOL, JEM-4000FX) and two 40 kV ion beam accelerators. This system allows evaluation of microscopic changes of structure and chemical bonding state of materials in the dynamic processes under two kinds of ion beam irradiations, that is required for the simulation test of the first wall of nuclear fusion reactors onto which He + , H + , and H 2 + ions are irradiated simultaneously. These two ion accelerators were equipped symmetrically both sides of the electron microscope and individually controlled. Each ion beam extracted from a duo-plasmatron ion gun is bent downward by an angle of 30deg with a mass-separating magnet, and introduced into specimen chamber of the electron microscope. Inside the specimen chamber the beam is deflected again by an angle of 30deg with an electrostatic prism so as to be incident on the specimen surface. Finally, two ion beams from both side are incident on the specimen surface at an angle of 60deg. The maximum ion current density of helium is more than 250μA/cm 2 at the specimen at an ion energy of 17 keV. Images of the electron microscope during dual ion beam irradiation are observed through a TV camera and recorded with a VTR. (author)

  10. Multiscale phase mapping of LiFePO4-based electrodes by transmission electron microscopy and electron forward scattering diffraction.

    Science.gov (United States)

    Robert, Donatien; Douillard, Thierry; Boulineau, Adrien; Brunetti, Guillaume; Nowakowski, Pawel; Venet, Denis; Bayle-Guillemaud, Pascale; Cayron, Cyril

    2013-12-23

    LiFePO4 and FePO4 phase distributions of entire cross-sectioned electrodes with various Li content are investigated from nanoscale to mesoscale, by transmission electron microscopy and by the new electron forward scattering diffraction technique. The distributions of the fully delithiated (FePO4) or lithiated particles (LiFePO4) are mapped on large fields of view (>100 × 100 μm(2)). Heterogeneities in thin and thick electrodes are highlighted at different scales. At the nanoscale, the statistical analysis of 64 000 particles unambiguously shows that the small particles delithiate first. At the mesoscale, the phase maps reveal a core-shell mechanism at the scale of the agglomerates with a preferential pathway along the electrode porosities. At larger scale, lithiation occurs in thick electrodes "stratum by stratum" from the surface in contact with electrolyte toward the current collector.

  11. In Situ Transmission Electron Microscopy Studies of the Magnetization Reversal Mechanism in Information Storage Materials.

    Science.gov (United States)

    Petford-Long; Portier; Bayle-Guillemaud; Anthony; Brug

    1998-05-01

    : The Foucault and Fresnel modes of Lorentz microscopy, together with a quantitative magnetization mapping technique, summed image differential phase-contrast imaging, were used to study the magnetization reversal mechanism of the sense layer in spin-valve structures exhibiting the giant magnetoresistance effect. In addition to studies of sheet film, lithographically defined spin-valve elements were investigated. A current can be passed through the element during magnetizing so that the effect of the applied current on the giant magnetoresistance and magnetization reversal mechanism can be studied. Results are presented for a number of different spin-valve structures.

  12. In Situ Transmission Electron Microscopy Observation of Nanostructural Changes in Phase-Change Memory

    KAUST Repository

    Meister, Stefan; Kim, SangBum; Cha, Judy J.; Wong, H.-S. Philip; Cui, Yi

    2011-01-01

    Phase-change memory (PCM) has been researched extensively as a promising alternative to flash memory. Important studies have focused on its scalability, switching speed, endurance, and new materials. Still, reliability issues and inconsistent

  13. Using conventional and in situ transmission electron microscopy techniques to understand nanoscale crystallography

    Science.gov (United States)

    Hudak, Bethany M.

    Science, technology, engineering, and mathematics (STEM) education has become an emphasized component of PreK-12 education in the United States. The US is struggling to produce enough science, mathematics, and technology experts to meet its national and global needs, and the mean scores of science and mathematics students are not meeting the expected levels desired by our leaders (Hossain & Robinson, 2011). In an effort to improve achievement scores in mathematics and science, school districts must consider many components that can contribute to the development of a classroom where students are engaged and growing academically. Computer technology (CT) for student use is a popular avenue for school districts to pursue in their goal to attain higher achievement. The purpose of this study is to examine the use of iPads in a one-to-one setting, where every student has his own device 24/7, to determine the effects, if any, on academic achievement in the areas of mathematics and science. This comparison study used hierarchical linear modeling (HLM) to examine three middle schools in a private school district. Two of the schools have implemented a one-to-one iPad program with their sixth through eighth grades and the third school uses computers on limited occasions in the classroom and in a computer lab setting. The questions addressed were what effect, if any, do the implementation of a one-to-one iPad program and a teacher's perception of his use of constructivist teaching strategies have on student academic achievement in the mathematics and science middle school classrooms. The research showed that although the program helped promote the use of constructivist activities through the use of technology, the one-to-one iPad initiative had no effect on academic achievement in the middle school mathematics and science classrooms.

  14. Ab initio transmission electron microscopy image simulations of coherent Ag-MgO interfaces

    International Nuclear Information System (INIS)

    Mogck, S.; Kooi, B.J.; Hosson, J.Th.M. de; Finnis, M.W.

    2004-01-01

    Density-functional theory calculations, within the plane-wave-ultrasoft pseudopotential framework, were performed in the projection for MgO and for the coherent (111) Ag-MgO polar interface. First-principles calculations were incorporated in high-resolution transmission electron microscopy (HRTEM) simulations by converting the charge density into electron scattering factors to examine the influence of charge transfer, charge redistribution at the interface, and ionicity on the dynamical electron scattering and on calculated HRTEM images. It is concluded that the ionicity of oxides and the charge redistribution at interfaces play a significant role in HRTEM image simulations. In particular, the calculations show that at oxygen-terminated (111) Ag-MgO interfaces the first oxygen layer at the interface is much brighter than that in calculations with neutral atoms, in agreement with experimental observations

  15. Nucleation of diamond by pure carbon ion bombardment--a transmission electron microscopy study

    International Nuclear Information System (INIS)

    Yao, Y.; Liao, M.Y.; Wang, Z.G.; Lifshitz, Y.; Lee, S.

    2005-01-01

    A cross-sectional high-resolution transmission electron microscopy (HRTEM) study of a film deposited by a 1 keV mass-selected carbon ion beam onto silicon held at 800 deg. C is presented. Initially, a graphitic film with its basal planes perpendicular to the substrate is evolving. The precipitation of nanodiamond crystallites in upper layers is confirmed by HRTEM, selected area electron diffraction, and electron energy loss spectroscopy. The nucleation of diamond on graphitic edges as predicted by Lambrecht et al. [W. R. L. Lambrecht, C. H. Lee, B. Segall, J. C. Angus, Z. Li, and M. Sunkara, Nature, 364 607 (1993)] is experimentally confirmed. The results are discussed in terms of our recent subplantation-based diamond nucleation model

  16. Ultrastructural alterations in ciliary cells exposed to ionizing radiation. A scanning and transmission electron microscopic study

    Energy Technology Data Exchange (ETDEWEB)

    Baldetorp, L; Mecklenburg, C v; Haakansson, C H [Lund Univ. (Sweden). Hospital; Lund Univ. (Sweden). Dept. of Zoology)

    1977-01-01

    Early effects of ionizing radiation were investigated in an experimental in vitro system using the ciliary cells of the tracheal mucous membrane of the rabbit, irradiated at 30/sup 0/C and at more than 90% humidity. The changes in physiological activities of the ciliary cells caused by irradation were continously registered during the irradation. The specimens were examined immediately after irradiation electron microscopically. The morphological changes in irradiated material after 10-70 Gy are compared with normal material. After 40-70 Gy, scanning electron microscopy revealed the formation of vesicles on cilia, and club-like protrusions and adhesion of their tips. After 30-70 Gy, a swelling of mitochondrial membranes and cristae was apparent transmission electron microscopically. The membrane alterations caused by irradiation are assumed to disturb the permeability and flow of ATP from the mitochondria, which in turn leads to the recorded changes in the activity of the ciliated cells.

  17. Observations of localised dielectric excitations, secondary events and ionisation damage by scanning transmission electron microscopy

    International Nuclear Information System (INIS)

    Howie, A.

    1988-01-01

    In the scanning transmission electron microscope (STEM) a high intensity /approximately/0.5nm diameter, probe of 100 keV electrons is formed. This can be positioned to collect energy loss spectra from surfaces, interfaces, small spheres or other particles at controlled values of impact parameter or can be scanned across the object (usually a thin film) to produce high resolution images formed from a variety of signals - small angle or large angle (Z contrast) elastic scattering, inelastic scattering (both valence and core losses), secondary electron emission and x-ray or optical photon emission. The high spatial resolution achievable in a variety of simple structures raises many unsolved theoretical problems concerning the generation, propagation and decay of excitations in inhomogeneous media. These range from quite well posed problems in the mathematical physics of dielectric excitation to problems of plasmon propagation and rather more exotic and less well understood problems of radiation damage. 15 refs., 4 figs

  18. Imaging of soft and hard materials using a Boersch phase plate in a transmission electron microscope

    Energy Technology Data Exchange (ETDEWEB)

    Alloyeau, D., E-mail: alloyeau.damien@gmail.com [National Center for Electron Microscopy, Lawrence Berkeley National Laboratory, One Cyclotron Road, MS/72, Berkeley, CA 94720 (United States); Hsieh, W.K. [National Center for Electron Microscopy, Lawrence Berkeley National Laboratory, One Cyclotron Road, MS/72, Berkeley, CA 94720 (United States); Anderson, E.H.; Hilken, L. [Center for X-ray Optics, Lawrence Berkeley National Laboratory, Berkeley CA 94720 (United States); Benner, G. [Carl Zeiss NTS GmbH, Oberkochen 73447 (Germany); Meng, X. [Electrical Engineering and Computer Sciences, UC Berkeley, Berkeley, CA 94720-1770 (United States); Chen, F.R. [Department of Engineering and System Science, National Tsing Hua University, Hsinchu, Taiwan (China); Kisielowski, C. [National Center for Electron Microscopy, Lawrence Berkeley National Laboratory, One Cyclotron Road, MS/72, Berkeley, CA 94720 (United States)

    2010-04-15

    Using two levels of electron beam lithography, vapor phase deposition techniques, and FIB etching, we have fabricated an electrostatic Boersch phase plate for contrast enhancement of weak phase objects in a transmission electron microscope. The phase plate has suitable dimensions for the imaging of small biological samples without compromising the high-resolution capabilities of the microscope. A micro-structured electrode allows for phase tuning of the unscattered electron beam, which enables the recording of contrast enhanced in-focus images and in-line holograms. We have demonstrated experimentally that our phase plate improves the contrast of carbon nanotubes while maintaining high-resolution imaging performance, which is demonstrated for the case of an AlGaAs heterostructure. The development opens a new way to study interfaces between soft and hard materials.

  19. Experimental transmission electron microscopy studies and phenomenological model of bismuth-based superconducting compounds

    International Nuclear Information System (INIS)

    Elboussiri, Khalid

    1991-01-01

    The main part of this thesis is devoted to an experimental study by transmission electron microscopy of the different phases of the superconducting bismuth cuprates Bi_2Sr_2Ca_n_-_1Cu_nO_2_n_+_4. In high resolution electron microscopy, the two types of incommensurate modulation realized in these compounds have been observed. A model of structure has been proposed from which the simulated images obtained are consistent with observations. The medium resolution images correlated with the electron diffraction data have revealed existence of a multi-soliton regime with latent lock in phases of commensurate periods between 4b and 10b. At last, a description of different phases of these compounds as a result of superstructures from a disordered perovskite type structure is proposed (author) [fr

  20. Study of the nanostructure of Gum Metal using energy-filtered transmission electron microscopy

    International Nuclear Information System (INIS)

    Yano, T.; Murakami, Y.; Shindo, D.; Kuramoto, S.

    2009-01-01

    The nanostructure of Gum Metal, which has many anomalous mechanical properties, was investigated using transmission electron microscopy with energy filtering. A precise analysis of the weak diffuse electron scattering that was observed in the electron diffraction patterns of the Gum Metal specimen revealed that Gum Metal contains a substantial amount of the nanometer-sized ω phase. The morphology of the ω phase appeared to have a correlation with the faulting in the {2 1 1} planes, which are one of the characteristic lattice imperfections of the Gum Metal specimen. It is likely that the nanometer-sized ω phase may be a type of obstacle related to the restriction of the dislocation movement, which has been a significant problem in research on Gum Metal

  1. Probing plasmons in three dimensions by combining complementary spectroscopies in a scanning transmission electron microscope

    International Nuclear Information System (INIS)

    Hachtel, J A; Haglund, R F; Pantelides, S T; Marvinney, C; Mayo, D; Mouti, A; Lupini, A R; Chisholm, M F; Mu, R; Pennycook, S J

    2016-01-01

    The nanoscale optical response of surface plasmons in three-dimensional metallic nanostructures plays an important role in many nanotechnology applications, where precise spatial and spectral characteristics of plasmonic elements control device performance. Electron energy loss spectroscopy (EELS) and cathodoluminescence (CL) within a scanning transmission electron microscope have proven to be valuable tools for studying plasmonics at the nanoscale. Each technique has been used separately, producing three-dimensional reconstructions through tomography, often aided by simulations for complete characterization. Here we demonstrate that the complementary nature of the two techniques, namely that EELS probes beam-induced electronic excitations while CL probes radiative decay, allows us to directly obtain a spatially- and spectrally-resolved picture of the plasmonic characteristics of nanostructures in three dimensions. The approach enables nanoparticle-by-nanoparticle plasmonic analysis in three dimensions to aid in the design of diverse nanoplasmonic applications. (paper)

  2. Dynamical observation of lithium insertion/extraction reaction during charge-discharge processes in Li-ion batteries by in situ spatially resolved electron energy-loss spectroscopy.

    Science.gov (United States)

    Shimoyamada, Atsushi; Yamamoto, Kazuo; Yoshida, Ryuji; Kato, Takehisa; Iriyama, Yasutoshi; Hirayama, Tsukasa

    2015-12-01

    All-solid-state Li-ion batteries (LIBs) with solid electrolytes are expected to be the next generation devices to overcome serious issues facing conventional LIBs with liquid electrolytes. However, the large Li-ion transfer resistance at the electrode/solid-electrolyte interfaces causes low power density and prevents practical use. In-situ-formed negative electrodes prepared by decomposing the solid electrolyte Li(1+x+3z)Alx(Ti,Ge)(2-x)Si(3z)P(3-z)O12 (LASGTP) with an excess Li-ion insertion reaction are effective electrodes providing low Li-ion transfer resistance at the interfaces. Prior to our work, however, it had still been unclear how the negative electrodes were formed in the parent solid electrolytes. Here, we succeeded in dynamically visualizing the formation by in situ spatially resolved electron energy-loss spectroscopy in a transmission electron microscope mode (SR-TEM-EELS). The Li-ions were gradually inserted into the solid electrolyte region around 400 nm from the negative current-collector/solid-electrolyte interface in the charge process. Some of the ions were then extracted in the discharge process, and the rest were diffused such that the distribution was almost flat, resulting in the negative electrodes. The redox reaction of Ti(4+)/Ti(3+) in the solid electrolyte was also observed in situ during the Li insertion/extraction processes. The in situ SR-TEM-EELS revealed the mechanism of the electrochemical reaction in solid-state batteries. © The Author 2015. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

  3. Elemental distribution imaging by energy-filtering transmission electron microscopy (EFTEM) and its applications

    International Nuclear Information System (INIS)

    Kurata, Hiroki

    1996-01-01

    EFTEM is new microscopy with the object of visualizing high resolution quantitative elemental distribution. The measurement principles and the present state of EFTEM studies are explained by the examples of measurement of the elemental distributions. EFTEM is a combination of the transmission electron microscope with the electron energy loss spectroscopy (EFLS). EFTEM method sets the slit in the specific energy field and put the electron passing the slit back in the microscopic image. The qualitative elemental analysis is obtained by observing the position of the absorption end of core electronic excitation spectrum and the quantitative one by determining the core electronic excitation strength of the specific atom depend on filtering with energy selector slit. The binding state and the local structure in the neighborhood of excited atom is determined by the fine structure of absorption end. By the chemical mapping method, the distribution image of chemical binding state is visualized by the imaging chemical map obtained by filtering the specific peak strength of fine structure with the narrow energy selector slit. The fine powder of lead chromate (PbCrO 4 ) covered with silica glass was shown as a typical example of the elemental distribution image of core electronic excitation spectrum. The quantitative analysis method of elemental distribution image is explained. The possibility of single atom analysis at nanometer was shown by the example of nanotube observed by EFTEM. (S.Y.)

  4. Practical considerations for high spatial and temporal resolution dynamic transmission electron microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Armstrong, Michael R. [Materials Science and Technology Division, Chemistry and Materials Science Directorate, Lawrence Livermore National Laboratory, P.O. Box 808, L-356, Livermore, CA 94550 (United States)], E-mail: armstrong30@llnl.gov; Boyden, Ken [Materials Science and Technology Division, Chemistry and Materials Science Directorate, Lawrence Livermore National Laboratory, P.O. Box 808, L-356, Livermore, CA 94550 (United States); Browning, Nigel D. [Materials Science and Technology Division, Chemistry and Materials Science Directorate, Lawrence Livermore National Laboratory, P.O. Box 808, L-356, Livermore, CA 94550 (United States); Department of Chemical Engineering and Materials Science, University of California-Davis, One Shields Avenue, Davis, CA 95616 (United States); Campbell, Geoffrey H.; Colvin, Jeffrey D.; De Hope, William J.; Frank, Alan M. [Materials Science and Technology Division, Chemistry and Materials Science Directorate, Lawrence Livermore National Laboratory, P.O. Box 808, L-356, Livermore, CA 94550 (United States); Gibson, David J.; Hartemann, Fred [N Division, Physics and Advanced Technologies Directorate, Lawrence Livermore National Laboratory, P.O. Box 808, L-280, Livermore, CA 94550 (United States); Kim, Judy S. [Materials Science and Technology Division, Chemistry and Materials Science Directorate, Lawrence Livermore National Laboratory, P.O. Box 808, L-356, Livermore, CA 94550 (United States); Department of Chemical Engineering and Materials Science, University of California-Davis, One Shields Avenue, Davis, CA 95616 (United States); King, Wayne E.; La Grange, Thomas B.; Pyke, Ben J.; Reed, Bryan W.; Shuttlesworth, Richard M.; Stuart, Brent C.; Torralva, Ben R. [Materials Science and Technology Division, Chemistry and Materials Science Directorate, Lawrence Livermore National Laboratory, P.O. Box 808, L-356, Livermore, CA 94550 (United States)

    2007-04-15

    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 5x10{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. Practical considerations for high spatial and temporal resolution dynamic transmission electron microscopy

    International Nuclear Information System (INIS)

    Armstrong, Michael R.; Boyden, Ken; Browning, Nigel D.; Campbell, Geoffrey H.; Colvin, Jeffrey D.; De Hope, William J.; Frank, Alan M.; Gibson, David J.; Hartemann, Fred; Kim, Judy S.; King, Wayne E.; La Grange, Thomas B.; Pyke, Ben J.; Reed, Bryan W.; Shuttlesworth, Richard M.; Stuart, Brent C.; Torralva, Ben R.

    2007-01-01

    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 5x10 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 -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

  6. In situ electron backscatter diffraction investigation of recrystallization in a copper wire.

    Science.gov (United States)

    Brisset, François; Helbert, Anne-Laure; Baudin, Thierry

    2013-08-01

    The microstructural evolution of a cold drawn copper wire (reduction area of 38%) during primary recrystallization and grain growth was observed in situ by electron backscatter diffraction. Two thermal treatments were performed, and successive scans were acquired on samples undergoing heating from ambient temperature to a steady state of 200°C or 215°C. During a third in situ annealing, the temperature was continuously increased up to 600°C. Nuclei were observed to grow at the expense of the deformed microstructure. This growth was enhanced by the high stored energy difference between the nuclei and their neighbors (driving energy in recrystallization) and by the presence of high-angle grain boundaries of high mobility. In the early stages of growth, the nuclei twin and the newly created orientations continue to grow to the detriment of the strained copper. At high temperatures, the disappearance of some twins was evidenced by the migration of the incoherent twin boundaries. Thermal grooving of grain boundaries is observed at these high temperatures and affects the high mobile boundaries but tends to preserve the twin boundaries of lower energy. Thus, grooving may contribute to the twin vanishing.

  7. In situ growth optimization in focused electron-beam induced deposition

    Directory of Open Access Journals (Sweden)

    Paul M. Weirich

    2013-12-01

    Full Text Available We present the application of an evolutionary genetic algorithm for the in situ optimization of nanostructures that are prepared by focused electron-beam-induced deposition (FEBID. It allows us to tune the properties of the deposits towards the highest conductivity by using the time gradient of the measured in situ rate of change of conductance as the fitness parameter for the algorithm. The effectiveness of the procedure is presented for the precursor W(CO6 as well as for post-treatment of Pt–C deposits, which were obtained by the dissociation of MeCpPt(Me3. For W(CO6-based structures an increase of conductivity by one order of magnitude can be achieved, whereas the effect for MeCpPt(Me3 is largely suppressed. The presented technique can be applied to all beam-induced deposition processes and has great potential for a further optimization or tuning of parameters for nanostructures that are prepared by FEBID or related techniques.

  8. 3D simulation of electron and ion transmission of GEM-based detectors

    Science.gov (United States)

    Bhattacharya, Purba; Mohanty, Bedangadas; Mukhopadhyay, Supratik; Majumdar, Nayana; da Luz, Hugo Natal

    2017-10-01

    Time Projection Chamber (TPC) has been chosen as the main tracking system in several high-flux and high repetition rate experiments. These include on-going experiments such as ALICE and future experiments such as PANDA at FAIR and ILC. Different R&D activities were carried out on the adoption of Gas Electron Multiplier (GEM) as the gas amplification stage of the ALICE-TPC upgrade version. The requirement of low ion feedback has been established through these activities. Low ion feedback minimizes distortions due to space charge and maintains the necessary values of detector gain and energy resolution. In the present work, Garfield simulation framework has been used to study the related physical processes occurring within single, triple and quadruple GEM detectors. Ion backflow and electron transmission of quadruple GEMs, made up of foils with different hole pitch under different electromagnetic field configurations (the projected solutions for the ALICE TPC) have been studied. Finally a new triple GEM detector configuration with low ion backflow fraction and good electron transmission properties has been proposed as a simpler GEM-based alternative suitable for TPCs for future collider experiments.

  9. Validities of three multislice algorithms for quantitative low-energy transmission electron microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Ming, W.Q.; Chen, J.H., E-mail: jhchen123@hnu.edu.cn

    2013-11-15

    Three different types of multislice algorithms, namely the conventional multislice (CMS) algorithm, the propagator-corrected multislice (PCMS) algorithm and the fully-corrected multislice (FCMS) algorithm, have been evaluated in comparison with respect to the accelerating voltages in transmission electron microscopy. Detailed numerical calculations have been performed to test their validities. The results show that the three algorithms are equivalent for accelerating voltage above 100 kV. However, below 100 kV, the CMS algorithm will introduce significant errors, not only for higher-order Laue zone (HOLZ) reflections but also for zero-order Laue zone (ZOLZ) reflections. The differences between the PCMS and FCMS algorithms are negligible and mainly appear in HOLZ reflections. Nonetheless, when the accelerating voltage is further lowered to 20 kV or below, the PCMS algorithm will also yield results deviating from the FCMS results. The present study demonstrates that the propagation of the electron wave from one slice to the next slice is actually cross-correlated with the crystal potential in a complex manner, such that when the accelerating voltage is lowered to 10 kV, the accuracy of the algorithms is dependent of the scattering power of the specimen. - Highlights: • Three multislice algorithms for low-energy transmission electron microscopy are evaluated. • The propagator-corrected algorithm is a good alternative for voltages down to 20 kV. • Below 20 kV, a fully-corrected algorithm has to be employed for quantitative simulations.

  10. Validities of three multislice algorithms for quantitative low-energy transmission electron microscopy

    International Nuclear Information System (INIS)

    Ming, W.Q.; Chen, J.H.

    2013-01-01

    Three different types of multislice algorithms, namely the conventional multislice (CMS) algorithm, the propagator-corrected multislice (PCMS) algorithm and the fully-corrected multislice (FCMS) algorithm, have been evaluated in comparison with respect to the accelerating voltages in transmission electron microscopy. Detailed numerical calculations have been performed to test their validities. The results show that the three algorithms are equivalent for accelerating voltage above 100 kV. However, below 100 kV, the CMS algorithm will introduce significant errors, not only for higher-order Laue zone (HOLZ) reflections but also for zero-order Laue zone (ZOLZ) reflections. The differences between the PCMS and FCMS algorithms are negligible and mainly appear in HOLZ reflections. Nonetheless, when the accelerating voltage is further lowered to 20 kV or below, the PCMS algorithm will also yield results deviating from the FCMS results. The present study demonstrates that the propagation of the electron wave from one slice to the next slice is actually cross-correlated with the crystal potential in a complex manner, such that when the accelerating voltage is lowered to 10 kV, the accuracy of the algorithms is dependent of the scattering power of the specimen. - Highlights: • Three multislice algorithms for low-energy transmission electron microscopy are evaluated. • The propagator-corrected algorithm is a good alternative for voltages down to 20 kV. • Below 20 kV, a fully-corrected algorithm has to be employed for quantitative simulations

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

    NARCIS (Netherlands)

    Hendriks, Frank C.|info:eu-repo/dai/nl/412642697; Mohammadian, Sajjad|info:eu-repo/dai/nl/374721327; Ristanovic, Zoran|info:eu-repo/dai/nl/328233005; Kalirai, Samanbir; Meirer, Florian; Vogt, Eelco T. C.|info:eu-repo/dai/nl/073717398; Bruijnincx, Pieter C. A.|info:eu-repo/dai/nl/33799529X; Gerritsen, Hans|info:eu-repo/dai/nl/071548777; Weckhuysen, Bert M.|info:eu-repo/dai/nl/285484397

    2018-01-01

    Establishing structure–activity relationships in complex, hierarchically structured nanomaterials, such as fluid catalytic cracking (FCC) catalysts, requires characterization with complementary, correlated analysis techniques. An integrated setup has been developed to perform transmission electron

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

    International Nuclear Information System (INIS)

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

    2013-01-01

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

  13. Photoinduced electron transfer to fullerene C70 (An in situ EPR study)

    International Nuclear Information System (INIS)

    Brezova, V.; Dvoranova, D.; Kostova, B.; Stasko, A.

    1999-01-01

    The photoexcitation of fullerene C 70 by monochromatic light (λ = 546 nm) in the presence of electron donating substrate 3,3',5,5'-tetramethyl-benzidine (TMB) resulted in the charge-transfer, quenching the fullerene triplet state and forming corresponding C 70 anion-radicals. Analogously to the photo-reduction of C 60 , two EPR signal were observed upon in situ irradiation in the cavity of EPR spectrometer. EPR singlet A characterized by g-value, g A = 2.0009 and peak-to-peak line-width, pp A = 0.013 mT was assigned to the C 70 mono-anion. Signal B (g B = 2.0011; pp B = 0.011 mT) was tentatively attributed to the C 70 di-anion or to the associated forms of mono-anions. The stabilization of photo-generated anion-radicals significantly depends on solvent polarity. (authors)

  14. In Situ Characterization of Inconel 718 Post-Dynamic Recrystallization within a Scanning Electron Microscope

    Directory of Open Access Journals (Sweden)

    Meriem Zouari

    2017-11-01

    Full Text Available Microstructure evolution within the post-dynamic regime following hot deformation was investigated in Inconel 718 samples with different dynamically recrystallized volume fractions and under conditions such that no δ-phase particles were present. In situ annealing treatments carried out to mimic post-dynamic conditions inside the Scanning Electron Microscope (SEM chamber suggest the occurrence of both metadynamic and static recrystallization mechanisms. Static recrystallization was observed in addition to metadynamic recrystallization, only when the initial dynamically recrystallized volume fraction was very small. The initial volume fraction of dynamically recrystallized grains appears to be decisive for subsequent microstructural evolution mechanisms and kinetics. In addition, the formation of annealing twins is observed along with the growth of recrystallized grains, but then the twin density decreases as the material enters the capillarity-driven grain growth regime.

  15. In-situ Indentation and Correlated Precession Electron Diffraction Analysis of a Polycrystalline Cu Thin Film

    Science.gov (United States)

    Guo, Qianying; Thompson, Gregory B.

    2018-04-01

    In-situ TEM nanoindentation of a polycrystalline Cu film was cross-correlated with precession electron diffraction (PED) to quantify the microstructural evolution. The use of PED is shown to clearly reveal features, such as grain size, that are easily masked by diffraction contrast created by the deformation. Using PED, the accompanying grain refinement and change in texture as well as the preservation of specific grain boundary structures, including a ∑3 boundary, under the indent impression were quantified. The nucleation of dislocations, evident in low-angle grain boundary formations, was also observed under the indent. PED quantification of texture gradients created by the indentation process linked well to bend contours observed in the bright-field images. Finally, PED enabled generating a local orientation spread map that gave an approximate estimation of the spatial distribution of strain created by the indentation impression.

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

    Science.gov (United States)

    Rodríguez, L A; Magén, C; Snoeck, E; Gatel, C; Marín, L; Serrano-Ramón, L; Prieto, J L; Muñoz, M; Algarabel, P A; Morellon, L; De Teresa, J M; Ibarra, M R

    2013-11-01

    A generalized procedure for the in situ application of magnetic fields by means of the excitation of the objective lens for magnetic imaging experiments in Lorentz microscopy and electron holography is quantitatively described. A protocol for applying magnetic fields with arbitrary in-plane magnitude and orientation is presented, and a freeware script for Digital Micrograph(™) is provided to assist the operation of the microscope. Moreover, a method to accurately reconstruct hysteresis loops is detailed. We show that the out-of-plane component of the magnetic field cannot be always neglected when performing quantitative measurements of the local magnetization. Several examples are shown to demonstrate the accuracy and functionality of the methods. © 2013 Elsevier B.V. All rights reserved.

  17. An ion-sputtering gun to clean crystal surfaces in-situ in an ultra-high-vacuum electron microscope

    International Nuclear Information System (INIS)

    Morita, Etsuo; Takayanagi, Kunio; Kobayashi, Kunio; Yagi, Katsumichi; Honjo, Goro

    1980-01-01

    The design and performance of an ion-sputtering gun for cleaning crystal surfaces in-situ in an ultra-high-vacuum electron microscope are reported. The electron microscopic aspects of ion-bombardment damage to ionic magnesium oxide, covalent germanium and silicon, and metallic gold and copper crystals, and the effects of annealing after and during sputtering are described. The growth of various kinds of films deposited in-situ on crystals cleaned by ion-sputtering are described and discussed. (author)

  18. Transmission electron microscopy characterization of microstructural features in aluminum-lithium-copper alloys

    Science.gov (United States)

    Avalos-Borja, M.; Larson, L. A.; Pizzo, P. P.

    1984-01-01

    A transmission electron microscopy (TEM) examination of aluminum-lithium-copper alloys was conducted. The principal purpose is to characterize the nature, size, and distribution of stringer particles which result from the powder metallurgy (P/M) processing of these alloys. Microstructural features associated with the stringer particles are reported that help explain the stress corrosion susceptibility of the powder metallurgy-processed Al-Li-Cu alloys. In addition, matrix precipitaton events are documented for a variety of heat treatments and process variations. Hot rolling is observed to significantly alter the nature of matrix precipitation, and the observations are correlated with concomitant mechanical property variations.

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

    Science.gov (United States)

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

    2015-11-01

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

  20. Transmission Electron Microscopy Specimen Preparation Method for Multiphase Porous Functional Ceramics

    DEFF Research Database (Denmark)

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

    2013-01-01

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

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

    DEFF Research Database (Denmark)

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

    2013-01-01

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

  2. Dynamics of annular bright field imaging in scanning transmission electron microscopy

    International Nuclear Information System (INIS)

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

    2010-01-01

    We explore the dynamics of image formation in the so-called annular bright field mode in scanning transmission electron microscopy, whereby an annular detector is used with detector collection range lying within the cone of illumination, i.e. the bright field region. We show that this imaging mode allows us to reliably image both light and heavy columns over a range of thickness and defocus values, and we explain the contrast mechanisms involved. The role of probe and detector aperture sizes is considered, as is the sensitivity of the method to intercolumn spacing and local disorder.

  3. Transmission electron microscopy study of vertical quantum dots molecules grown by droplet epitaxy

    Energy Technology Data Exchange (ETDEWEB)

    Hernandez-Maldonado, D., E-mail: david.hernandez@uca.es [Departamento de Ciencia de los Materiales e I.M. y Q.I., Facultad de Ciencias, Universidad de Cadiz, Campus Rio San Pedro, s/n, 11510 Puerto Real, Cadiz (Spain); Herrera, M.; Sales, D.L. [Departamento de Ciencia de los Materiales e I.M. y Q.I., Facultad de Ciencias, Universidad de Cadiz, Campus Rio San Pedro, s/n, 11510 Puerto Real, Cadiz (Spain); Alonso-Gonzalez, P.; Gonzalez, Y.; Gonzalez, L. [Instituto de Microelectronica de Madrid (CNM-CSIC), Isaac Newton 8 (PTM), 28760 Tres Cantos, Madrid (Spain); Pizarro, J.; Galindo, P.L. [Departamento de Lenguajes y Sistemas Informaticos, CASEM, Universidad de Cadiz, Campus Rio San Pedro, s/n, 11510 Puerto Real, Cadiz (Spain); Molina, S.I. [Departamento de Ciencia de los Materiales e I.M. y Q.I., Facultad de Ciencias, Universidad de Cadiz, Campus Rio San Pedro, s/n, 11510 Puerto Real, Cadiz (Spain)

    2010-07-01

    The compositional distribution of InAs quantum dots grown by molecular beam epitaxy on GaAs capped InAs quantum dots has been studied in this work. Upper quantum dots are nucleated preferentially on top of the quantum dots underneath, which have been nucleated by droplet epitaxy. The growth process of these nanostructures, which are usually called as quantum dots molecules, has been explained. In order to understand this growth process, the analysis of the strain has been carried out from a 3D model of the nanostructure built from transmission electron microscopy images sensitive to the composition.

  4. Single particle analysis based on Zernike phase contrast transmission electron microscopy.

    Science.gov (United States)

    Danev, Radostin; Nagayama, Kuniaki

    2008-02-01

    We present the first application of Zernike phase-contrast transmission electron microscopy to single-particle 3D reconstruction of a protein, using GroEL chaperonin as the test specimen. We evaluated the performance of the technique by comparing 3D models derived from Zernike phase contrast imaging, with models from conventional underfocus phase contrast imaging. The same resolution, about 12A, was achieved by both imaging methods. The reconstruction based on Zernike phase contrast data required about 30% fewer particles. The advantages and prospects of each technique are discussed.

  5. Transmission electron microscopy studies on nanometer-sized ω phase produced in Gum Metal

    International Nuclear Information System (INIS)

    Yano, Takaaki; Murakami, Yasukazu; Shindo, Daisuke; Hayasaka, Yuichiro; Kuramoto, Shigeru

    2010-01-01

    The morphology, numerical density and average spacing of the ω phase formed in Gum Metal, a Ti-based alloy showing unique mechanical properties, were studied by transmission electron microscopy. Based on dark-field image observations and precise thickness measurements using a thin-foil specimen, the average spacing of the nanometer-sized ω phase was determined to be 6 nm. This spacing appeared to be sufficiently small for trapping dislocations. The results are discussed in conjunction with the dislocation-free deformation mechanism proposed for Gum Metal.

  6. Transmission electron microscopy study of vertical quantum dots molecules grown by droplet epitaxy

    International Nuclear Information System (INIS)

    Hernandez-Maldonado, D.; Herrera, M.; Sales, D.L.; Alonso-Gonzalez, P.; Gonzalez, Y.; Gonzalez, L.; Pizarro, J.; Galindo, P.L.; Molina, S.I.

    2010-01-01

    The compositional distribution of InAs quantum dots grown by molecular beam epitaxy on GaAs capped InAs quantum dots has been studied in this work. Upper quantum dots are nucleated preferentially on top of the quantum dots underneath, which have been nucleated by droplet epitaxy. The growth process of these nanostructures, which are usually called as quantum dots molecules, has been explained. In order to understand this growth process, the analysis of the strain has been carried out from a 3D model of the nanostructure built from transmission electron microscopy images sensitive to the composition.

  7. Preparation of high-quality ultrathin transmission electron microscopy specimens of a nanocrystalline metallic powder.

    Science.gov (United States)

    Riedl, Thomas; Gemming, Thomas; Mickel, Christine; Eymann, Konrad; Kirchner, Alexander; Kieback, Bernd

    2012-06-01

    This article explores the achievable transmission electron microscopy specimen thickness and quality by using three different preparation methods in the case of a high-strength nanocrystalline Cu-Nb powder alloy. Low specimen thickness is essential for spatially resolved analyses of the grains in nanocrystalline materials. We have found that single-sided as well as double-sided low-angle Ar ion milling of the Cu-Nb powders embedded into epoxy resin produced wedge-shaped particles of very low thickness (coating on the sections consisting of epoxy deployed as the embedding material and considerable nanoscale thickness variations. Copyright © 2011 Wiley Periodicals, Inc.

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

    Directory of Open Access Journals (Sweden)

    Annette Meister

    2017-10-01

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

  9. High-resolution transmission electron microscopy and energetics of flattened carbon nonoshells

    International Nuclear Information System (INIS)

    Bourgeois, L.N.; Bursill, L.A.

    1998-01-01

    When examined under a high-resolution transmission electron microscope, carbon soot produced alongside buckytubes in an arc-discharge is found to contain a small percentage of flattened carbon shells. These objects are shown to be small graphite flakes which eliminated their dangling bonds by terminating their edges with highly curved junctions. Ideal models for these structures are presented, and their energy estimated. The calculations show that the establishment of highly curved junctions is energetically favourable for a graphite flake in an inert atmosphere. Flattened shells also appear more stable than their 'inflated' counterparts (fullerene 'onions' and buckytubes) when the shell dimensions obey specific criteria.(authors)

  10. Simulation calculation for the energy deposition profile and the transmission fraction of intense pulsed electron beam at various incident angles

    International Nuclear Information System (INIS)

    Yang Hailiang; Qiu Aici; Zhang Jiasheng; Huang Jianjun; Sun Jianfeng

    2002-01-01

    The incident angles have a heavy effect on the intense pulsed electron beam energy deposition profile, energy deposition fraction and beam current transmission fraction in material. The author presents electron beam energy deposition profile and energy deposition fraction versus electron energy (0.5-2.0 MeV), at various incident angles for three aluminum targets of various thickness via theoretical calculation. The intense pulsed electron beam current transmission fractions versus electron energy (0.4-1.4 MeV) at various incident angles for three thickness of carbon targets were also theoretically calculated. The calculation results indicate that the deposition energy in unit mass of material surface layer increase with the rise of electron beam incident angle, and electron beam with low incident angle (closer to normal incident angle) penetrates deeper into the target material. The electron beams deposit more energy in unit mass of material surface layer at 60 degree-70 degree incident angle

  11. Two-dimensional electron flow in pulsed power transmission lines and plasma opening switches

    International Nuclear Information System (INIS)

    Church, B.W.; Longcope, D.W.; Ng, C.K.; Sudan, R.N.

    1991-01-01

    The operation of magnetically insulated transmission lines (MITL) and the interruption of current in a plasma opening switch (POS) are determined by the physics of the electrons emitted by the cathode surface. A mathematical model describes the self-consistent two-dimensional flow of an electron fluid. A finite element code, FERUS, has been developed to solve the two equations which describe Poisson's and Ampere's law in two dimensions. The solutions from this code are obtained for parameters where the electron orbits are considerably modified by the self-magnetic field of the current. Next, the self-insulated electron flow in a MITL with a step change in cross-section is studied using a conventional two-dimensional fully electromagnetic particle-in-cell code, MASK. The equations governing two-dimensional quasi-static electron flow are solved numerically by a third technique which is suitable for predicting current interruption in a POS. The object of the study is to determine the critical load impedance, Z CL , required for current interruption for a given applied voltage, cathode voltage and plasma length. (author). 9 refs, 5 figs

  12. Direct characterization of phase transformations and morphologies in moving reaction zones in Al/Ni nanolaminates using dynamic transmission electron microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Kim, J.S., E-mail: judy.kim@materials.ox.ac.uk [Condensed Matter and Materials Division, Lawrence Livermore National Laboratory, 7000 East Avenue, Livermore, CA 94550 (United States); Chemical Engineering and Materials Science/Molecular and Cellular Biology, University of California-Davis, 1 Shields Avenue, Davis, CA 95616 (United States); LaGrange, T.; Reed, B.W. [Condensed Matter and Materials Division, Lawrence Livermore National Laboratory, 7000 East Avenue, Livermore, CA 94550 (United States); Knepper, R.; Weihs, T.P. [Department of Materials Science and Engineering, Johns Hopkins University, 3400 N. Charles St., Baltimore, MD 21218 (United States); Browning, N.D. [Condensed Matter and Materials Division, Lawrence Livermore National Laboratory, 7000 East Avenue, Livermore, CA 94550 (United States); Chemical Engineering and Materials Science/Molecular and Cellular Biology, University of California-Davis, 1 Shields Avenue, Davis, CA 95616 (United States); Campbell, G.H. [Condensed Matter and Materials Division, Lawrence Livermore National Laboratory, 7000 East Avenue, Livermore, CA 94550 (United States)

    2011-05-15

    Highlights: > Fast phase transformations are examined in Al/Ni reactive nanolaminates. > Results visible only by dynamic transmission electron microscopy at ns resolution. > NiAl forms under 15 ns after reaction front in all three stoichiometries studied. > DTEM imaging reveals a transient cellular morphology in nonequiatomic films. - Abstract: Phase transformations and transient morphologies are examined as exothermic formation reactions self-propagate across Al/Ni nanolaminate films. The rapid evolution of these phases and sub-micrometer morphological features requires nanoscale temporal and spatial resolution that is not available with traditional in situ electron microscopy. This work uses dynamic transmission electron microscopy to identify intermetallic products and phase morphologies, as exothermic formation reactions self-propagate in nanolaminate films grown with 3:2, 2:3 and 1:1 Al/Ni atomic ratios. Single-shot diffraction patterns with 15 ns temporal resolution reveal that the NiAl intermetallic forms within {approx}15 ns of the reaction front's arrival in all three types of films and is the only intermetallic phase to form, as the reactions self-propagate and quench very rapidly. Time-resolved imaging reveals a transient cellular morphology in the Al-rich and Ni-rich foils, but not in the equiatomic films. The cellular features in the Al-rich and Ni-rich films are attributed to a cooling trajectory through a two-phase field of liquid + NiAl.

  13. The use of transmission electron microscopy in the quantification of nanoparticle dose

    International Nuclear Information System (INIS)

    Hondow, N; Brydson, R; Brown, A

    2014-01-01

    There are an increasing number of potential applications for nanoparticles in clinical medicine, including targeted drug delivery and contrast agents for biomedical imaging. Current in vitro studies are concerned with the biological impact of nanoparticles, with electron microscopy commonly employed to image their intracellular location. It is critical to quantify the absolute nanoparticle dose internalized by cells in a given exposure, and to understand the factors which affect this. In this work we are aiming to develop a full quantitative description of quantum dot uptake by an in vitro cell line. Transmission electron microscopy of thin cell sections provides the location and number of cellular vesicles per 2-D cell slice plus the number of quantum dots per vesicle. These results can then be correlated to other techniques to quantify the internalized nanoparticle dose distribution for whole cells

  14. Cross-section transmission electron microscopy of the ion implantation damage in annealed diamond

    Energy Technology Data Exchange (ETDEWEB)

    Derry, T.E. [DST/NRF Centre of Excellence in Strong Materials and School of Physics, University of the Witwatersrand, Wits 2050, Johannesburg (South Africa)], E-mail: Trevor.Derry@wits.ac.za; Nshingabigwi, E.K. [DST/NRF Centre of Excellence in Strong Materials and School of Physics, University of the Witwatersrand, Wits 2050, Johannesburg (South Africa); Department of Physics, National University of Rwanda, P.O. Box 117, Huye (Rwanda); Levitt, M. [DST/NRF Centre of Excellence in Strong Materials and School of Physics, University of the Witwatersrand, Wits 2050, Johannesburg (South Africa); Neethling, J. [DST/NRF CoE-SM and Physics Department, Nelson Mandela Metropolitan University, Port Elizabeth (South Africa); Naidoo, S.R. [DST/NRF Centre of Excellence in Strong Materials and School of Physics, University of the Witwatersrand, Wits 2050, Johannesburg (South Africa)

    2009-08-15

    It has formerly been shown that low-damage levels, produced during the implantation doping of diamond as a semiconductor, anneal easily while high levels 'graphitize' (above about 5.2 x 10{sup 15} ions/cm{sup 2}). The difference in the defect types and their profiles, in the two cases, has never been directly observed. We have succeeded in using cross-section transmission electron microscopy to do so. The experiments were difficult because the specimens must be polished to {approx}40 {mu}m thickness, then implanted on edge and annealed, before final ion beam thinning to electron transparency. The low-damage micrographs reveal some deeply penetrating dislocations, whose existence had been predicted in earlier work.

  15. Transmission electron microscope study of neutron irradiation-induced defects in silicon

    International Nuclear Information System (INIS)

    Oshima, Ryuichiro; Kawano, Tetsuya; Fujimoto, Ryoji

    1994-01-01

    Commercial Czochralski-grown silicon (Cz-Si) and float-zone silicon (Fz-Si) wafers were irradiated with fission neutrons at various fluences from 10 19 to 10 22 n/cm 2 at temperatures ranging from 473 K to 1043 K. The irradiation induced defect structures were examined by transmission electron microscopy and ultra high voltage electron microscopy, which were compared with Marlowe code computer simulation results. It was concluded that the vacancy-type damage structure formed at 473 K were initiated from collapse of vacancy-rich regions of cascades, while interstitial type defect clusters formed by irradiation above 673 K were associated with interstitial oxygen atoms and free interstitials which diffused out of the cascades. Complex defect structures were identified to consist of {113} and {111} planar faults by the parallel beam illumination diffraction analysis. (author)

  16. Transmission Electron Microscopy for Wood and Fiber Analysis − A Review

    Directory of Open Access Journals (Sweden)

    Mehedi Reza

    2015-07-01

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

  17. Dynamics of Supported Metal Nanoparticles Observed in a CS Corrected Environmental Transmission Electron Microscope

    DEFF Research Database (Denmark)

    Hansen, Thomas Willum; Dunin-Borkowski, Rafal E.; Wagner, Jakob Birkedal

    resulting in the formation of larger particles and a loss of catalytic performance. Several models of sintering in different systems have been put forward [1,2]. However, most investigations have been post mortem studies, revealing only the final state of the catalyst. Transmission electron microscopy (TEM....... The combined capabilities of ETEM and image CS correction provide unique possibilities to study this relationship. However, in order to fully quantify image contrast from such experiments, a deeper understanding of the scattering of fast electrons in the presence of gas molecules in the pole piece gap...... of the microscope is needed. As industrial catalysts are usually complex high surface area materials, they are often not suited for fundamental studies. For this purpose, model systems consisting of gold nanoparticles on sheets of low surface area boron nitride and graphite supports were produced. Sheets...

  18. Long distance electron transmission couples sulphur, iron, calcium and oxygen cycling in marine sediment

    DEFF Research Database (Denmark)

    Risgaard-Petersen, Nils; Nielsen, Lars Peter

    sulfide oxidation leads to electric field formation, sulfide depletion and acidification of the upper centimeters of the sediment. This promoted ion migration and dissolution of carbonates and iron sulfides. Sulfide released from iron sulfides was the major e-donor in the system. Ferrous iron released...... from iron sulfides was to a large extend deposited in the oxic zone as iron oxides and Ca2+ eventually precipitates at the surface as due to high pH caused by cathodic oxygen reduction. The result show how long distance electron transmission allows oxygen to drive the allocation of important minerals...... geochemical alterations in the upper centimetres of the anoxic sediment: Sulphides were oxidized to sulphate in anoxic sediment layers. Electrons from this half-reaction were passed to the oxic layers cm above. In this way the domain of oxygen was extended far beyond it’s physically presence. Bioelectrical...

  19. Power electron beam front shortening in magnetically insulated transmission line with inner coaxial dielectric insert

    International Nuclear Information System (INIS)

    Galstjan, E.A.; Kazanskiy, L.N.

    1995-01-01

    By now the technology of high-power high-current relativistic electron beams with microsecond duration has been developed. The same technology is used in high-power electric pulse generation. However at present the high-power beams of subnanosecond duration are necessary for some investigations and applications. The maximum power parameter achieved by means of the usual technology is limited by a value in the range of 100-300 MW. For this reason a search for new ways to generate high-power REB (relativistic electron beam) is a topical problem. It is obvious that this problem may be reduced to the generation of pulses with a subnanosecond front duration. There are many methods to shorten a pulse duration to its front duration for instance, by using parts of short-circuited transmission lines

  20. Optical depth sectioning in the aberration-corrected scanning transmission and scanning confocal electron microscope

    International Nuclear Information System (INIS)

    Behan, G; Nellist, P D

    2008-01-01

    The use of spherical aberration correctors in the scanning transmission electron microscope (STEM) has the effect of reducing the depth of field of the microscope, making three-dimensional imaging of a specimen possible by optical sectioning. Depth resolution can be improved further by placing aberration correctors and lenses pre and post specimen to achieve an imaging mode known as scanning confocal electron microscopy (SCEM). We present the calculated incoherent point spread functions (PSF) and optical transfer functions (OTF) of a STEM and SCEM. The OTF for a STEM is shown to have a missing cone region which results in severe blurring along the optic axis, which can be especially severe for extended objects. We also present strategies for reconstruction of experimental data, such as three-dimensional deconvolution of the point spread function.