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Sample records for situ transmission electron

  1. 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...

  2. 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....

  3. 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.

  4. 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.

  5. 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

  6. 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...

  7. 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.

  8. 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)

  9. 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

  10. 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

  11. 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

  12. 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

  13. 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.

  14. 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

  15. 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

  16. 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...

  17. 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...

  18. 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]....

  19. 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

  20. 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...

  1. 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.

  2. 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.

  3. 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.

  4. 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

  5. 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.

  6. 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.

  7. 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.)

  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. 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.

  10. 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....

  11. 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.

  12. 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)

  13. 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

  14. 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

  15. 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.

  16. 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.

  17. 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.

  18. 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.

  19. 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.

  20. 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

  1. 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.

  2. 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)

  3. 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.

  4. 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.

  5. 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.

  6. 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.

  7. 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

  8. 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.

  9. 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

  10. 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

  11. 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.

  12. 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.

  13. 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.

  14. 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.

  15. 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.

  16. 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.

  17. 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

  18. 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

  19. 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.

  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. 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)

  2. 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.

  3. 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.

  4. 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

  5. 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...

  6. 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)

  7. 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.

  8. 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.

  9. 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

  10. 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.

  11. 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

  12. 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.

  13. 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

  14. 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.

  15. 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.

  16. 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.

  17. 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

  18. 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.

  19. 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

  20. 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.

  1. 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...

  2. 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

  3. 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

  4. 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.

  5. 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

  6. 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.

  7. 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)

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

    International Nuclear Information System (INIS)

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

    2012-01-01

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

  9. 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

  10. Novel in-situ lamella fabrication technique for in-situ TEM.

    Science.gov (United States)

    Canavan, Megan; Daly, Dermot; Rummel, Andreas; McCarthy, Eoin K; McAuley, Cathal; Nicolosi, Valeria

    2018-03-29

    In-situ transmission electron microscopy is rapidly emerging as the premier technique for characterising materials in a dynamic state on the atomic scale. The most important aspect of in-situ studies is specimen preparation. Specimens must be electron transparent and representative of the material in its operational state, amongst others. Here, a novel fabrication technique for the facile preparation of lamellae for in-situ transmission electron microscopy experimentation using focused ion beam milling is developed. This method involves the use of rotating microgrippers during the lift-out procedure, as opposed to the traditional micromanipulator needle and platinum weld. Using rotating grippers, and a unique adhesive substance, lamellae are mounted onto a MEMS device for in-situ TEM annealing experiments. We demonstrate how this technique can be used to avoid platinum deposition as well as minimising damage to the MEMS device during the thinning process. Our technique is both a cost effective and readily implementable alternative to the current generation of preparation methods for in-situ liquid, electrical, mechanical and thermal experimentation within the TEM as well as traditional cross-sectional lamella preparation. Copyright © 2018 Elsevier B.V. All rights reserved.

  11. 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)

  12. 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.

  13. 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.

  14. 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.)

  15. 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...

  16. 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"

  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. 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.

  19. 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...

  20. 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)

  1. 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.

  2. 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...

  3. 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.

  4. 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.

  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. 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....

  7. 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.

  8. 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...

  9. 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.

  10. 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.

  11. 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...

  12. 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.

  13. 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.

  14. 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...

  15. 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.

  16. 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.

  17. 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

  18. 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.

  19. 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

  20. 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.

  1. 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.

  2. In Situ Ptychography of Heterogeneous Catalysts using Hard X-Rays

    DEFF Research Database (Denmark)

    Baier, Sina; Damsgaard, Christian Danvad; Scholz, Maria

    2016-01-01

    A new closed cell is presented for in situ X-ray ptychography which allows studies under gas flow and at elevated temperature. In order to gain complementary information by transmission and scanning electron microscopy, the cell makes use of a Protochips E-chipTM which contains a small, thin...... the same sample holder for ex situ electron microscopy before and after the in situ study underlines the unique possibilities available with this combination of electron microscopy and X-ray microscopy on the same sample....

  3. 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.

  4. 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)

  5. 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

  6. 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]...

  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. 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

  9. 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.

  10. 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.

  11. 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.

  12. 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.

  13. 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.

  14. 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...

  15. 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...

  16. 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.

  17. 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

  18. 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 .

  19. 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.

  20. 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...

  1. 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

  2. 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.

  3. 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.

  4. 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.

  5. 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.

  6. 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

  7. 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.

  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. 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

  10. 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.

  11. 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

  12. 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.

  13. 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...

  14. 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....

  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. In Situ TEM Creation of Nanowire Devices

    DEFF Research Database (Denmark)

    Alam, Sardar Bilal

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

  17. 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

  18. In situ TEM Raman spectroscopy and laser-based materials modification

    Energy Technology Data Exchange (ETDEWEB)

    Allen, F.I., E-mail: fiallen@lbl.gov [Department of Materials Science and Engineering, University of California, Berkeley, CA 94720 (United States); National Center for Electron Microscopy, Molecular Foundry, Lawrence Berkeley National Laboratory, Berkeley, CA 94720 (United States); Kim, E. [Department of Mechanical Engineering, University of California, Berkeley, CA 94720 (United States); Andresen, N.C. [Engineering Division, Lawrence Berkeley National Laboratory, Berkeley, CA 94720 (United States); Grigoropoulos, C.P. [Department of Mechanical Engineering, University of California, Berkeley, CA 94720 (United States); Minor, A.M., E-mail: aminor@lbl.gov [Department of Materials Science and Engineering, University of California, Berkeley, CA 94720 (United States); National Center for Electron Microscopy, Molecular Foundry, Lawrence Berkeley National Laboratory, Berkeley, CA 94720 (United States)

    2017-07-15

    We present a modular assembly that enables both in situ Raman spectroscopy and laser-based materials processing to be performed in a transmission electron microscope. The system comprises a lensed Raman probe mounted inside the microscope column in the specimen plane and a custom specimen holder with a vacuum feedthrough for a tapered optical fiber. The Raman probe incorporates both excitation and collection optics, and localized laser processing is performed using pulsed laser light delivered to the specimen via the tapered optical fiber. Precise positioning of the fiber is achieved using a nanomanipulation stage in combination with simultaneous electron-beam imaging of the tip-to-sample distance. Materials modification is monitored in real time by transmission electron microscopy. First results obtained using the assembly are presented for in situ pulsed laser ablation of MoS{sub 2} combined with Raman spectroscopy, complimented by electron-beam diffraction and electron energy-loss spectroscopy. - Highlights: • Raman spectroscopy and laser-based materials processing in a TEM are demonstrated. • A lensed Raman probe is mounted in the sample chamber for close approach. • Localized laser processing is achieved using a tapered optical fiber. • Raman spectroscopy and pulsed laser ablation of MoS{sub 2} are performed in situ.

  19. In situ TEM Raman spectroscopy and laser-based materials modification

    International Nuclear Information System (INIS)

    Allen, F.I.; Kim, E.; Andresen, N.C.; Grigoropoulos, C.P.; Minor, A.M.

    2017-01-01

    We present a modular assembly that enables both in situ Raman spectroscopy and laser-based materials processing to be performed in a transmission electron microscope. The system comprises a lensed Raman probe mounted inside the microscope column in the specimen plane and a custom specimen holder with a vacuum feedthrough for a tapered optical fiber. The Raman probe incorporates both excitation and collection optics, and localized laser processing is performed using pulsed laser light delivered to the specimen via the tapered optical fiber. Precise positioning of the fiber is achieved using a nanomanipulation stage in combination with simultaneous electron-beam imaging of the tip-to-sample distance. Materials modification is monitored in real time by transmission electron microscopy. First results obtained using the assembly are presented for in situ pulsed laser ablation of MoS_2 combined with Raman spectroscopy, complimented by electron-beam diffraction and electron energy-loss spectroscopy. - Highlights: • Raman spectroscopy and laser-based materials processing in a TEM are demonstrated. • A lensed Raman probe is mounted in the sample chamber for close approach. • Localized laser processing is achieved using a tapered optical fiber. • Raman spectroscopy and pulsed laser ablation of MoS_2 are performed in situ.

  20. 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.

  1. 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.

  2. 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.

  3. 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

  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. 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.)

  6. 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.

  7. 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...

  8. 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.

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

    International Nuclear Information System (INIS)

    Chen, C L; Mori, H

    2009-01-01

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

  10. 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.

  11. Report on the Installation and Preparedness of a Protochips Fusion in-situ Heating Holder for TEM

    Energy Technology Data Exchange (ETDEWEB)

    Edmondson, Philip D. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

    2017-03-01

    This brief report documents the procurement and installation of a Protochips Fusion (formerly Aduro) high-temperature, high stability transmission electron microscopy (TEM) specimen holder that allows for the high spatial resolution characterization of material specimens at high temperature in situ of an electron microscope. This specimen holder was specifically procured for use with The FEI Talos F200X Scanning/Transmission Electron Microscope (STEM) in Oak Ridge National Laboratory’s (ORNL’s) Low Activation Materials Development and Analysis (LAMDA) Laboratory. The Protochips Fusion holder will enable high-resolution structural and chemical analysis of irradiated materials at high temperature, becoming a unique capability worldwide, and would encourage high-quality in situ experiments to be conducted on irradiated materials.

  12. 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.

  13. 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

  14. 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)

  15. 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...

  16. 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.

  17. 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)

  18. 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

  19. 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

  20. 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.

  1. 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.

  2. 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

  3. 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...

  4. In situ studies of NO reduction by H

    NARCIS (Netherlands)

    Roobol, S. B.; Onderwaater, W. G.; van Spronsen, M. A.; Carla, F; Balmes, O; Navarro-Paredes, V; Vendelbo, S.B.; Kooyman, P.J.; Elkjær, C. F.; Helveg, S; Felici, R; Frenken, J. W.M.; Groot, I.M.N.

    2017-01-01

    In situ surface X-ray diffraction and transmission electron microscopy at 1 bar show massive material transport of platinum during high-temperature NO reduction with H2. A Pt(110) single-crystal surface shows a wide variety of surface reconstructions and extensive faceting of the

  5. 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

  6. 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.

  7. 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

  8. 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

  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. 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.

  11. 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.

  12. 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.

  13. 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...

  14. Void formation in NiTi shape memory alloys by medium-voltage electron irradiation

    International Nuclear Information System (INIS)

    Schlossmacher, P.; Stober, T.

    1995-01-01

    In-situ electron irradiation experiments of NiTi shape memory alloys, using high-voltage transmission electron microscopes, result in amorphization of the intermetallic compound. In all of these experiments high-voltages more than 1.0 MeV had to be applied in order to induce the crystalline-to-amorphous transformation. To their knowledge no irradiation effects of medium-voltage electrons of e.g. 0.5 MeV have been reported in the literature. In this contribution, the authors describe void formation in two different NiTi shape memory alloys, resulting from in-situ electron irradiation, using a 300 kV electron beam in a transmission electron microscope. First evidence is presented that void formation is correlated with the total oxygen content of the alloys

  15. 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....

  16. 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.

  17. Crystallization of TiO2 Nanotubes by In Situ Heating TEM

    KAUST Repository

    Casu, Alberto

    2018-01-15

    The thermally-induced crystallization of anodically grown TiO2 amorphous nanotubes has been studied so far under ambient pressure conditions by techniques such as differential scanning calorimetry and in situ X-ray diffraction, then looking at the overall response of several thousands of nanotubes in a carpet arrangement. Here we report a study of this phenomenon based on an in situ transmission electron microscopy approach that uses a twofold strategy. First, a group of some tens of TiO2 amorphous nanotubes was heated looking at their electron diffraction pattern change versus temperature, in order to determine both the initial temperature of crystallization and the corresponding crystalline phases. Second, the experiment was repeated on groups of few nanotubes, imaging their structural evolution in the direct space by spherical aberration-corrected high resolution transmission electron microscopy. These studies showed that, differently from what happens under ambient pressure conditions, under the microscope’s high vacuum (p < 10−5 Pa) the crystallization of TiO2 amorphous nanotubes starts from local small seeds of rutile and brookite, which then grow up with the increasing temperature. Besides, the crystallization started at different temperatures, namely 450 and 380 °C, when the in situ heating was performed irradiating the sample with electron beam energy of 120 or 300 keV, respectively. This difference is due to atomic knock-on effects induced by the electron beam with diverse energy.

  18. 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

  19. 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

  20. A flexible multi-stimuli in situ (S)TEM: Concept, optical performance, and outlook

    International Nuclear Information System (INIS)

    Börrnert, Felix; Müller, Heiko; Riedel, Thomas; Linck, Martin; Kirkland, Angus I.; Haider, Max.; Büchner, Bernd; Lichte, Hannes

    2015-01-01

    The progress in (scanning) transmission electron microscopy development had led to an unprecedented knowledge of the microscopic structure of functional materials at the atomic level. Additionally, although not widely used yet, electron holography is capable to map the electric and magnetic potential distributions at the sub-nanometer scale. Nevertheless, in situ studies inside a (scanning) transmission electron microscope ((S)TEM) are extremely challenging because of the much restricted size and accessibility of the sample space. Here, we introduce a concept for a dedicated in situ (S)TEM with a large sample chamber for flexible multi-stimuli experimental setups and report about the electron optical performance of the instrument. We demonstrate a maximum resolving power of about 1 nm in conventional imaging mode and substantially better than 5 nm in scanning mode while providing an effectively usable “pole piece gap” of 70 mm. - Highlights: • A concept for a (S)TEM with a large sample chamber is outlined. • An actual microscope is modified and has now a 70 mm high sample space. • The resolving power is about 1 nm in TEM and better than 5 nm in STEM mode. • Possible dedicated in situ microscopes with present technology are discussed

  1. A flexible multi-stimuli in situ (S)TEM: Concept, optical performance, and outlook

    Energy Technology Data Exchange (ETDEWEB)

    Börrnert, Felix, E-mail: felix.boerrnert@triebenberg.de [Speziallabor Triebenberg, Technische Universität Dresden, 01062 Dresden (Germany); IFW Dresden, PF 27 01 16, 01171 Dresden (Germany); Department of Materials, University of Oxford, Parks Road, Oxford OX1 3PH (United Kingdom); Müller, Heiko; Riedel, Thomas; Linck, Martin [CEOS GmbH, Englerstraße 28, 69126 Heidelberg (Germany); Kirkland, Angus I. [Department of Materials, University of Oxford, Parks Road, Oxford OX1 3PH (United Kingdom); Haider, Max. [CEOS GmbH, Englerstraße 28, 69126 Heidelberg (Germany); Büchner, Bernd [IFW Dresden, PF 27 01 16, 01171 Dresden (Germany); Lichte, Hannes [Speziallabor Triebenberg, Technische Universität Dresden, 01062 Dresden (Germany)

    2015-04-15

    The progress in (scanning) transmission electron microscopy development had led to an unprecedented knowledge of the microscopic structure of functional materials at the atomic level. Additionally, although not widely used yet, electron holography is capable to map the electric and magnetic potential distributions at the sub-nanometer scale. Nevertheless, in situ studies inside a (scanning) transmission electron microscope ((S)TEM) are extremely challenging because of the much restricted size and accessibility of the sample space. Here, we introduce a concept for a dedicated in situ (S)TEM with a large sample chamber for flexible multi-stimuli experimental setups and report about the electron optical performance of the instrument. We demonstrate a maximum resolving power of about 1 nm in conventional imaging mode and substantially better than 5 nm in scanning mode while providing an effectively usable “pole piece gap” of 70 mm. - Highlights: • A concept for a (S)TEM with a large sample chamber is outlined. • An actual microscope is modified and has now a 70 mm high sample space. • The resolving power is about 1 nm in TEM and better than 5 nm in STEM mode. • Possible dedicated in situ microscopes with present technology are discussed.

  2. 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.

  3. 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

  4. 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.

  5. In Situ Study of Noncatalytic Metal Oxide Nanowire Growth

    DEFF Research Database (Denmark)

    Rackauskas, Simas; Jiang, Hua; Wagner, Jakob Birkedal

    2014-01-01

    a catalyst is still widely disputed and unclear. Here, we show that the nanowire growth during metal oxidation is limited by a nucleation of a new layer. On the basis of in situ transmission electron microscope investigations we found that the growth occurs layer by layer at the lowest specific surface...

  6. 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

  7. 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

  8. Location specific in situ TEM straining specimens made using FIB

    International Nuclear Information System (INIS)

    Field, R.D.; Papin, P.A.

    2004-01-01

    A method has been devised and demonstrated for producing in situ straining specimens for the transmission electron microscope (TEM) from specific locations in a sample using a dual-beam focused ion beam (FIB) instrument. The specimen is removed from a polished surface in the FIB using normal methods and then attached to a pre-fabricated substrate in the form of a modified TEM tensile specimen. In this manner, specific features of the microstructure of a polished optical mount can be selected for in situ tensile straining. With the use of electron backscattered diffraction (EBSD), this technique could be extended to select specific orientations of the specimen as well

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

    Science.gov (United States)

    Takeda, Seiji; Yoshida, Hideto

    2013-02-01

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

  10. 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

  11. 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.

  12. 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.

  13. 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.

  14. 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.

  15. 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.

  16. 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.

  17. 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.

  18. 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.

  19. Quantitative in situ TEM tensile testing of an individual nickel nanowire

    International Nuclear Information System (INIS)

    Lu Yang; Peng Cheng; Ganesan, Yogeeswaran; Lou Jun; Huang Jianyu

    2011-01-01

    In this paper, we have demonstrated the usage of a novel micro-mechanical device (MMD) to perform quantitative in situ tensile tests on individual metallic nanowires inside a transmission electron microscope (TEM). Our preliminary experiment on a 360 nm diameter nickel nanowire showed that the sample fractured at an engineering stress of ∼ 1.2 GPa and an engineering strain of ∼ 4%, which is consistent with earlier experiments performed inside a scanning electron microscope (SEM). With in situ high resolution TEM imaging and diffraction capabilities, this novel experimental set-up could provide unique opportunities to reveal the underlying deformation and damage mechanisms for metals at the nanoscale.

  20. 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...

  1. 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.

  2. 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

  3. 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

  4. 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.

  5. 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

  6. Effect of silica particles modified by in-situ and ex-situ methods on the reinforcement of silicone rubber

    International Nuclear Information System (INIS)

    Song, Yingze; Yu, Jinhong; Dai, Dan; Song, Lixian; Jiang, Nan

    2014-01-01

    Highlights: • In-situ and ex-situ methods were applied to modify silica particles. • In-situ method was more beneficial to preparing silica particles with high BET surface area. • Silicone rubber filled with in-situ modified silica exhibits excellent mechanical and thermal properties. - Abstract: In-situ and ex-situ methods were applied to modify silica particles in order to investigate their effects on the reinforcement of silicone rubber. Surface area and pore analyzer, laser particle size analyzer, Fourier-transform infrared spectroscopy (FTIR), contact-angle instrument, and transmission electron microscope (TEM) were utilized to investigate the structure and properties of the modified silica particles. Dynamic mechanical thermal analyzer (DMTA) was employed to characterize the vulcanizing behavior and mechanical properties of the composites. Thermogravimetric analysis (TGA) was performed to test the thermal stability of the composites. FTIR and contact angle analysis indicated that silica particles were successfully modified by these two methods. The BET surface area and TEM results reflected that in-situ modification was more beneficial to preparing silica particles with irregular shape and higher BET surface area in comparison with ex-situ modification. The DMTA and TGA data revealed that compared with ex-situ modification, the in-situ modification produced positive influence on the reinforcement of silicone rubber

  7. 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.

  8. Localised corrosion in aluminium alloy 2024-T3 using in situ TEM

    NARCIS (Netherlands)

    Malladi, S.; Shen, C.; Xu, Q.; De Kruijff, T.; Yücelen, E.; Tichelaar, F.; Zandbergen, H.

    2013-01-01

    An approach to carry out chemical reactions using aggressive gases in situ in a transmission electron microscope (TEM), at ambient pressures of 1.5 bar using a windowed environmental cell, called a nanoreactor, is presented here. The nanoreactor coupled with a specially developed holder with

  9. 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

  10. In situ visualization of Ni-Nb bulk metallic glasses phase transition

    OpenAIRE

    Oreshkin, A. I.; Mantsevich, V. N.; Savinov, S. V.; Oreshkin, S. I.; Panov, V. I.; Yavari, A. R.; Miracle, D. B.; Louzguine-Luzgin, D. V.

    2013-01-01

    We report the results of the Ni-based bulk metallic glass structural evolution and crystallization behavior in situ investigation. The X-ray diffraction (XRD), transmission electron microscopy (TEM), nano-beam diffraction (NBD), differential scanning calorimetry (DSC), radial distribution function (RDF) and scanning probe microscopy/spectroscopy (STM/STS) techniques were applied to analyze the structure and electronic properties of Ni63.5Nb36.5 glasses before and after crystallization. It was...

  11. 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...

  12. 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.

  13. 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

  14. 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.

  15. 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.

  16. 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.

  17. Illuminating Electron Microscopy of Photocatalysts

    DEFF Research Database (Denmark)

    Cavalca, Filippo

    .1% of the surface of the planet with a device that converts solar energy into a useable form at 10% efficiency would give more than the present worldwide consumption of fossil energy. Photocatalysts are of fundamental interest for sustainable energy research because they provide a viable route for converting solar...... energy into chemical bonds. By means of Transmission Electron Microscopy (TEM) it is possible to gain insight in the fundamentals of their reaction mechanisms, chemical behaviour, structure and morphology before, during and after reaction using in situ investigations. In particular, the environmental TEM...... the microscope that allows electron microscopy under nonconventional TEM conditions and new kinds of in situ spectroscopy....

  18. In-Situ Growth and Characterization of Indium Tin Oxide Nanocrystal Rods

    Directory of Open Access Journals (Sweden)

    Yan Shen

    2017-11-01

    Full Text Available Indium tin oxide (ITO nanocrystal rods were synthesized in-situ by a vapor-liquid-solid (VLS method and electron beam evaporation technique. When the electron-beam gun bombarded indium oxide (In2O3 and tin oxide (SnO2 mixed sources, indium and tin droplets appeared and acted as catalysts. The nanocrystal rods were in-situ grown on the basis of the metal catalyst point. The nanorods have a single crystal structure. Its structure was confirmed by X-ray diffraction (XRD and transmission electron microscopy (TEM. The surface morphology was analyzed by scanning electron microscopy (SEM. During the evaporation, a chemical process was happened and an In2O3 and SnO2 solid solution was formed. The percentage of doped tin oxide was calculated by Vegard’s law to be 3.18%, which was in agreement with the mixture ratio of the experimental data. The single crystal rod had good semiconductor switch property and its threshold voltage of single rod was approximately 2.5 V which can be used as a micro switch device. The transmission rate of crystalline nanorods ITO film was over 90% in visible band and it was up to 95% in the blue green band as a result of the oxygen vacancy recombination luminescence.

  19. 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

  20. 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

  1. 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).

  2. 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

  3. 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.

  4. 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

  5. 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.

  6. Influence of electron beam exposure on crystallization of phase-change materials

    NARCIS (Netherlands)

    Pandian, Ramanathaswamy; Kooi, Bart J.; De Hosson, Jeff Th. M.; Pauza, Andrew

    2007-01-01

    Isothermal crystallization of amorphous SbxTe films capped with ZnS-SiO2 or GeCrN layers was performed using in situ heating within a transmission electron microscope. The effect of the electron beam of the microscope on the crystallization process was investigated. It was found that electron

  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. 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

  9. 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...

  10. 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.

  11. In-situ TEM investigation of microstructural evolution in magnetron sputtered Al-Zr and Al-Zr-Si coatings during heat treatment

    DEFF Research Database (Denmark)

    Gudla, Visweswara Chakravarthy; Rechendorff, Kristian; Balogh, Zoltan Imre

    2016-01-01

    The magnetron sputtered Al–Zr and Al–Zr–Si coatings were heat treated in-situ in a transmission electron microscope as well as ex-situ to observe their annealing behaviour and phase transformations. The samples were heated up to a temperature of 550 °C and then cooled to room temperature. A layer...

  12. 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)

  13. 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.

  14. 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.

  15. 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.

  16. 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}.

  17. 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 ...

  18. 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...

  19. 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.

  20. In situ TEM nanoindentation and dislocation-grain boundary interactions : a tribute to David Brandon

    NARCIS (Netherlands)

    de Hosson, J.T.M.; Soer, W.A.; Minor, A.M.; Shan, Z.W.; Stach, E.A.; Asif, S.A.S.; Warren, O.L.

    2006-01-01

    As a tribute to the scientific work of Professor David Brandon, this paper delineates the possibilities of utilizing in situ transmission electron microscopy to unravel dislocation-grain boundary interactions. In particular, we have focused on the deformation characteristics of Al-Mg films. To this

  1. 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.

  2. 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.

  3. 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.

  4. In situ TEM electromechanical testing of nanowires and nanotubes.

    Science.gov (United States)

    Espinosa, Horacio D; Bernal, Rodrigo A; Filleter, Tobin

    2012-11-05

    The emergence of one-dimensional nanostructures as fundamental constituents of advanced materials and next-generation electronic and electromechanical devices has increased the need for their atomic-scale characterization. Given its spatial and temporal resolution, coupled with analytical capabilities, transmission electron microscopy (TEM) has been the technique of choice in performing atomic structure and defect characterization. A number of approaches have been recently developed to combine these capabilities with in-situ mechanical deformation and electrical characterization in the emerging field of in-situ TEM electromechanical testing. This has enabled researchers to establish unambiguous synthesis-structure-property relations for one-dimensional nanostructures. In this article, the development and latest advances of several in-situ TEM techniques to carry out mechanical and electromechanical testing of nanowires and nanotubes are reviewed. Through discussion of specific examples, it is shown how the merging of several microsystems and TEM has led to significant insights into the behavior of nanowires and nanotubes, underscoring the significant role in-situ techniques play in the development of novel nanoscale systems and materials. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. 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.

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

    DEFF Research Database (Denmark)

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

    2010-01-01

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

  7. 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.

  8. 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.

  9. In Situ Study of Thermal Stability of Copper Oxide Nanowires at Anaerobic Environment

    Directory of Open Access Journals (Sweden)

    Lihui Zhang

    2014-01-01

    Full Text Available Many metal oxides with promising electrochemical properties were developed recently. Before those metal oxides realize the use as an anode in lithium ion batteries, their thermal stability at anaerobic environment inside batteries should be clearly understood for safety. In this study, copper oxide nanowires were investigated as an example. Several kinds of in situ experiment methods including in situ optical microscopy, in situ Raman spectrum, and in situ transmission electron microscopy were adopted to fully investigate their thermal stability at anaerobic environment. Copper oxide nanowires begin to transform as copper(I oxide at about 250°C and finish at about 400°C. The phase transformation proceeds with a homogeneous nucleation.

  10. 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.

  11. 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...

  12. 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.

  13. 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.)

  14. 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...

  15. 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

  16. 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.

  17. 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.

  18. 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...

  19. 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.)

  20. 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

  1. 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.

  2. 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

  3. Solvent-assisted in situ synthesis of cysteamine-capped silver nanoparticles

    Science.gov (United States)

    Oliva, José M.; Ríos de la Rosa, Julio M.; Sayagués, María J.; Sánchez-Alcázar, José A.; Merkling, Patrick J.; Zaderenko, Ana P.

    2018-03-01

    Silver nanoparticles offer a huge potential for biomedical applications owing to their exceptional properties and small size. Specifically, cysteamine-capped silver nanoparticles could form the basis for new anticancer therapies combining the cytotoxic effect of the silver core with the inherent antitumor activity of cysteamine, which inhibit cancer cell proliferation and suppress invasion and metastasis. In addition, the capability of the cysteamine coating monolayer to couple a variety of active principles and targeting (bio)molecules of interest proves key to the tailoring of this platform in order to exploit the pathophysiology of specific tumor types. Nevertheless, the chain length and conformational flexibility of cysteamine, together with its ability to attach to the surface of silver nanoparticles via both the thiol and the amine group, have made the in situ synthesis of these particles an especially challenging task. Herein we report a solvent-assisted in situ synthesis method that solves this problem. The obtained nanoparticles have been fully characterized by UV-visible absorption spectroscopy, Fourier transform infrared spectroscopy, transmission electron microscopy, electron diffraction measurement, high resolution transmission electron microscopy, scanning transmission electron microscopy, energy dispersive x-ray spectroscopy nanoanalysis, and dynamic light scattering measurement. Our synthesis method achieves extremely high yield and surface coating ratio, and colloidal stability over a wide range of pH values including physiological pH. Additionally, we have demonstrated that cysteamine-capped nanoparticles obtained by this method can be conjugated to an antibody for active targeting of the epidermal growth factor receptor, which plays an important role in the pathogenesis and progression of a wide variety of tumors, and induce cell death in human squamous carcinoma cells. We believe this method can be readily extended to combinations of noble

  4. 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

  5. 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

  6. 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.

  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. 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

  9. 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

  10. 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.

  11. 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

  12. 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.

  13. In-situ nanomechanical study on bending characteristics of individual multi-walled carbon nanotubes

    Energy Technology Data Exchange (ETDEWEB)

    Tsai, Ping-Chi, E-mail: pctjbenchen@yahoo.com.tw [Department of Mechanical Engineering, National Chung Cheng University, Chia-Yi 621, Taiwan (China); Advanced Institute of Manufacturing with High-Tech Innovations, National Chung Cheng University, Chia-Yi 621, Taiwan (China); Jeng, Yeau-Ren, E-mail: imeyrj@ccu.edu.tw [Department of Mechanical Engineering, National Chung Cheng University, Chia-Yi 621, Taiwan (China); Advanced Institute of Manufacturing with High-Tech Innovations, National Chung Cheng University, Chia-Yi 621, Taiwan (China)

    2016-03-21

    Bending characteristics of individual thin-walled carbon nanotubes (CNTs) are investigated through a novel in-situ nanoindentation in transmission electron microscopy. Unlike thick-walled CNTs, the graphitic layers of thin ones buckle into V-shaped kinks rather than Yoshimura ripples. These kinks are found to be entirely reversible without residual plastic deformation following unloading.

  14. Near-Curie magnetic anomaly at the Ni/C interface observed by Electron Holography

    DEFF Research Database (Denmark)

    Ferrari, Loris; Matteucci, Giorgio; Schofield, Marvin A

    2010-01-01

    We analyze with electron holography carried out in a transmission electron microscope the near-Curie behavior of magnetism at the edge of a Nickel thin film coated with Carbon. In-situ experiments with finely controlled variations of the sample temperature reveal an anomaly in the ferromagnetic...

  15. 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.

  16. 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).

  17. 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

  18. 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

  19. 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.

  20. 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

  1. Precise rotational alignment of x-ray transmission diffraction gratings

    International Nuclear Information System (INIS)

    Hill, S.L.

    1988-01-01

    Gold transmission diffraction gratings used for x-ray spectroscopy must sometimes be rotationally aligned to the axis of a diagnostic instrument to within sub-milliradian accuracy. We have fabricated transmission diffraction gratings with high line-densities (grating period of 200 and 300 nm) using uv holographic and x-ray lithography. Since the submicron features of the gratings are not optically visible, precision alignment is time consuming and difficult to verify in situ. We have developed a technique to write an optically visible alignment pattern onto these gratings using a scanning electron microscope (SEM). At high magnification (15000 X) several submicron lines of the grating are observable in the SEM, making it possible to write an alignment pattern parallel to the grating lines in an electron-beam-sensitive coating that overlays the grating. We create an alignment pattern by following a 1-cm-long grating line using the SEM's joystick-controlled translation stage. By following the same grating line we are assured the traveled direction of the SEM electron beam is parallel to the grating to better than 10 μradian. The electron-beam-exposed line-width can be large (5 to 15 μm wide) depending on the SEM magnification, and is therefore optically visible. The exposed pattern is eventually made a permanent feature of the grating by ion beam etching or gold electroplating. The pattern can be used to accurately align the grating to the axis of a diagnostic instrument. More importantly, the alignment of the grating can be quickly verified in situ

  2. In-situ Multimodal Imaging and Spectroscopy of Mg Electrodeposition at Electrode-Electrolyte Interfaces

    Science.gov (United States)

    Wu, Yimin A.; Yin, Zuwei; Farmand, Maryam; Yu, Young-Sang; Shapiro, David A.; Liao, Hong-Gang; Liang, Wen-I.; Chu, Ying-Hao; Zheng, Haimei

    2017-02-01

    We report the study of Mg cathodic electrochemical deposition on Ti and Au electrode using a multimodal approach by examining the sample area in-situ using liquid cell transmission electron microscopy (TEM), scanning transmission X-ray microscopy (STXM) and X-ray absorption spectroscopy (XAS). Magnesium Aluminum Chloride Complex was synthesized and utilized as electrolyte, where non-reversible features during in situ charging-discharging cycles were observed. During charging, a uniform Mg film was deposited on the electrode, which is consistent with the intrinsic non-dendritic nature of Mg deposition in Mg ion batteries. The Mg thin film was not dissolvable during the following discharge process. We found that such Mg thin film is hexacoordinated Mg compounds by in-situ STXM and XAS. This study provides insights on the non-reversibility issue and failure mechanism of Mg ion batteries. Also, our method provides a novel generic method to understand the in situ battery chemistry without any further sample processing, which can preserve the original nature of battery materials or electrodeposited materials. This multimodal in situ imaging and spectroscopy provides many opportunities to attack complex problems that span orders of magnitude in length and time scale, which can be applied to a broad range of the energy storage systems.

  3. Transmission Electron Microscopy of the Textured Silver Back Reflector of a Thin Film Silicon Solar Cell: From Crystallography to Optical Absorption

    DEFF Research Database (Denmark)

    Duchamp, Martial; Söderström, K.; Jeangros, Q.

    2011-01-01

    The study of light trapping in amorphous, microcrystalline and micromorph thin-film Si solar cells is an important and active field of investigation. It has been demonstrated that the use of a rough Ag back-reflector lead to an increase of short circuit current but also to losses through...... the creation of surface plasmon polaritons. Here, we use transmission electron microscopy (TEM) techniques to study the grain structure of a Ag thin-film that was sputtered on top of 2-μm-thick rough ZnO layer - defects, such as twin-boundaries have been observed. A smoothing of the top Ag surface was also...... observed after ex-situ annealing. Electron energy-loss spectroscopy with a monochromatic beam was used to measure the surface plasmon resonance with nm spatial resolution. 1 eV and 3 eV Ag surface plasmon resonances have been observed on as-grown layers. Such measurements provide valuable information about...

  4. 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)

  5. 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.

  6. 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.

  7. 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

  8. 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...

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

    Directory of Open Access Journals (Sweden)

    Takeshi Fujita

    2017-10-01

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

  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. 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)

  12. 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

  13. 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.)

  14. Effects of size on the mechanical response of metallic glasses investigated through in situ TEM bending and compression experiments

    NARCIS (Netherlands)

    Chen, C.Q.; Pei, Y.T.; Hosson, J.T.M. De

    Quantitative bending and compression tests on micropillars made of two different amorphous alloys, with tip diameters ranging from 93 to 645 rim, are performed in situ in a transmission electron microscope (TEM). Under microcompression each pillar shows an intermittent plastic flow accommodated by

  15. Advanced electron microscopy characterization of nanomaterials for catalysis

    Directory of Open Access Journals (Sweden)

    Dong Su

    2017-04-01

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

  16. 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

  17. 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.

  18. 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

  19. 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.

  20. 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...

  1. 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…

  2. 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.

  3. Laser Based In Situ Techniques: Novel Methods for Generating Extreme Conditions in TEM Samples

    Energy Technology Data Exchange (ETDEWEB)

    Taheri, M; Lagrange, T; Reed, B; Armstrong, M; Campbell, G; DeHope, W; Kim, J; King, W; Masiel, D; Browning, N

    2008-02-25

    The Dynamic Transmission Electron Microscope (DTEM) is introduced as a novel tool for in situ processing of materials. Examples of various types of dynamic studies outline the advantages and differences of laser-based heating in the DTEM in comparison to conventional (resistive) heating in situ TEM methods. We demonstrate various unique capabilities of the drive laser, namely, in situ processing of nanoscale materials, rapid and high temperature phase transformations, and controlled thermal activation of materials. These experiments would otherwise be impossible without the use of the DTEM drive laser. Thus, the potential of the DTEM to as a new technique to process and characterize the growth of a myriad of micro and nanostructures is demonstrated.

  4. 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.

  5. 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...

  6. 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

  7. 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

  8. 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.

  9. 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

  10. ''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

  11. 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.

  12. Polystyrene/magnesium hydroxide nanocomposite particles prepared by surface-initiated in-situ polymerization

    International Nuclear Information System (INIS)

    Liu Hui; Yi Jianhong

    2009-01-01

    In order to avoid their agglomeration and incompatibility with hydrophobic polystyrene substrate, magnesium hydroxide nanoparticles were encapsulated by surface-initiated in-situ polymerization of styrene. The process contained two steps: electrostatic adsorption of initiator and polymerization of monomer on the surface of magnesium hydroxide. It was found that high adsorption ratio in the electrostatic adsorption of initiator could be attained only in acidic region, and the adsorption belonged to typical physical process. Compared to traditional in-situ polymerization, higher grafting ratio was obtained in surface-initiated in-situ polymerization, which can be attributed to weaker steric hindrance. Both Fourier transform infrared spectroscopy (FTIR) and transmission electron microscopy (TEM) indicated that polystyrene/magnesium hydroxide nanocomposite particles had been successfully prepared by surface-initiated in-situ polymerization. The resulting samples were also analyzed and characterized by means of contact angle testing, dispersibility evaluation and thermogravimetric analysis

  13. The influence of C{sub s}/C{sub c} correction in analytical imaging and spectroscopy in scanning and transmission electron microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Zaluzec, Nestor J., E-mail: zaluzec@microscopy.com

    2015-04-15

    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{sub s}) in high resolution phase contrast imaging. Following shortly behind, has been the development of chromatic aberration correction (C{sub c}) which augments those accomplishments. In this paper we will review and summarize how the combination of C{sub s}/C{sub 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.

  14. 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.

  15. 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

  16. 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.

  17. 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)

  18. 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.

  19. 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.

  20. 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.

  1. Influence of Structural Defects on Biomineralized ZnS Nanoparticle Dissolution: An In-Situ Electron Microscopy Study

    Energy Technology Data Exchange (ETDEWEB)

    Eskelsen, Jeremy R. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Environmental Sciences Division; Xu, Jie [Univ. of Texas, El Paso, TX (United States). Geological Sciences; Chiu, Michelle Y. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Environmental Sciences Division; Moon, Ji-Won [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Biosciences Division; Wilkins, Branford O. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Environmental Sciences Division; Graham, David E. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Biosciences Division; Gu, Baohua [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Environmental Sciences Division; Pierce, Eric M. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Environmental Sciences Division

    2017-12-19

    The dissolution of metal sulfides, such as ZnS, plays an important role in the fate of metal contaminants in the environment. Here we have examined the dissolution behavior of ZnS nanoparticles synthesized via several abiotic and biological pathways. Specifically, the biogenic ZnS nanoparticles were produced by an anaerobic, metal-reducing bacterium Thermoanaerobacter sp. X513 in a Zn-amended, thiosulfate-containing growth medium, whereas the abiogenic ZnS nanoparticles were produced by mixing an aqueous Zn solution with either H2S-rich gas or Na2S solution. For biogenic synthesis, we prepared two types of samples, in the presence or absence of trace silver (Ag). The size distribution, crystal structure, aggregation behavior, and internal defects of the synthesized ZnS nanoparticles were primarily examined using high-resolution transmission electron microscopy coupled with X-ray energy dispersive spectroscopy. The characterization results show that both the biogenic and abiogenic samples were dominantly composed of sphalerite. In the absence of Ag, the biogenic ZnS nanoparticles were significantly larger (i.e., ~10 nm) than the abiogenic ones (i.e., ~3–5 nm) and contained structural defects (e.g., twins and stacking faults). The presence of trace Ag showed a restraining effect on the particle size of the biogenic ZnS, resulting in quantum-dot-sized nanoparticles (i.e., ~3 nm). In situ dissolution experiments for the synthesized ZnS were conducted with a liquid-cell coupled to a transmission electron microscope (LCTEM), and the primary factors (i.e., the presence or absence structural defects) were evaluated for their effects on the dissolution behavior using the biogenic and abiogenic ZnS nanoparticle samples with the largest average particle size. Analysis of the dissolution results (i.e., change in particle radius with time) using the Kelvin equation shows that the defect-bearing biogenic ZnS nanoparticles (γ = 0.799 J/m2) have

  2. 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

  3. 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

  4. 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...

  5. 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

  6. 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

  7. 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.

  8. 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...

  9. 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

  10. 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.

  11. Using the in situ lift-out technique to prepare TEM specimens on a single-beam FIB instrument

    International Nuclear Information System (INIS)

    Lekstrom, M; McLachlan, M A; Husain, S; McComb, D W; Shollock, B A

    2008-01-01

    Transmission electron microscope (TEM) specimens are today routinely prepared using focussed ion beam (FIB) instruments. Specifically, the lift-out method has become an increasingly popular technique and involves removing thin cross-sections from site-specific locations and transferring them to a TEM grid. This lift-out process can either be performed ex situ or in situ. The latter is mainly carried out on combined dual-beam FIB and scanning electron microscope (SEM) systems whereas conventional single-beam instruments often are limited to the traditional ex situ method. It is nevertheless desirable to enhance the capabilities of existing single-beam instruments to allow for in situ lift-out preparation to be performed since this technique offers a number of advantages over the older ex situ method. A single-beam FIB instrument was therefore modified to incorporate an in situ micromanipulator fitted with a tungsten needle, which can be attached to a cut-out FIB section using ion beam induced platinum deposition. This article addresses the issues of using an ion beam to monitor the in situ manipulation process as well as approaches that can be used to create stronger platinum welds between two objects, and finally, views on how to limit the extent of ion beam damage to the specimen surface.

  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. 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.

  14. 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.

  15. In situ deformation and mechanical properties of bismuth telluride prepared via zone melting

    Science.gov (United States)

    Lai, Tang-Yu; Hsiao, Yu-Jen; Fang, Te-Hua

    2018-03-01

    In this study, we prepared Bi2Te3 nanostructures via zone melting and characterized their mechanical properties by nanoindentation and in situ transmission electron microscopy (TEM). The nanoindentation results revealed that a significant ‘pop-in’ phenomenon occurs under high-loading conditions with multiple dislocations and phase transitions in the material structure. Young’s modulus of the nanostructures was found to be 42.7 ± 2.56 GPa from nanoindentation measurements and 12.3 ± 0.1 GPa from in situ TEM measurements. The results of this study may be useful for the future development of Bi2Te3 thermoelectric devices via printing processes.

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

    International Nuclear Information System (INIS)

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

    2010-01-01

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

  17. Orientation and phase mapping in the transmission electron microscope using precession-assisted diffraction spot recognition: state-of-the-art results.

    Science.gov (United States)

    Viladot, D; Véron, M; Gemmi, M; Peiró, F; Portillo, J; Estradé, S; Mendoza, J; Llorca-Isern, N; Nicolopoulos, S

    2013-10-01

    A recently developed technique based on the transmission electron microscope, which makes use of electron beam precession together with spot diffraction pattern recognition now offers the possibility to acquire reliable orientation/phase maps with a spatial resolution down to 2 nm on a field emission gun transmission electron microscope. The technique may be described as precession-assisted crystal orientation mapping in the transmission electron microscope, precession-assisted crystal orientation mapping technique-transmission electron microscope, also known by its product name, ASTAR, and consists in scanning the precessed electron beam in nanoprobe mode over the specimen area, thus producing a collection of precession electron diffraction spot patterns, to be thereafter indexed automatically through template matching. We present a review on several application examples relative to the characterization of microstructure/microtexture of nanocrystalline metals, ceramics, nanoparticles, minerals and organics. The strengths and limitations of the technique are also discussed using several application examples. ©2013 The Authors. Journal of Microscopy published by John Wiley & Sons Ltd on behalf of Royal Microscopical Society.

  18. 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.

  19. 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.

  20. 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.

  1. An electron microscopy appraisal of tensile fracture in metallic glasses

    International Nuclear Information System (INIS)

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

    2008-01-01

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

  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. 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.

  4. 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....

  5. 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.

  6. 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

  7. 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.

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

    International Nuclear Information System (INIS)

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

    2015-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-10-15

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

  10. Development of an environmental high-voltage electron microscope for reaction science.

    Science.gov (United States)

    Tanaka, Nobuo; Usukura, Jiro; Kusunoki, Michiko; Saito, Yahachi; Sasaki, Katuhiro; Tanji, Takayoshi; Muto, Shunsuke; Arai, Shigeo

    2013-02-01

    Environmental transmission electron microscopy and ultra-high resolution electron microscopic observation using aberration correctors have recently emerged as topics of great interest. The former method is an extension of the so-called in situ electron microscopy that has been performed since the 1970s. Current research in this area has been focusing on dynamic observation with atomic resolution under gaseous atmospheres and in liquids. Since 2007, Nagoya University has been developing a new 1-MV high voltage (scanning) transmission electron microscope that can be used to observe nanomaterials under conditions that include the presence of gases, liquids and illuminating lights, and it can be also used to perform mechanical operations to nanometre-sized areas as well as electron tomography and elemental analysis by electron energy loss spectroscopy. The new instrument has been used to image and analyse various types of samples including biological ones.

  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. Analytical electron microscope study of the omega phase transformation in a zirconium--niobium alloy

    Energy Technology Data Exchange (ETDEWEB)

    Zaluzec, N.J.

    1979-06-01

    An in-situ study of the as-quenched omega phase transformation in Zr--15% Nb was conducted between the temperatures of 77 and 300/sup 0/K using analytical electron microscopy. The domain size of the omega regions observed in this investigation was on the order of 30 A, consistent with previous observations in this system. No alignment of omega domains along <222> directions of the bcc lattice was observed and in-situ thermal cycling experiments failed to produce a long period structure of alternating ..beta.. and ..omega.. phase regions as predicted by one theory of this transformation. Several techniques of microstructural analysis were developed, refined, and standardized. Grouped under the general classification of Analytical Electron Microscopy (AEM) they provide the experimentalist with a unique tool for the microcharacterization of solids, allowing semiquantitative to quantitative analysis of the morphology, crystallography, elemental composition, and electronic structure of regions as small as 20 A in diameter. These techniques have complications, and it was necessary to study the AEM system used in this work so that instrumental artifacts which invalidate the information produced in the microscope environment might be eliminated. Once these factors had been corrected, it was possible to obtain a wealth of information about the microvolume of material under investigation. The microanalytical techniques employed during this research include: energy dispersive x-ray spectroscopy (EDS) using both conventional and scanning transmission electron microscopy (CTEM, STEM), transmission scanning electron diffraction (TSED), the stationary diffraction pattern technique, and electron energy loss spectroscopy (ELS) using a dedicated scanning transmission electron microscope (DSTEM).

  13. Analytical electron microscope study of the omega phase transformation in a zirconium--niobium alloy

    International Nuclear Information System (INIS)

    Zaluzec, N.J.

    1979-06-01

    An in-situ study of the as-quenched omega phase transformation in Zr--15% Nb was conducted between the temperatures of 77 and 300 0 K using analytical electron microscopy. The domain size of the omega regions observed in this investigation was on the order of 30 A, consistent with previous observations in this system. No alignment of omega domains along directions of the bcc lattice was observed and in-situ thermal cycling experiments failed to produce a long period structure of alternating β and ω phase regions as predicted by one theory of this transformation. Several techniques of microstructural analysis were developed, refined, and standardized. Grouped under the general classification of Analytical Electron Microscopy (AEM) they provide the experimentalist with a unique tool for the microcharacterization of solids, allowing semiquantitative to quantitative analysis of the morphology, crystallography, elemental composition, and electronic structure of regions as small as 20 A in diameter. These techniques have complications, and it was necessary to study the AEM system used in this work so that instrumental artifacts which invalidate the information produced in the microscope environment might be eliminated. Once these factors had been corrected, it was possible to obtain a wealth of information about the microvolume of material under investigation. The microanalytical techniques employed during this research include: energy dispersive x-ray spectroscopy (EDS) using both conventional and scanning transmission electron microscopy (CTEM, STEM), transmission scanning electron diffraction (TSED), the stationary diffraction pattern technique, and electron energy loss spectroscopy (ELS) using a dedicated scanning transmission electron microscope

  14. Experimental Observations of In-Situ Secondary Electron Yield Reduction in the PEP-II Particle Accelerator Beam Line

    International Nuclear Information System (INIS)

    Pivi, Mauro

    2010-01-01

    Beam instability caused by the electron cloud has been observed in positron and proton storage rings and it is expected to be a limiting factor in the performance of the positron Damping Ring (DR) of future Linear Colliders (LC) such as ILC and CLIC. To test a series of promising possible electron cloud mitigation techniques as surface coatings and grooves, in the Positron Low Energy Ring (LER) of the PEP-II accelerator, we have installed several test vacuum chambers including (i) a special chamber to monitor the variation of the secondary electron yield of technical surface materials and coatings under the effect of ion, electron and photon conditioning in situ in the beam line; (ii) chambers with grooves in a straight magnetic-free section; and (iii) coated chambers in a dedicated newly installed 4-magnet chicane to study mitigations in a magnetic field region. In this paper, we describe the ongoing R and D effort to mitigate the electron cloud effect for the LC damping ring, focusing on the first experimental area and on results of the reduction of the secondary electron yield due to in situ conditioning.

  15. Styrene grafted natural rubber reinforced by in situ silica generated via sol–gel technique

    Energy Technology Data Exchange (ETDEWEB)

    Sittiphan, Torpong [Program of Petrochemistry and Polymer Sciences, Faculty of Science, Chulalongkorn University, Bangkok 10330 (Thailand); Prasassarakich, Pattarapan [Department of Chemical Technology, Faculty of Science, Chulalongkorn University, Bangkok 10330 (Thailand); Poompradub, Sirilux, E-mail: sirilux.p@chula.ac.th [Department of Chemical Technology, Faculty of Science, Chulalongkorn University, Bangkok 10330 (Thailand)

    2014-02-15

    Highlights: • Sol–gel reaction by NR latex was the absence of use of organic solvent and base catalyst. • Well dispersed in situ formed silica particles in the rubber matrix were obtained. • In situ silica was better to improve mechanical properties of rubber vulcanizates. -- Abstract: The filling of styrene graft natural rubber (ST-GNR) with in situ formed silica was performed using the sol–gel reaction via the latex solution method. The mechanical properties of ST-GNR/NR vulcanizate were improved when using the in situ formed silica to levels higher than those obtained with the commercial ex situ formed silica filled ST-GNR/NR vulcanizates at a comparable silica content of 12 parts by weight per hundred parts of rubber. Transmission electron microscopy analysis revealed that the in situ silica particles were small (∼40 nm diameter) and well dispersed, while the commercial silica particles were larger (∼60 nm diameter) and markedly agglomerated in the rubbery matrix. The mechanical properties of the composites prepared via both the solid rubber and latex solution methods were comparable.

  16. 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

  17. 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.

  18. 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...

  19. Electron transparent graphene windows for environmental scanning electron microscopy in liquids and dense gases.

    Science.gov (United States)

    Stoll, Joshua D; Kolmakov, Andrei

    2012-12-21

    Due to its ultrahigh electron transmissivity in a wide electron energy range, molecular impermeability, high electrical conductivity and excellent mechanical stiffness, suspended graphene membranes appear to be a nearly ideal window material for in situ (in vivo) environmental electron microscopy of nano- and mesoscopic objects (including bio-medical samples) immersed in liquids and/or in dense gaseous media. In this paper, taking advantage of a small modification of the graphene transfer protocol onto metallic and SiN supporting orifices, reusable environmental cells with exchangeable graphene windows have been designed. Using colloidal gold nanoparticles (50 nm) dispersed in water as model objects for scanning electron microscopy in liquids as proof of concept, different conditions for imaging through the graphene membrane were tested. Limiting factors for electron microscopy in liquids, such as electron beam induced water radiolysis and damage of the graphene membrane at high electron doses, are discussed.

  20. 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.

  1. Suppression of self-interstitials in silicon during ion implantation via in-situ photoexcitation

    International Nuclear Information System (INIS)

    Ravi, J.; Erokhin, Yu.; Christensen, K.; Rozgonyi, G.A.; Patnaik, B.K.; White, C.W.

    1995-02-01

    The influence of in-situ photoexcitation during low temperature implantation on self-interstitial agglomeration following annealing has been investigated using transmission electron microscopy (TEM). A reduction in the level of as-implanted damage determined by RBS and TEM occurs athermally during 150 keV self-ion implantation. The damage reduction following a 300 C anneal suggests that it is mostly divacancy related. Subsequent thermal annealing at 800 C resulted in the formation of (311) rod like defects or dislocation loops for samples with and without in-situ photoexcitation, respectively. Estimation of the number of self-interstitials bound by these defects in the sample without in-situ photoexcitation corresponds to the implanted dose; whereas for the in-situ photoexcitation sample a suppression of ∼2 orders in magnitude is found. The kinetics of the athermal annealing process are discussed within the framework of either a recombination enhanced defect reaction mechanism, or a charge state enhanced defect migration and Coulomb interaction

  2. In situ TEM observation of the Boudouard reaction: Multi-layered graphene formation from CO on cobalt nanoparticles at atmospheric pressure

    NARCIS (Netherlands)

    Bremmer, G.M.; Zacharaki, E.; Sjåstad, A.O.; Navarro, V.; Frenken, J.W.M.; Kooyman, P.J.

    2017-01-01

    Using a MEMS nanoreactor in combination with a specially designed in situ Transmission Electron Microscope (TEM) holder and gas supply system, we imaged the formation of multiple layers of graphene encapsulating a cobalt nanoparticle, at 1 bar CO:N2 (1:1) and 500 °C. The cobalt nanoparticle was

  3. 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

  4. 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.

  5. Electron microscopic studies of natural gas oxidation catalyst – Effects of thermally accelerated aging on catalyst microstructure

    DEFF Research Database (Denmark)

    Honkanen, Mari; Hansen, Thomas Willum; Jiang, Hua

    2017-01-01

    Structural changes of PtPd nanoparticles in a natural gas oxidation catalyst were studied at elevated temperatures in air and low-oxygen conditions and in situ using environmental transmission electron microscopy (ETEM). The fresh catalyst shows

  6. Irradiation-induced creep in metallic nanolaminates characterized by In situ TEM pillar nanocompression

    Energy Technology Data Exchange (ETDEWEB)

    Dillon, Shen J., E-mail: sdillon@illinois.edu [Department of Materials Science and Engineering, University of Illinois Urbana-Champagin, Urbana, IL 61801 (United States); Bufford, Daniel C. [Sandia National Laboratories, Albuquerque, NM 87185 (United States); Jawaharram, Gowtham S.; Liu, Xuying; Lear, Calvin [Department of Materials Science and Engineering, University of Illinois Urbana-Champagin, Urbana, IL 61801 (United States); Hattar, Khalid [Sandia National Laboratories, Albuquerque, NM 87185 (United States); Averback, Robert S. [Department of Materials Science and Engineering, University of Illinois Urbana-Champagin, Urbana, IL 61801 (United States)

    2017-07-15

    This work reports on irradiation-induced creep (IIC) measured on nanolaminate (Cu-W and Ni-Ag) and nanocrystalline alloys (Cu-W) at room temperature using a combination of heavy ion irradiation and nanopillar compression performed concurrently in situ in a transmission electron microscope. Appreciable IIC is observed in multilayers with 50 nm layer thicknesses at high stress, ≈½ the yield strength, but not in multilayers with only 5 nm layer thicknesses.

  7. Polyaniline-coated halloysite nanotubes via in-situ chemical polymerization

    Energy Technology Data Exchange (ETDEWEB)

    Zhang Long [State Key Laboratory of Applied Organic Chemistry and Institute of Polymer Science and Engineering, College of Chemistry and Chemical Engineering, Lanzhou University, Lanzhou 730000 (China); Wang Tingmei [State Key Laboratory of Solid Lubrication, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000 (China); Liu Peng [State Key Laboratory of Applied Organic Chemistry and Institute of Polymer Science and Engineering, College of Chemistry and Chemical Engineering, Lanzhou University, Lanzhou 730000 (China)], E-mail: pliu@lzu.edu.cn

    2008-12-30

    Polyaniline coated halloysite nanotubes (PANI/HNTs) were prepared by the in-situ soapless emulsion polymerization of the anilinium chloride adsorbed halloysite nanotubes (HNTs), obtained by the dispersion of HNTs in acidic aqueous solution of aniline with magnetic stirring and ultrasonic irradiation, by using ammonium persulfate (APS) as oxidant. The effect of the acidities of the polymerizing media on the crystal structure of the nanotubes was investigated with X-ray diffraction (XRD) technique. The surface conducting coatings of the hybrids were characterized with X-ray photoelectron spectroscopy (XPS). The morphological analyses showed that the polyaniline coated halloysite nanotubes via the in-situ chemical oxidation polymerization with ultrasonic irradiation had the better well-defined structures, by the transmission electron microscopy (TEM). The conductivities of the PANI/HNTs hybrids increased with the increasing of the amounts of HCl dopant added in the emulsion polymerization.

  8. Polyaniline-coated halloysite nanotubes via in-situ chemical polymerization

    International Nuclear Information System (INIS)

    Zhang Long; Wang Tingmei; Liu Peng

    2008-01-01

    Polyaniline coated halloysite nanotubes (PANI/HNTs) were prepared by the in-situ soapless emulsion polymerization of the anilinium chloride adsorbed halloysite nanotubes (HNTs), obtained by the dispersion of HNTs in acidic aqueous solution of aniline with magnetic stirring and ultrasonic irradiation, by using ammonium persulfate (APS) as oxidant. The effect of the acidities of the polymerizing media on the crystal structure of the nanotubes was investigated with X-ray diffraction (XRD) technique. The surface conducting coatings of the hybrids were characterized with X-ray photoelectron spectroscopy (XPS). The morphological analyses showed that the polyaniline coated halloysite nanotubes via the in-situ chemical oxidation polymerization with ultrasonic irradiation had the better well-defined structures, by the transmission electron microscopy (TEM). The conductivities of the PANI/HNTs hybrids increased with the increasing of the amounts of HCl dopant added in the emulsion polymerization.

  9. Third generation hybrid drive. Transmission-based integration of power electronics; Dritte Generation Hybridantrieb. Getriebenahe Integration der Leistungselektronik

    Energy Technology Data Exchange (ETDEWEB)

    Schoen, Wolfgang [ZF Friedrichshafen AG, Friedrichshafen (DE). Hybridantriebe (F und E); Lutz, Steffen [BMW AG, Muenchen (Germany); Hensler, Alexander [Technische Univ. Chemnitz (Germany); Munding, Andreas [Liebherr Elektronik GmbH, Lindau (Germany); Thoben, Markus [Infineon Technologies AG, Warstein (Germany); Zeidler, Dietmar [Kemet Electronics GmbH, Landsberg am Lech (Germany)

    2011-06-15

    The power electronics components in today's hybrid vehicles are situated at different places in the vehicle - till now far away from harsh and hot surroundings. In order to develop an integrated solution near the transmission, ZF and BMW launched the research project 'Electric components for active power transmissions' (EfA). On the basis of an eight-speed full hybrid transmission and together with Infineon, Kemet, Liebherr, and the University of Technology of Chemnitz, they are developing a power electronics unit, which facilitates doubling the power density while increasing the operating temperature. The project EfA will be concluded in June 2011. (orig.)

  10. 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

  11. 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.

  12. Behaviour of TEM metal grids during in-situ heating experiments.

    Science.gov (United States)

    Zhang, Zaoli; Su, Dangsheng

    2009-05-01

    The stability of Ni, Cu, Mo and Au transmission electron microscope (TEM) grids coated with ultra-thin amorphous carbon (alpha-C) or silicon monoxide film is examined by in-situ heating up to a temperature in the range 500-850 degrees C in a transmission electron microscope. It is demonstrated that some grids can generate nano-particles either due to the surface diffusion of metal atoms on amorphous film or due to the metal evaporation/redeposition. The emergence of nano-particles can complicate experimental observations, particularly in in-situ heating studies of dynamic behaviours of nano-materials in TEM. The most widely used Cu grid covered with amorphous carbon is unstable, and numerous Cu nano-particles start to form once the heating temperature reaches 600 degrees C. In the case of Ni grid covered with alpha-C film, a large number of Ni nano-crystals occur immediately when the temperature approaches 600 degrees C, accompanied by the graphitization of amorphous carbon. In contrast, both Mo and Au grids covered with alpha-C film exhibit good stability at elevated temperature, for instance, up to 680 and 850 degrees C for Mo and Au, respectively, and any other metal nano-particles are detected. Cu grid covered Si monoxide thin film is stable up to 550 degrees C, but Si nano-crystals appear under intensive electron beam. The generated nano-particles are well characterized by spectroscopic techniques (EDXS/EELS) and high-resolution TEM. The mechanism of nano-particle formation is addressed based on the interactions between the metal grid and the amorphous carbon film and on the sublimation of metal.

  13. In situ investigation of ordering phase transformations in FePt magnetic nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Wittig, James E., E-mail: j.wittig@vanderbilt.edu [Interdisciplinary Materials Science, Vanderbilt University, PMB 351683, 2301 Vanderbilt Place, Nashville, TN 37232 (United States); Bentley, James, E-mail: bentleyj48@gmail.com [Materials Science and Technology Division, Oak Ridge National Laboratory, PO Box 2008, Oak Ridge, TN 37831-6376 (United States); Allard, Lawrence F., E-mail: allardlfjr@ornl.gov [Materials Science and Technology Division, Oak Ridge National Laboratory, PO Box 2008, Oak Ridge, TN 37831-6376 (United States)

    2017-05-15

    In situ high-resolution electron microscopy was used to reveal information at the atomic level for the disordered-to-ordered phase transformation of equiatomic FePt nanoparticles that can exhibit outstanding magnetic properties after transforming from disordered face-centered-cubic into the tetragonal L1{sub 0} ordered structure. High-angle annular dark-field imaging in the scanning transmission electron microscope provided sufficient contrast between the Fe and Pt atoms to readily monitor the ordering of the atoms during in situ heating experiments. However, during continuous high-magnification imaging the electron beam influenced the kinetics of the transformation so annealing had to be performed with the electron beam blanked. At 500 °C where the reaction rate was relatively slow, observation of the transformation mechanisms using this sequential imaging protocol revealed that ordering proceeded from (002) surface facets but was incomplete and multiple-domain particles were formed that contained anti-phase domain boundaries and anti-site defects. At 600 and 700 °C, the limitations of sequential imaging were revealed as a consequence of increased transformation kinetics. Annealing for only 5 min at 700 °C produced complete single-domain L1{sub 0} order; such single-domain particles were more spherical in shape with (002) facets. The in situ experiments also provided information concerning nanoparticle sintering, coalescence, and consolidation. Although there was resistance to complete sintering due to the crystallography of L1{sub 0} order, the driving force from the large surface-area-to-volume ratio resulted in considerable nanoparticle coalescence, which would render such FePt nanoparticles unsuitable for use as magnetic recording media. Comparison of the in situ data acquired using the protocol described above with parallel ex situ annealing experiments showed that identical behavior resulted in all cases. - Highlights: • HAADF STEM imaging reveals the

  14. Transmission microscopy of unmodified biological materials: comparative radiation dosages with electrons and ultrasoft X-ray photons

    International Nuclear Information System (INIS)

    Sayre, D.; Feder, R.; Spiller, E.; Kirz, J.; Kim, D.M.

    1977-01-01

    The minimum radiation dosage in a specimen consistent with transmission microscopy at resolution d and specimen thickness t is calculated for model specimens resembling biological materials in their natural state. The calculations cover 10 4 -10 7 eV electrons and 1.3-90 A photons in a number of microscopy modes. The results indicate that over a considerable part of the (t,d)-plane transmission microscopy on such specimens can be carried out at lower dosage with photons than with electrons. Estimates of the maximum resolutions obtainable with electrons and photons, consistent with structural survival of the specimen, are obtained, as are data on optimal operating conditions for microscopy with the two particles

  15. 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.

  16. 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

  17. 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

  18. 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)

  19. 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

  20. 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

  1. 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.

  2. 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.

  3. 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.

  4. 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

  5. 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.

  6. Damage and in-situ annealing during ion implantation

    International Nuclear Information System (INIS)

    Sadana, D.K.; Washburn, J.; Byrne, P.F.; Cheung, N.W.

    1982-11-01

    Formation of amorphous (α) layers in Si during ion implantation in the energy range 100 keV-11 MeV and temperature range liquid nitrogen (LN)-100 0 C has been investigated. Cross-sectional transmission electron microscopy (XTEM) shows that buried amorphous layers can be created for both room temperature (RT) and LN temperature implants, with a wider 100 percent amorphous region for the LN cooled case. The relative narrowing of the α layer during RT implantation is attributed to in-situ annealing. Implantation to the same fluence at temperatures above 100 0 C does not produce α layers. To further investigate in situ annealing effects, specimens already containing buried α layers were further irradiated with ion beams in the temperature range RT-400 0 C. It was found that isolated small α zones (less than or equal to 50 diameter) embedded in the crystalline matrix near the two α/c interfaces dissolved into the crystal but the thickness of the 100 percent α layer was not appreciably affected by further implantation at 200 0 C. A model for in situ annealing during implantation is presented

  7. Observation of superconducting fluxons by transmission electron microscopy: A Fourier space approach to calculate the electron optical phase shifts and images

    International Nuclear Information System (INIS)

    Beleggia, M.; Pozzi, G.

    2001-01-01

    An approach is presented for the calculation of the electron optical phase shift experienced by high-energy electrons in a transmission electron microscope, when they interact with the magnetic field associated with superconducting fluxons in a thin specimen tilted with respect to the beam. It is shown that by decomposing the vector potential in its Fourier components and by calculating the phase shift of each component separately, it is possible to obtain the Fourier transform of the electron optical phase shift, which can be inverted either analytically or numerically. It will be shown how this method can be used to recover the result, previously obtained by the real-space approach, relative to the case of a straight flux tube perpendicular to the specimen surfaces. Then the method is applied to the case of a London fluxon in a thin film, where the bending and the broadening of the magnetic-field lines due to the finite specimen thickness are now correctly taken into account and not treated approximately by means of a parabolic fit. Finally, it will be shown how simple models for the pancake structure of the fluxon can be analyzed within this framework and the main features of electron transmission images predicted

  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. 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.

  10. 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.

  11. Determination of the cork bark porosity through the gamma ray transmission technology and electronic scanning microscopy image analysis

    International Nuclear Information System (INIS)

    Moraes, Antonio M.C.; Moreira, Anderson C.; Appoloni, Carlos R.

    2007-01-01

    This work applies the gamma transmission techniques (GTR) and imaging by scanning electron microscopy (SEM) for determination of porosity in the sparkling wine bottle corks. The gamma transmission experimental apparatus consists of a micrometric table (ZX) of sample movement automated, a Am-241 source (59,53 keV, 100 mCi), lead collimators, sample-holder, Na I(Tl) detector and appropriated electronics. For the microscopic images an FEI (Quanta 200), electronic microscope with associated electronics was used, and the image analysis was performed with IMAGO software. The average porosity for 22 samples analysed by GTR was of φ=58 +- 4.6 percent. By the imaging technique the found average porosity was φ=60.0 +- 6.2 percent. (author)

  12. Theoretical study of the transmission of low-energy (0-10 eV) electrons through thin-film organic molecular solids: benzene

    International Nuclear Information System (INIS)

    Goulet, T.; Jay-Gerin, J.-P.

    1986-01-01

    A theoretical study of the transmission of low-energy (0 to 10 eV) electrons incident from vacuum through thin-film organic molecular solids deposited on a cold metal substrate is presented and developed for the specific case of solid benzene. In essence, using a semiclassical description of electron transport in solids with an energy-independent scattering mean free path and assuming an isotropic electron scattering, the behavior of a penetrating electron in the film is simulated when a large number of scattering events are present. The good agreement between the calculated electron transmission spectra and those obtained experimentally indicates that our study provides a realistic description of the electron transport in the film, and accounts for the influence of the various electron-molecule scattering processes upon the energy dependence of the transmitted current. In particular, we show that the excitonic subionization energy losses are at the origin of the main structures of the observed electron transmission spectra. It is also shown that our study can successfully be used to estimate the probabilities of the various electron scattering processes which occur in the film, as well as the electron mean free path (l). For solid benzene, l is about 8 A in the considered electron energy range. (author)

  13. 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.

  14. Attraction of semiconductor nanowires: An in situ observation

    International Nuclear Information System (INIS)

    Chen, Bin; Gao, Qiang; Chang, Li; Wang, Yanbo; Chen, Zibin; Liao, Xiaozhou; Tan, Hark Hoe; Zou, Jin; Ringer, Simon P.; Jagadish, Chennupati

    2013-01-01

    Graphical abstract: -- Abstract: In situ deformation transmission electron microscopy was used to study the attraction behavior of GaAs semiconductor nanowires (NWs). The NWs demonstrated an interesting phenomenon of either head-to-head or body-to-body attraction at distances that depend on the NW diameters. The NWs with a diameter of ∼25 nm attracted at a distance of ∼25 nm, while large-diameter NWs of ∼55 nm showed no obvious attraction. The underlying mechanism governing the attraction of the NWs is proposed and discussed with a mechanistic model. The diameter dependence on the NW attraction behavior is discussed. The finding provides an understanding of the Ampère force in nanostructured materials caused by an electron-beam-induced current while technologically it provides useful hints for designing NW-based devices according to the diameter-dependent attraction behavior of NWs

  15. 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.

  16. 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...

  17. Electron-beam-irradiation-induced crystallization of amorphous solid phase change materials

    Science.gov (United States)

    Zhou, Dong; Wu, Liangcai; Wen, Lin; Ma, Liya; Zhang, Xingyao; Li, Yudong; Guo, Qi; Song, Zhitang

    2018-04-01

    The electron-beam-irradiation-induced crystallization of phase change materials in a nano sized area was studied by in situ transmission electron microscopy and selected area electron diffraction. Amorphous phase change materials changed to a polycrystalline state after being irradiated with a 200 kV electron beam for a long time. The results indicate that the crystallization temperature strongly depends on the difference in the heteronuclear bond enthalpy of the phase change materials. The selected area electron diffraction patterns reveal that Ge2Sb2Te5 is a nucleation-dominated material, when Si2Sb2Te3 and Ti0.5Sb2Te3 are growth-dominated materials.

  18. One-step synthesis of graphene/polyaniline hybrids by in situ intercalation polymerization and their electromagnetic properties

    Science.gov (United States)

    Chen, Xiangnan; Meng, Fanchen; Zhou, Zuowan; Tian, Xin; Shan, Liming; Zhu, Shibu; Xu, Xiaoling; Jiang, Man; Wang, Li; Hui, David; Wang, Yong; Lu, Jun; Gou, Jihua

    2014-06-01

    A new method is introduced for the preparation of graphene/polyaniline hybrids using a one-step intercalation polymerization of aniline inside the expanded graphite. The structural and morphological characterizations were performed by X-ray diffraction analysis, transmission electron microscopy and field emission scanning electron microscopy. Both the experimental and first-principles simulated results show that the aniline cation formed by aniline and H+ tends to be drawn towards the electron-enriched zone and to intercalate into the interlayer of graphite. Subsequently, an in situ polymerization leads to the separation of graphite into graphene sheet, resulting from the exothermic effect and more vigorous movements of the chain molecules of polyaniline. The interactions between polyaniline and graphene were confirmed by Fourier transform infrared spectroscopy and Raman spectra. In addition, the graphene/polyaniline hybrid exhibited a breakthrough in the improvement of microwave absorption.A new method is introduced for the preparation of graphene/polyaniline hybrids using a one-step intercalation polymerization of aniline inside the expanded graphite. The structural and morphological characterizations were performed by X-ray diffraction analysis, transmission electron microscopy and field emission scanning electron microscopy. Both the experimental and first-principles simulated results show that the aniline cation formed by aniline and H+ tends to be drawn towards the electron-enriched zone and to intercalate into the interlayer of graphite. Subsequently, an in situ polymerization leads to the separation of graphite into graphene sheet, resulting from the exothermic effect and more vigorous movements of the chain molecules of polyaniline. The interactions between polyaniline and graphene were confirmed by Fourier transform infrared spectroscopy and Raman spectra. In addition, the graphene/polyaniline hybrid exhibited a breakthrough in the improvement of

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

    DEFF Research Database (Denmark)

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

    2012-01-01

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

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

    International Nuclear Information System (INIS)

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

    2016-01-01

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

  1. In situ deposition of hydroxyapatite on graphene nanosheets

    International Nuclear Information System (INIS)

    Neelgund, Gururaj M.; Oki, Aderemi; Luo, Zhiping

    2013-01-01

    Graphical abstract: A facile chemical precipitation method is reported for effective in situ deposition of hydroxyapatite on graphene nanosheets. Prior to grafting of hydroxyapatite, chemically modified graphene nanosheets were obtained by the reduction of graphene oxide in presence of ethylenediamine. Display Omitted Highlights: ► It is a facile and effective method for deposition of HA on GR nanosheets. ► It avoids the use of harmful reducing agents like hydrazine, NaBH 4 etc. ► GR nanosheets were produced using bio-compatible, ethylenediamine. ► The graphitic structure of synthesized GR nanosheets was high ordered. ► The ratio of Ca to P in HA was 1.64, which is close to ratio in natural bone. -- Abstract: Graphene nanosheets were effectively functionalized by in situ deposition of hydroxyapatite through a facile chemical precipitation method. Prior to grafting of hydroxyapatite, chemically modified graphene nanosheets were obtained by the reduction of graphene oxide in presence of ethylenediamine. The resulting hydroxyapatite functionalized graphene nanosheets were characterized by attenuated total reflection IR spectroscopy, X-ray diffraction, field emission scanning electron microscopy, transmission electron microscopy, X-ray energy dispersive spectroscopy, Raman spectroscopy and thermogravimetric analysis. These characterization techniques revealed the successful grafting of hydroxyapatite over well exfoliated graphene nanosheets without destroying their structure.

  2. In situ deposition of hydroxyapatite on graphene nanosheets

    Energy Technology Data Exchange (ETDEWEB)

    Neelgund, Gururaj M. [Department of Chemistry, Prairie View A and M University, Prairie View, TX 77446 (United States); Oki, Aderemi, E-mail: aroki@pvamu.edu [Department of Chemistry, Prairie View A and M University, Prairie View, TX 77446 (United States); Luo, Zhiping [Microscopy and Imaging Center and Materials Science and Engineering Program, Texas A and M University, College Station, TX 77843 (United States)

    2013-02-15

    Graphical abstract: A facile chemical precipitation method is reported for effective in situ deposition of hydroxyapatite on graphene nanosheets. Prior to grafting of hydroxyapatite, chemically modified graphene nanosheets were obtained by the reduction of graphene oxide in presence of ethylenediamine. Display Omitted Highlights: ► It is a facile and effective method for deposition of HA on GR nanosheets. ► It avoids the use of harmful reducing agents like hydrazine, NaBH{sub 4} etc. ► GR nanosheets were produced using bio-compatible, ethylenediamine. ► The graphitic structure of synthesized GR nanosheets was high ordered. ► The ratio of Ca to P in HA was 1.64, which is close to ratio in natural bone. -- Abstract: Graphene nanosheets were effectively functionalized by in situ deposition of hydroxyapatite through a facile chemical precipitation method. Prior to grafting of hydroxyapatite, chemically modified graphene nanosheets were obtained by the reduction of graphene oxide in presence of ethylenediamine. The resulting hydroxyapatite functionalized graphene nanosheets were characterized by attenuated total reflection IR spectroscopy, X-ray diffraction, field emission scanning electron microscopy, transmission electron microscopy, X-ray energy dispersive spectroscopy, Raman spectroscopy and thermogravimetric analysis. These characterization techniques revealed the successful grafting of hydroxyapatite over well exfoliated graphene nanosheets without destroying their structure.

  3. 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

  4. 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...

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

    DEFF Research Database (Denmark)

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

    2016-01-01

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

  6. 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...

  7. 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.

  8. Automated magnification calibration in transmission electron microscopy using Fourier analysis of replica images

    International Nuclear Information System (INIS)

    Laak, Jeroen A.W.M. van der; Dijkman, Henry B.P.M.; Pahlplatz, Martin M.M.

    2006-01-01

    The magnification factor in transmission electron microscopy is not very precise, hampering for instance quantitative analysis of specimens. Calibration of the magnification is usually performed interactively using replica specimens, containing line or grating patterns with known spacing. In the present study, a procedure is described for automated magnification calibration using digital images of a line replica. This procedure is based on analysis of the power spectrum of Fourier transformed replica images, and is compared to interactive measurement in the same images. Images were used with magnification ranging from 1,000x to 200,000x. The automated procedure deviated on average 0.10% from interactive measurements. Especially for catalase replicas, the coefficient of variation of automated measurement was considerably smaller (average 0.28%) compared to that of interactive measurement (average 3.5%). In conclusion, calibration of the magnification in digital images from transmission electron microscopy may be performed automatically, using the procedure presented here, with high precision and accuracy

  9. 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

  10. Cathode-Control Alloying at an Au-ZnSe Nanowire Contact via in Situ Joule Heating

    International Nuclear Information System (INIS)

    Zeng Ya-Ping; Qu Bai-Hua; Yu Hong-Chun; Wang Yan-Guo

    2012-01-01

    Controllable interfacial alloying is achieved at a Au-ZnSe nanowire (M-S) contact via in situ Joule heating inside transmission electron microscopy (TEM). TEM inspection reveals that the Au electrode is locally molten at the M-S contact and the tip of the ZnSe nanowire is covered by the Au melting. Experimental evidences confirm that the alloying at the reversely biased M-S contact is due to the high resistance of the Schottky barrier at this M-S contact, coincident to cathode-control mode. Consequently, in situ Joule heating can be an effective method to improve the performance of nanoelectronics based on a metal-semiconductor-metal nanostructure. (cross-disciplinary physics and related areas of science and technology)

  11. 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.

  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. 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

  15. 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

  16. In Situ TEM Creation and Electrical Characterization of Nanowire Devices

    DEFF Research Database (Denmark)

    Kallesøe, Christian; Wen, Cheng-Yen; Booth, Timothy J.

    2012-01-01

    bridge devices in situ and relate these to the structure. We also describe processes to modify the contact and the nanowire surface after device formation. The technique we describe allows the direct analysis of the processes taking place during device formation and use, correlating specific nanoscale......We demonstrate the observation and measurement of simple nanoscale devices over their complete lifecycle from creation to failure within a transmission electron microscope. Devices were formed by growing Si nanowires, using the vapor–liquid–solid method, to form bridges between Si cantilevers. We...... structural and electrical parameters on an individual device basis....

  17. 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.

  18. 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

  19. 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...

  20. 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...

  1. Electrochemical migration of tin in electronics and microstructure of the dendrites

    DEFF Research Database (Denmark)

    Minzari, Daniel; Grumsen, Flemming Bjerg; Jellesen, Morten Stendahl

    2011-01-01

    The macro-, micro-, and nano-scale morphology and structure of tin dendrites, formed by electrochemical migration on a surface mount ceramic chip resistor having electrodes consisting of tin with small amounts of Pb (∼2wt.%) was investigated by scanning electron microscopy and transmission electr...... by the dehydration of the hydrated oxide originally formed in solution ex-situ in ambient air.......The macro-, micro-, and nano-scale morphology and structure of tin dendrites, formed by electrochemical migration on a surface mount ceramic chip resistor having electrodes consisting of tin with small amounts of Pb (∼2wt.%) was investigated by scanning electron microscopy and transmission electron...... microscopy including Energy dispersive X-ray spectroscopy and electron diffraction. The tin dendrites were formed under 5 or 12V potential bias in 10ppm by weight NaCl electrolyte as a micro-droplet on the resistor during electrochemical migration experiments. The dendrites formed were found to have...

  2. 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

  3. 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.

  4. Spectroscopic studies of organic-inorganic composite film cured by low energy electron beam

    International Nuclear Information System (INIS)

    Mahathir Mohamed; Dahlan Mohd; Ibrahim Abdullah; Eda Yuhana Ariffin

    2009-01-01

    Liquid epoxidized natural rubber acrylate (LENRA) film was reinforced with silica particles formed in-situ via sol gel process. Combination of these two components produces organic-inorganic composites. Tetraethyl orthosilicate (TEOS) was used as precursor material for silica generation. Sol gel reactions was carried out at different concentrations of TEOS i.e. between 10 and 50 phr. The compounds that contain silica were crosslinked by electron beam. Structural properties studies were carried out by Fourier Transform Infrared Spectrometer (FTIR). It was found that miscibility between organic and inorganic components improved with the presence of silanol groups (Si-OH) and polar solvent i.e. THF, via hydrogen bonding formation between siloxane and LENRA. Morphology study by the transmission electron microscopy (TEM) and scanning electron microscopy (SEM) showed in-situ generated silica particles were homogenous and well dispersed at any concentrations of TEOS. (author)

  5. In situ observation of triple junction motion during recovery of heavily deformed aluminum

    DEFF Research Database (Denmark)

    Yu, Tianbo; Hughes, Darcy A.; Hansen, Niels

    2015-01-01

    -junctions are pinned by deformation-induced interconnecting and lamellar boundaries, which slow down the recovery process and lead to a stop-go migration pattern. This pinning mechanism stabilizes the deformation microstructure, i.e. the structure is stabilized by balancing the driving and pinning forces controlling......Microstructural evolution during in situ annealing of heavily cold-rolled aluminum has been studied by transmission electron microscopy, confirming that an important recovery mechanism is migration of triple junctions formed by three lamellar boundaries (Y-junctions). The migrating Y...

  6. In situ preparation of magnetic nanocomposites of goethite in a styrene-maleimide copolymer template

    International Nuclear Information System (INIS)

    Sepulveda-Guzman, S.; Perez-Camacho, O.; Rodriguez-Fernandez, O.; Garcia-Zamora, M.

    2005-01-01

    Magnetic composites were prepared by in situ precipitation of α-FeOOH (goethite) using a new styrene-co-N-4 carboxybutylmaleimide cross-linked copolymer as template. Thermogravimetric analysis showed iron oxide content in the composites up to 45%. The iron oxide phase was identified as goethite by X-ray diffraction analysis. Transmission electron microscopy revealed that the crosslinking extent of polymeric templates affected both the shape and dimension of the goethite particles, and consequently, the magnetic behavior of the polymer/iron oxide composites

  7. In-situ deformation studies of an aluminum metal-matrix composite in a scanning electron microscope

    Science.gov (United States)

    Manoharan, M.; Lewandowski, J. J.

    1989-01-01

    Tensile specimens made of a metal-matrix composite (cast and extruded aluminum alloy-based matrix reinforced with Al2O3 particulate) were tested in situ in a scanning electron microscope equipped with a deformation stage, to directly monitor the crack propagation phenomenon. The in situ SEM observations revealed the presence of microcracks both ahead of and near the crack-tip region. The microcracks were primarily associated with cracks in the alumina particles. The results suggest that a region of intense deformation exists ahead of the crack and corresponds to the region of microcracking. As the crack progresses, a region of plastically deformed material and associated microcracks remains in the wake of the crack.

  8. High temperature in-situ observations of multi-segmented metal nanowires encapsulated within carbon nanotubes by in-situ filling technique.

    Science.gov (United States)

    Hayashi, Yasuhiko; Tokunaga, Tomoharu; Iijima, Toru; Iwata, Takuya; Kalita, Golap; Tanemura, Masaki; Sasaki, Katsuhiro; Kuroda, Kotaro

    2012-08-08

    Multi-segmented one-dimensional metal nanowires were encapsulated within carbon nanotubes (CNTs) through in-situ filling technique during plasma-enhanced chemical vapor deposition process. Transmission electron microscopy (TEM) and environmental TEM were employed to characterize the as-prepared sample at room temperature and high temperature. The selected area electron diffractions revealed that the Pd4Si nanowire and face-centered-cubic Co nanowire on top of the Pd nanowire were encapsulated within the bottom and tip parts of the multiwall CNT, respectively. Although the strain-induced deformation of graphite walls was observed, the solid-state phases of Pd4Si and Co-Pd remain even at above their expected melting temperatures and up to 1,550 ± 50°C. Finally, the encapsulated metals were melted and flowed out from the tip of the CNT after 2 h at the same temperature due to the increase of internal pressure of the CNT.

  9. 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.

  10. 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.

  11. Total electron content measurements at Gauhati using 140 MHz ATS-6 transmissions

    International Nuclear Information System (INIS)

    Tyagi, T.R.; Singh, L.; Minakshi Devi; Barbara, A.K.

    1977-01-01

    The amplitude and phase of 140 MHz transmissions from geostationary satellite ATS-6 (0 0 N, 35 0 E) have been recorded at Gauhati (26.16 0 N; 91.75 0 E) for the period Nov. 1975 to Aug. 1976. The calibration technique for geostationary satellite Faraday rotation measurements suggested by Checcacci and Giorgeo has been improved and generalized. It is then utilized to remove the n ambiguity in Faraday rotation values and also to estimate the correct value of diurnal minimum Faraday rotation angle so that the recorded Faraday rotation values can be converted into electron content values. Typical diurnal variation curves have been obtained for all the months except for equinoxes when the satellite transmission was off very often due to ecliptic conditions and hence no complete diurnal curves could be obtained for these months. It has been found that though December and January behave like typical winter months, the month of November is more like an equinoctial month. Similarly, though June and July behave like typical summer months, the month of May is more or less similar to equinoxes. The characteristic features of the diurnal and seasonal behaviour of the electron content have been discussed. (author)

  12. 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.)

  13. 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

  14. 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

  15. 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

  16. 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)

  17. 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.

  18. Number transmission of 0.6 and 0.8MeV electrons in elemental materials

    International Nuclear Information System (INIS)

    Harami, Taikan; Takagaki, Torao; Matsuda, Koji; Nakai, Yohta.

    1975-01-01

    The number transmissions of electrons in Be, Al, Cu and Ag were obtained experimentally for well collimated electron beams of 0.6 and 0.8 MeV. Experimental results of the present work join smoothly to the previous ones of 1.0 MeV to 2.0 MeV electrons. The ratios of extrapolated range Rsub(ex) to true range R 0 give generally minimum values near 1 MeV (approximately 2mc 2 ) as well as the stopping power. An investigation was done for empirical equation of the form eta=exp(-xP/CEsup(m)), where E is the incident electron energy, x, penetration depth, and p, C and m are the parameters determined from experimental data. (author)

  19. 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.

  20. 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

  1. 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...

  2. 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

  3. 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

  4. 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)

  5. Biological Applications and Transmission Electron Microscopy Investigations of Mesoporous Silica Nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Trewyn, Brian G. [Iowa State Univ., Ames, IA (United States)

    2006-01-01

    The research presented and discussed within involves the development of novel biological applications of mesoporous silica nanoparticles (MSN) and an investigation of mesoporous material by transmission electron microscopy (TEM). Mesoporous silica nanoparticles organically functionalized shown to undergo endocytosis in cancer cells and drug release from the pores was controlled intracellularly and intercellularly. Transmission electron microscopy investigations demonstrated the variety of morphologies produced in this field of mesoporous silica nanomaterial synthesis. A series of room-temperature ionic liquid (RTIL) containing mesoporous silica nanoparticle (MSN) materials with various particle morphologies, including spheres, ellipsoids, rods, and tubes, were synthesized. By changing the RTIL template, the pore morphology was tuned from the MCM-41 type of hexagonal mesopores to rotational moire type of helical channels, and to wormhole-like porous structures. These materials were used as controlled release delivery nanodevices to deliver antibacterial ionic liquids against Escherichia coli K12. The involvement of a specific organosiloxane function group, covalently attached to the exterior of fluorescein doped mesoporous silica nanoparticles (FITC-MSN), on the degree and kinetics of endocytosis in cancer and plant cells was investigated. The kinetics of endocystosis of TEG coated FITC-MSN is significantly quicker than FITC-MSN as determined by flow cytometry experiments. The fluorescence confocal microscopy investigation showed the endocytosis of TEG coated-FITC MSN triethylene glycol grafted fluorescein doped MSN (TEG coated-FITC MSN) into both KeLa cells and Tobacco root protoplasts. Once the synthesis of a controlled-release delivery system based on MCM-41-type mesoporous silica nanorods capped by disulfide bonds with superparamagnetic iron oxide nanoparticles was completed. The material was characterized by general methods and the dosage and kinetics of the

  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. Electron-beam-induced-current and active secondary-electron voltage-contrast with aberration-corrected electron probes

    Energy Technology Data Exchange (ETDEWEB)

    Han, Myung-Geun, E-mail: mghan@bnl.gov [Condensed Matter Physics & Materials Science, Brookhaven National Laboratory, Upton, NY 11973 (United States); Garlow, Joseph A. [Condensed Matter Physics & Materials Science, Brookhaven National Laboratory, Upton, NY 11973 (United States); Materials Science and Engineering Department, Stony Brook University, Stony Brook, NY 11794 (United States); Marshall, Matthew S.J.; Tiano, Amanda L. [Department of Chemistry, Stony Brook University, Stony Brook, NY 11974 (United States); Wong, Stanislaus S. [Condensed Matter Physics & Materials Science, Brookhaven National Laboratory, Upton, NY 11973 (United States); Department of Chemistry, Stony Brook University, Stony Brook, NY 11974 (United States); Cheong, Sang-Wook [Department of Physics and Astronomy, Rutgers Center for Emergent Materials, Rutgers University, Piscataway, NJ 08854 (United States); Walker, Frederick J.; Ahn, Charles H. [Department of Applied Physics and Center for Research on Interface Structures and Phenomena, Yale University, New Haven, CT 06520 (United States); Department of Mechanical Engineering and Materials Science, Yale University, New Haven, CT 06520 (United States); Zhu, Yimei [Condensed Matter Physics & Materials Science, Brookhaven National Laboratory, Upton, NY 11973 (United States)

    2017-05-15

    Highlights: • Electron-beam-induced-current (EBIC) and active secondary-electron voltage-contrast (SE-VC) are demonstrated in STEM mode combined with in situ electrical biasing in a TEM. • Electrostatic potential maps in ferroelectric thin films, multiferroic nanowires, and single crystals obtained by off-axis electron holography were compared with EBIC and SE-VC data. • Simultaneous EBIC and active SE-VC performed with atomic resolution STEM are demonstrated. - Abstract: The ability to map out electrostatic potentials in materials is critical for the development and the design of nanoscale electronic and spintronic devices in modern industry. Electron holography has been an important tool for revealing electric and magnetic field distributions in microelectronics and magnetic-based memory devices, however, its utility is hindered by several practical constraints, such as charging artifacts and limitations in sensitivity and in field of view. In this article, we report electron-beam-induced-current (EBIC) and secondary-electron voltage-contrast (SE-VC) with an aberration-corrected electron probe in a transmission electron microscope (TEM), as complementary techniques to electron holography, to measure electric fields and surface potentials, respectively. These two techniques were applied to ferroelectric thin films, multiferroic nanowires, and single crystals. Electrostatic potential maps obtained by off-axis electron holography were compared with EBIC and SE-VC to show that these techniques can be used as a complementary approach to validate quantitative results obtained from electron holography analysis.

  8. HVEM in situ deformation of Al-Li-X alloys

    International Nuclear Information System (INIS)

    Crooks, R.E.; Kenik, E.A.; Starke, E.A. Jr.

    1983-01-01

    Lithium additions to aluminum alloys increase both the strength and elastic modulus while decreasing the density, thereby resulting in very attractive combinations of properties. The commercial utilization of these alloys, however, has been hindered by a lack of adequate ductility at peak strength. Recent investigations have attributed the low ductility to intense, localized deformation. This is considered to be due to the promotion of planar slip by coherent, shearable, delta' (Al 3 Li) precipitates and the presence of precipitate free zones (PFZ's) at high angle grain boundaries. An Al-Cu-Li-Mg-Zr alloy, produced by rapidly solidified powder processing, was found to exhibit ductility improvements over comparable, lithium-containing alloys. Thin foils prepared from bulk tensile samples were examined by transmission electron microscopy (TEM), and no evidence of localized deformation was found. These, however, were only successfully produced from the region of uniform elongation below the neck and were thus limited to approximately 4% plastic strain. In order to observe the deformation behavior under severe strain, an in situ deformation study was conducted in a high voltage electron microscope (HVEM). Several investigators have used in situ HVEM techniques to study ductile fracture processes. The advantages of HVEM versus TEM for this purpose include: thicker specimens (due to a lower energy exchange of the electrons), a lower specimen contamination rate and a negligible increase in specimen temperature. Two lithium-containing alloys which had been previously reported to demonstrate localized, planar slip were studied for comparison

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

    International Nuclear Information System (INIS)

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

    2016-01-01

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

  10. 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.

  11. 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

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

    International Nuclear Information System (INIS)

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

    2006-01-01

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

  13. 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.

  14. Quantitative in-situ TEM nanotensile testing of single crystal Ni facilitated by a new sample preparation approach.

    Science.gov (United States)

    Samaeeaghmiyoni, Vahid; Idrissi, Hosni; Groten, Jonas; Schwaiger, Ruth; Schryvers, Dominique

    2017-03-01

    Twin-jet electro-polishing and Focused Ion Beam (FIB) were combined to produce small size Nickel single crystal specimens for quantitative in-situ nanotensile experiments in the transmission electron microscope. The combination of these techniques allows producing samples with nearly defect-free zones in the centre in contrast to conventional FIB-prepared samples. Since TEM investigations can be performed on the electro-polished samples prior to in-situ TEM straining, specimens with desired crystallographic orientation and initial microstructure can be prepared. The present results reveal a dislocation nucleation-controlled plasticity, in which small loops induced by FIB near the edges of the samples play a central role. Copyright © 2016 Elsevier Ltd. All rights reserved.

  15. 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.

  16. In situ electron holography of electric potentials inside a solid-state electrolyte: Effect of electric-field leakage

    Energy Technology Data Exchange (ETDEWEB)

    Aizawa, Yuka; Yamamoto, Kazuo; Sato, Takeshi [Nanostructures Research Laboratory, Japan Fine Ceramics Center, 2-4-1 Mutsuno, Atsuta-ku, Nagoya, Aichi 456-8587 (Japan); Murata, Hidekazu [Faculty of Science and Technology, Meijo University, 1-501 Shiogamaguchi, Tempaku-ku, Nagoya, Aichi 468-8502 (Japan); Yoshida, Ryuji; Fisher, Craig A.J. [Nanostructures Research Laboratory, Japan Fine Ceramics Center, 2-4-1 Mutsuno, Atsuta-ku, Nagoya, Aichi 456-8587 (Japan); Kato, Takehisa; Iriyama, Yasutoshi [Department of Materials, Physics and Energy Engineering, Nagoya University, Furo-cho, Chikusa-ku, Nagoya, Aichi 464-8601 (Japan); Hirayama, Tsukasa, E-mail: t-hirayama@jfcc.or.jp [Nanostructures Research Laboratory, Japan Fine Ceramics Center, 2-4-1 Mutsuno, Atsuta-ku, Nagoya, Aichi 456-8587 (Japan)

    2017-07-15

    In situ electron holography is used to observe changes of electric-potential distributions in an amorphous lithium phosphorus oxynitride (LiPON) solid-state electrolyte when different voltages are applied. 2D phase images are simulated by integrating the 3D potential distribution along the electron trajectory through a thin Cu/LiPON/Cu region. Good agreement between experimental and simulated phase distributions is obtained when the influence of the external electric field is taken into account using the 3D boundary-charge method. Based on the precise potential changes, the lithium-ion and lithium-vacancy distributions inside the LiPON layer and electric double layers (EDLs) are inferred. The gradients of the phase drops at the interfaces in relation to EDL widths are discussed. - Highlights: • Solid-state electrolyte LiPON has been observed by in situ electron holography. • Observed phase distributions are compared with those simulated numerically. • 3D electric fields around the specimen are taken into account in the simulation. • Electric-potential distributions inside LiPON have been obtained. • The lithium-ion and lithium-vacancy distributions inside the LiPON are inferred.

  17. 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)

  18. 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

  19. Electron cyclotron waves transmission: new approach for the characterization of electron distribution functions in Tokamak hot plasmas; La transmission d`ondes cyclotroniques electroniques: une approche nouvelle pour caracteriser les fonctions de distribution electronique des plasmas chauds de Tokamak

    Energy Technology Data Exchange (ETDEWEB)

    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.

  20. 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

  1. 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

  2. In Situ Synthesis of Reduced Graphene Oxide and Gold Nanocomposites for Nanoelectronics and Biosensing

    Directory of Open Access Journals (Sweden)

    Chen Peng

    2011-01-01

    Full Text Available Abstract In this study, an in situ chemical synthesis approach has been developed to prepare graphene–Au nanocomposites from chemically reduced graphene oxide (rGO in aqueous media. UV–Vis absorption, atomic force microscopy, scanning electron microscopy, transmission electron microscopy, and Raman spectroscopy were used to demonstrate the successful attachment of Au nanoparticles to graphene sheets. Configured as field-effect transistors (FETs, the as-synthesized single-layered rGO-Au nanocomposites exhibit higher hole mobility and conductance when compared to the rGO sheets, promising its applications in nanoelectronics. Furthermore, we demonstrate that the rGO-Au FETs are able to label-freely detect DNA hybridization with high sensitivity, indicating its potentials in nanoelectronic biosensing.

  3. 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.)

  4. Unusual tensile behaviour of fibre-reinforced indium matrix composite and its in-situ TEM straining observation

    International Nuclear Information System (INIS)

    Luo, Xin; Peng, Jianchao; Zandén, Carl; Yang, Yanping; Mu, Wei; Edwards, Michael; Ye, Lilei; Liu, Johan

    2016-01-01

    Indium-based thermal interface materials are superior in thermal management applications of electronic packaging compared to their polymer-based counterparts. However, pure indium has rather low tensile strength resulting in poor reliability. To enhance the mechanical properties of such a material, a new composite consisting of electrospun randomly oriented continuous polyimide fibres and indium was fabricated. The composite has been characterised by tensile tests and in-situ transmission electron microscopy straining observations. It is shown that the composite's ultimate tensile strength at 20 °C is five times higher than that of pure indium, and the strength of the composite exceeds the summation of strengths of the individual components. Furthermore, contrary to most metallic matrix materials, the ultimate tensile strength of the composite decreases with the increased strain rate in a certain range. The chemical composition and tensile fracture of the novel composite have been analysed comprehensively by means of scanning transmission electron microscopy and scanning electron microscopy. A strengthening mechanism based on mutually reinforcing structures formed by the indium and surrounding fibres is also presented, underlining the effect of compressing at the fibre/indium interfaces by dislocation pileups and slip pinning.

  5. Deterministic Integration of Quantum Dots into on-Chip Multimode Interference Beamsplitters Using in Situ Electron Beam Lithography.

    Science.gov (United States)

    Schnauber, Peter; Schall, Johannes; Bounouar, Samir; Höhne, Theresa; Park, Suk-In; Ryu, Geun-Hwan; Heindel, Tobias; Burger, Sven; Song, Jin-Dong; Rodt, Sven; Reitzenstein, Stephan

    2018-04-11

    The development of multinode quantum optical circuits has attracted great attention in recent years. In particular, interfacing quantum-light sources, gates, and detectors on a single chip is highly desirable for the realization of large networks. In this context, fabrication techniques that enable the deterministic integration of preselected quantum-light emitters into nanophotonic elements play a key role when moving forward to circuits containing multiple emitters. Here, we present the deterministic integration of an InAs quantum dot into a 50/50 multimode interference beamsplitter via in situ electron beam lithography. We demonstrate the combined emitter-gate interface functionality by measuring triggered single-photon emission on-chip with g (2) (0) = 0.13 ± 0.02. Due to its high patterning resolution as well as spectral and spatial control, in situ electron beam lithography allows for integration of preselected quantum emitters into complex photonic systems. Being a scalable single-step approach, it paves the way toward multinode, fully integrated quantum photonic chips.

  6. Photonics-oriented data transmission network for the KM3NeT prototype detector

    International Nuclear Information System (INIS)

    Hoek, M. van der; Mos, S.; Schmelling, J.W.; Hogenbirk, J.; Heine, E.; Jansweijer, P.; Kieft, G.; Peek, H.; Timmer, P.; Wolf, E. de; Zwart, A.

    2013-01-01

    The design of the readout and data acquisition system of the future KM3NeT neutrino telescope employs 10 Gbps photonic technologies for data transmission to shore. The photonic architecture can handle standard transmission protocols. The generic scheme is based on DWDM technology using lasers on shore and optical modulators in each of the 12,800 Digital Optical Modules arranged on several hundred vertical detection units anchored to the seabed. Each module will house 31 photomultipliers together with auxiliary instrumentation and readout electronics. A 100 km electro-optical fibre cable will connect the optical modules to the store. The readout system will guarantee an individual optical connection between each optical module and the shore. A small-scale prototype of a detection unit with four optical modules is in a realization phase and will allow for in situ testing of the data transmission network. We will present results of laboratory tests of the photonics-oriented transmission layer of the network that have been realized for the prototype detection unit

  7. How to determine the morphology of plasmonic nanocrystals without transmission electron microscopy?

    Energy Technology Data Exchange (ETDEWEB)

    Battie, Yann, E-mail: yann.battie@univ-lorraine.fr [Université de Lorraine, LCP-A2MC, Institut Jean Barriol (France); Izquierdo-Lorenzo, Irene [Université de Technologie de Troyes, LNIO (CNRS UMR 6279) (France); Resano-Garcia, Amandine; Naciri, Aotmane En; Akil, Suzanna [Université de Lorraine, LCP-A2MC, Institut Jean Barriol (France); Adam, Pierre Michel; Jradi, Safi [Université de Technologie de Troyes, LNIO (CNRS UMR 6279) (France)

    2016-08-15

    This paper reports the complete ellipsometric characterization of gold nanoparticles (NPs) embedded in a photoresist films. The effective dielectric function of nanocomposite films as well as the shape distribution and the volume fraction of NPs are extracted from ellipsometric measurements by introducing an effective medium theory which takes into account the NP shape distribution and the intrinsic confinement effect. This theory remains valid as long as the nanoparticle interaction is negligible. We show that the magnitude of the confinement depends on the nanoparticle shape and the environment through chemical damping. This suggests that the NP shape distribution can be directly estimated by ellipsometry, while the determination of absolute radius distribution requires transmission electron microscopy measurements. The imaginary part of the effective dielectric function exhibits a strong asymmetric surface plasmon band, while a large variation of the real part occurs close to the resonance. The redshift and the broadening of the plasmon band as the gold volume fraction increases are correlated to the evolution of NP shape distribution. This evolution is attributed to a competition between the nucleation and the coalescence of NPs. This unambiguously demonstrates that ellipsometry combined with a shape-distributed effective medium theory is a powerful alternative tool to transmission electron microscopy for the NP shape analysis.

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

    International Nuclear Information System (INIS)

    Chu, S.N.G.

    1990-01-01

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

  9. 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.

  10. Interface-mediated amorphization of coesite by 200 keV electron irradiation

    International Nuclear Information System (INIS)

    Gong, W.L.; Wang, L.M.; Ewing, R.C.; Xie, H.S.

    1997-01-01

    Electron-induced amorphization of coesite was studied as a function of irradiation temperature by in situ transmission electron microscopy at an incident energy of 200 keV. Electron-induced amorphization of coesite is induced by an ionization mechanism and is mainly dominated by an interface-mediated, heterogeneous nucleation-and-growth controlled process. Amorphous domains nucleate at surfaces, crystalline-amorphous (c-a) interfaces, and grain boundaries. This is the same process as the interface-mediated vitrification of coesite by isothermal annealing above the thermodynamic melting temperature (875 K), but below the glass transition temperature (1480 K). The interface-mediated amorphization of coesite by electron irradiation is morphologically similar to interface-mediated thermodynamic melting. copyright 1997 American Institute of Physics

  11. 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

  12. Structural and optical characterization of In_2O_3/PANI nanocomposite prepared by in-situ polymerization

    International Nuclear Information System (INIS)

    Janeoo, Shashi; Sharma, Mamta; Goswamy, J.; Singh, Gurinder

    2016-01-01

    Polyaniline-indium oxide (In_2O_3/PANI) nanocomposite have been prepared by in-situ polymerization of aniline and as-synthesized In_2O_3 nanoparticles. X-ray diffraction (XRD), Transmission electron microscopy (TEM), Fourier transformation infrared (FTIR) and UV/Vis spectroscopy techniques are used to investigate the structural and optical properties of In_2O_3/PANI nanocomposite. TEM analysis shows In_2O_3 nanoparticles are embedded in PANI nanofibers. FTIR spectra show the good interactions between PANI nanofibers and In_2O_3 nanoparticles. The band gap and electronic transitions in In_2O_3/PANI nanocomposite is determined by using UV/Vis spectra.

  13. Fluorescence in situ hybridization and molecular studies in infertile men with dysplasia of the fibrous sheath.

    Science.gov (United States)

    Baccetti, Baccio; Collodel, Giulia; Gambera, Laura; Moretti, Elena; Serafini, Francesca; Piomboni, Paola

    2005-07-01

    To perform fluorescence in situ hybridization (FISH) and molecular analysis in patients with the genetic sperm defect "dysplasia of the fibrous sheath" (DFS). Retrospective study. Regional Referral Center for Male Infertility, Siena, Italy. Twelve infertile patients with DFS sperm defects. Family history, lymphocytic karyotype, physical and hormonal assays, semen analysis. The DFS sperm phenotype was defined by light, fluorescent, and electron microscopy. Sperm chromosomal constitution was examined by FISH. Gene deletions were tested by polymerase chain reaction. The genetic sperm defect DFS was determined by transmission and scanning electron microscopy. Immunofluorescence staining of A-kinase anchoring protein 4 (AKAP4) showed a moderate and diffuse signal, revealing a disorganized and incompletely assembled fibrous sheath. In 11 of 12 DFS patients, polymerase chain reaction for detecting the presence of partial sequence of AKAP4/AKAP3 binding regions gave positive results. Fluorescence in situ hybridization was performed in decondensed sperm nuclei with probes for chromosomes 18, X, and Y. The mean disomy frequency of chromosome 18 was in the normal range, whereas the mean disomy frequencies of sex chromosomes and diploidies were twice those of controls. These results should be considered when DFS sperm are used in assisted reproductive technology, owing to the high risk of transmission of chromosomal unbalance and of DFS sperm defects to male offspring.

  14. In-situ TEM on (de)hydrogenation of Pd at 0.5–4.5 bar hydrogen pressure and 20–400°C

    International Nuclear Information System (INIS)

    Yokosawa, Tadahiro; Alan, Tuncay; Pandraud, Gregory; Dam, Bernard; Zandbergen, Henny

    2012-01-01

    We have developed a nanoreactor, sample holder and gas system for in-situ transmission electron microscopy (TEM) of hydrogen storage materials up to at least 4.5 bar. The MEMS-based nanoreactor has a microheater, two electron-transparent windows and a gas inlet and outlet. The holder contains various O-rings to have leak-tight connections with the nanoreactor. The system was tested with the (de)hydrogenation of Pd at pressures up to 4.5 bar. The Pd film consisted of islands being 15 nm thick and 50–500 nm wide. In electron diffraction mode we observed reproducibly a crystal lattice expansion and shrinkage owing to hydrogenation and dehydrogenation, respectively. In selected-area electron diffraction and bright/dark-field modes the (de)hydrogenation of individual Pd particles was followed. Some Pd islands are consistently hydrogenated faster than others. When thermally cycled, thermal hysteresis of about 10–16 °C between hydrogen absorption and desorption was observed for hydrogen pressures of 0.5–4.5 bar. Experiments at 0.8 bar and 3.2 bar showed that the (de)hydrogenation temperature is not affected by the electron beam. This result shows that this is a fast method to investigate hydrogen storage materials with information at the nanometer scale. -- Highlights: ► In-situ TEM experiments up to 4.5 bar. ► In-situ TEM on a hydrogen storage material at pressures used in practice. ► No electron beam effect on (de)hydrogenation. ► In-situ TEM allows for fast screening of hydrogen storage materials.

  15. Synthesis of nanocrystalline Zn0.5Mn0.5Fe2O4 via in situ polymerization technique

    International Nuclear Information System (INIS)

    Liu Xianming; Fu Shaoyun

    2007-01-01

    Nanocrystalline Zn 0.5 Mn 0.5 Fe 2 O 4 was synthesized through the pyrolysis of polyacrylate salt precursors prepared via in situ polymerization of the metal salts and acrylic acid. The pyrolysis behavior of the polymeric precursors was studied by use of thermal analysis. The as-obtained product was characterized by powder X-ray diffraction (XRD), transmission electron microscope (TEM), electron diffraction (ED) pattern, scanning electron microscopy (SEM) and electron dispersive X-ray (EDX) analysis. The results revealed that the particle size is in the range of 15-25 nm for Zn-Mn ferrites with good crystallinity. Magnetic properties of the sample at 300 K were measured using a vibrating sample magnetometer, which showed that the sample exhibited characteristics of superparamagnetism

  16. In-situ fabrication of hybrid polyoxometalate nanoparticles composite films

    International Nuclear Information System (INIS)

    Lan Yang; Mao Baodong; Wang Enbo; Song Yonghai; Kang Zhenhui; Wang Chunlei; Tian Chungui; Zhang Chao; Xu Lin; Li Zhuang

    2007-01-01

    Inorganic-organic hybrid nanoparticles multilayer films were fabricated by extending the method of nucleation and growth of particles in polymer assemblies. The polyelectrolyte matrix was constructed by layer-by-layer self-assembly method. Synthesis of polyoxometalate nanoparticles was achieved by alternately dipping the precursor polyelectrolyte matrix into AgNO 3 and H 4 SiW 12 O 40 aqueous solutions. Repeating the above synthesis process, Ag 4 SiW 12 O 40 nanoparticles with controllable diameters of 20 to 77 nm were synthesized in the multilayer films in-situ. UV-vis absorption spectra indicate that the nanoparticles grew gradually in the synthesis process. Transmission electron microscopy was used to observe the size and morphology of the nanoparticles

  17. Structure observation of single solidified droplet by in situ controllable quenching based on nanocalorimetry

    International Nuclear Information System (INIS)

    Zhao, Bingge; Li, Linfang; Yang, Bin; Yan, Ming; Zhai, Qijie; Gao, Yulai

    2013-01-01

    Highlights: •Controllable quenching rate up to 15,000 K/s was realized by FSC. •FSC sample was novelly characterized by FIB and HRTEM. •Solidification structure with undercooling of 110.9 K was investigated. •This study opens a new approach in rapid solidification and FSC measurement. -- Abstract: Fast scanning calorimetry (FSC) based on nanocalorimetry and thin film technique is a newly developed attractive tool to investigate the solidification behavior of single droplet by in situ controllable ultrafast cooling. In this paper, we introduced this novel technique to in situ control the quenching of single Sn3.5Ag metallic droplet at cooling rate up to 15,000 K/s with corresponding undercooling of 110.9 K. In particular, the solidification structure of this real time quenched single droplet was observed and analyzed with focused ion beam (FIB), scanning electron microscopy (SEM) and high resolution transmission electron microscopy (HRTEM). This research proposed a new approach to research the solidification structure of single droplet with precisely controlled size and extreme cooling rate

  18. Attainment of 40.5 pm spatial resolution using 300 kV scanning transmission electron microscope equipped with fifth-order aberration corrector.

    Science.gov (United States)

    Morishita, Shigeyuki; Ishikawa, Ryo; Kohno, Yuji; Sawada, Hidetaka; Shibata, Naoya; Ikuhara, Yuichi

    2018-02-01

    The achievement of a fine electron probe for high-resolution imaging in scanning transmission electron microscopy requires technological developments, especially in electron optics. For this purpose, we developed a microscope with a fifth-order aberration corrector that operates at 300 kV. The contrast flat region in an experimental Ronchigram, which indicates the aberration-free angle, was expanded to 70 mrad. By using a probe with convergence angle of 40 mrad in the scanning transmission electron microscope at 300 kV, we attained the spatial resolution of 40.5 pm, which is the projected interatomic distance between Ga-Ga atomic columns of GaN observed along [212] direction.

  19. In situ-synthesized cadmium sulfide nanowire photosensor with a parylene passivation layer for chemiluminescent immunoassays.

    Science.gov (United States)

    Im, Ju-Hee; Kim, Hong-Rae; An, Byoung-Gi; Chang, Young Wook; Kang, Min-Jung; Lee, Tae-Geol; Son, Jin Gyeng; Park, Jae-Gwan; Pyun, Jae-Chul

    2017-06-15

    The direct in situ synthesis of cadmium sulfide (CdS) nanowires (NWs) was presented by direct synthesis of CdS NWs on the gold surface of an interdigitated electrode (IDE). In this work, we investigated the effect of a strong oxidant on the surfaces of the CdS NWs using X-ray photoelectron spectroscopy, transmission electron microscopy, and time-of-flight secondary ion mass spectrometry. We also fabricated a parylene-C film as a surface passivation layer for in situ-synthesized CdS NW photosensors and investigated the influence of the parylene-C passivation layer on the photoresponse during the coating of parylene-C under vacuum using a quartz crystal microbalance and a photoanalyzer. Finally, we used the in situ-synthesized CdS NW photosensor with the parylene-C passivation layer to detect the chemiluminescence of horseradish peroxidase and luminol and applied it to medical detection of carcinoembryonic antigen. Copyright © 2017 Elsevier B.V. All rights reserved.

  20. Effects of thermal annealing on C/FePt granular multilayers: in situ and ex situ studies

    International Nuclear Information System (INIS)

    Babonneau, D; Abadias, G; Toudert, J; Girardeau, T; Fonda, E; Micha, J S; Petroff, F

    2008-01-01

    The comprehensive study of C/FePt granular multilayers prepared by ion-beam sputtering at room temperature and subsequent annealing is reported. The as-deposited multilayers consist of carbon-encapsulated FePt nanoparticles (average size ∼3 nm) with a disordered face-centered-cubic structure. The effects of thermal annealing on the structural and magnetic properties are investigated by using dedicated ex situ and in situ techniques, including high-resolution transmission electron microscopy, extended x-ray absorption fine structure, magnetometry, and coupled grazing incidence small-angle x-ray scattering and x-ray diffraction. Our structural data show that the particle size and interparticle distance increase slightly with annealing at temperatures below 790 K by thermally activated migration of Fe and Pt atoms. We find that thermal annealing at temperatures above 870 K results in the dramatic growth of the FePt nanoparticles by coalescence and their gradual L1 0 ordering. In addition, we observe a preferential graphitization of the carbon matrix, which provides protection against oxidation for the FePt nanoparticles. Magnetization measurements indicate that progressive magnetic hardening occurs after annealing. The dependences of the blocking temperature, saturation magnetization, coercivity, and magnetocrystalline anisotropy energy on the annealing temperature are discussed on the basis of the structural data