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Sample records for situ tem investigation

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

    International Nuclear Information System (INIS)

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

    2007-01-01

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

  2. In Situ TEM Electrical Measurements

    DEFF Research Database (Denmark)

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

    2016-01-01

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

  3. In situ TEM investigation of microstructural behavior of superplastic Al-Mg-Sc alloy

    Czech Academy of Sciences Publication Activity Database

    Dám, Karel; Lejček, Pavel; Michalcová, A.

    2013-01-01

    Roč. 76, č. 2 (2013), s. 69-75 ISSN 1044-5803 R&D Projects: GA ČR GBP108/12/G043; GA MŠk LM2011026; GA AV ČR KAN300100801 Institutional research plan: CEZ:AV0Z10100520 Keywords : aluminium alloy s * ultrafine-grained alloy s * in situ TEM * equal-channel angular pressing Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.925, year: 2013

  4. In-situ TEM investigations of graphic-epitaxy and small particles

    Science.gov (United States)

    Heinemann, K.

    1983-01-01

    Palladium was deposited inside a controlled-vacuum specimen chamber of a transmission electron microscope (TEM) onto MgO and alpha-alumina substrate surfaces. Annealing and various effects of gas exposure of the particulate Pd deposits were studied in-situ by high resolution TEM and electron diffraction. Whereas substrate temperatures of 500 C or annealing of room temperature (RT) deposits to 500 C were needed to obtain epitaxy on sapphire, RT deposits on MgO were perfectly epitaxial. For Pd/MgO a lattice expansion of 2 to 4% was noted; the highest values of expansion were found for the smallest particles. The lattice expansion of small Pd particles on alumina substrates was less than 1%. Long-time RT exposure of Pd/MgO in a vacuum yielded some moblity and coalescence events, but notably fewer than for Pd on sapphire. Exposure to air or oxygen greatly enhanced the particle mobility and coalescence and also resulted in the flattening of Pd particles on MgO substrates. Electron-beam irradiation further enhanced this effect. Exposure to air for several tens of hours of Pd/MgO led to strong coalescence.

  5. Fast FIB-milled Electron-transparent Microchips for in situ TEM Investigations

    DEFF Research Database (Denmark)

    Lei, Anders; Petersen, Dirch Hjorth; Kallesøe, Christian

    In this work we present a fast approach to 50 nm resolution structures defined in a generic TEM-chip template in few minutes. While creating complex electrical and NEMS circuits for a specific insitu TEM experiment can be a cumbersome process, microchips with 100 nm thin flakes of single crystall......In this work we present a fast approach to 50 nm resolution structures defined in a generic TEM-chip template in few minutes. While creating complex electrical and NEMS circuits for a specific insitu TEM experiment can be a cumbersome process, microchips with 100 nm thin flakes of single...

  6. 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

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

    International Nuclear Information System (INIS)

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

    2011-01-01

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

  8. 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

  9. Interactions between Lattice Dislocations and Grain Boundaries in Ni3Al Investigated by Means of In Situ TEM and Computer Modelling Experiments

    NARCIS (Netherlands)

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

    1992-01-01

    The interaction between lattice dislocations and grain boundaries in Ni3Al has been investigated by means of in situ TEM deformation experiments. The interaction between screw dislocations and a coherent twin boundary could be analyzed in detail. The interaction mechanism found experimentally was

  10. Kinetically controlled fabrication of gold nanorods and investigation of their thermal stability via in-situ TEM heating

    Science.gov (United States)

    Chankhunthod, N.; Aslam, Z.; Critchley, K.; Evans, S. D.; Brydson, R.

    2017-09-01

    Size controlled CTAB-capped AuNRs with various aspect ratios (ARs) ranging from 1.63±0.13 to 4.12±0.25 were synthesized following a modified seed-mediated method. Their thermal stability was examined by in-situ TEM heating. The results revealed a structural change from rods to spheres with increasing temperature. At lower temperatures 600ºC, particles became increasingly spherical. This behaviour occurred at temperatures lower than the melting point of bulk gold supporting a surface diffusion mechanism with material diffusing from the tips and redepositing at the middle of the rods. The rate of change in AR appeared to increase for thinner AuNRs.

  11. In-situ TEM investigations of graphic-epitaxy and small particles. Final Report, 1 January-31 December 1982

    International Nuclear Information System (INIS)

    Heinemann, K.

    1983-01-01

    Palladium was deposited inside a controlled-vacuum specimen chamber of a transmission electron microscope (TEM) onto MgO and alpha-alumina substrate surfaces. Annealing and various effects of gas exposure of the particulate Pd deposits were studied in-situ by high resolution TEM and electron diffraction. Whereas substrate temperatures of 500 C or annealing of room temperature (RT) deposits to 500 C were needed to obtain epitaxy on sapphire, RT deposits on MgO were perfectly epitaxial. For Pd/MgO a lattice expansion of 2 to 4% was noted the highest values of expansion were found for the smallest particles. The lattice expansion of small Pd particles on alumina substrates was less than 1%. Long-time RT exposure of Pd/MgO in a vacuum yielded some moblity and coalescence events, but notably fewer than for Pd on sapphire. Exposure to air or oxygen greatly enhanced the particle mobility and coalescence and also resulted in the flattening of Pd particles on MgO substrates. Electron-beam irradiation further enhanced this effect. Exposure to air for several tens of hours of Pd/MgO led to strong coalescence

  12. 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),...

  13. Investigating the Mechanical Behavior and Deformation Mechanisms of Ultrafinegrained Metal Films Using Ex-situ and In-situ TEM Techniques

    Science.gov (United States)

    Izadi, Ehsan

    Nanocrystalline (NC) and Ultrafine-grained (UFG) metal films exhibit a wide range of enhanced mechanical properties compared to their coarse-grained counterparts. These properties, such as very high strength, primarily arise from the change in the underlying deformation mechanisms. Experimental and simulation studies have shown that because of the small grain size, conventional dislocation plasticity is curtailed in these materials and grain boundary mediated mechanisms become more important. Although the deformation behavior and the underlying mechanisms in these materials have been investigated in depth, relatively little attention has been focused on the inhomogeneous nature of their microstructure (particularly originating from the texture of the film) and its influence on their macroscopic response. Furthermore, the rate dependency of mechanical response in NC/UFG metal films with different textures has not been systematically investigated. The objectives of this dissertation are two-fold. The first objective is to carry out a systematic investigation of the mechanical behavior of NC/UFG thin films with different textures under different loading rates. This includes a novel approach to study the effect of texture-induced plastic anisotropy on mechanical behavior of the films. Efforts are made to correlate the behavior of UFG metal films and the underlying deformation mechanisms. The second objective is to understand the deformation mechanisms of UFG aluminum films using in-situ transmission electron microscopy (TEM) experiments with Automated Crystal Orientation Mapping. This technique enables us to investigate grain rotations in UFG Al films and to monitor the microstructural changes in these films during deformation, thereby revealing detailed information about the deformation mechanisms prevalent in UFG metal films.

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

    Science.gov (United States)

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

    2015-11-27

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

  15. Short Communication on "In-situ TEM ion irradiation investigations on U3Si2 at LWR temperatures"

    Science.gov (United States)

    Miao, Yinbin; Harp, Jason; Mo, Kun; Bhattacharya, Sumit; Baldo, Peter; Yacout, Abdellatif M.

    2017-02-01

    The radiation-induced amorphization of U3Si2 was investigated by in-situ transmission electron microscopy using 1 MeV Kr ion irradiation. Both arc-melted and sintered U3Si2 specimens were irradiated at room temperature to confirm the similarity in their responses to radiation. The sintered specimens were then irradiated at 350 °C and 550 °C up to 7.2 × 1015 ions/cm2 to examine their amorphization behavior under light water reactor (LWR) conditions. U3Si2 remains crystalline under irradiation at LWR temperatures. Oxidation of the material was observed at high irradiation doses.

  16. In Situ TEM Investigation of the Electrochemical Behavior in CNTs/MnO2-Based Energy Storage Devices.

    Science.gov (United States)

    Tsai, Tsung-Chun; Huang, Guan-Min; Huang, Chun-Wei; Chen, Jui-Yuan; Yang, Chih-Chieh; Tseng, Tseung-Yuen; Wu, Wen-Wei

    2017-09-19

    Transition metal oxides have attracted much interest owing to their ability to provide high power density in lithium batteries; therefore, it is important to understand the electrochemical behavior and mechanism of lithiation-delithiation processes. In this study, we successfully and directly observed the structural evolution of CNTs/MnO 2 during the lithiation process using transmission electron microscopy (TEM). CNTs/MnO 2 were selected due to their high surface area and capacitance effect, and the lithiation mechanism of the CNT wall expansion was systematically analyzed. Interestingly, the wall spacings of CNTs/MnO 2 and CNTs were obviously expanded by 10.92% and 2.59%, respectively. The MnO 2 layer caused structural defects on the CNTs surface that could allow penetration of Li + and Mn 4+ through the tube wall and hence improve the ionic transportation speed. This study provided direct evidence for understanding the role of CNTs/MnO 2 in the lithiation process used in lithium ion batteries and also offers potential benefits for applications and development of supercapacitors.

  17. 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

  18. SAXS and TEM Investigation of Bentonite Structure

    International Nuclear Information System (INIS)

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

    2013-01-01

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

  19. 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.

  20. SOFC anode reduction studied by in situ TEM

    DEFF Research Database (Denmark)

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

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

  1. In situ TEM observation of solid-gas reactions

    International Nuclear Information System (INIS)

    Kishita, K; Kamino, T; Watabe, A; Kuroda, K; Saka, H

    2008-01-01

    Under a gaseous atmosphere at high temperatures, almost all the materials (metal, catalysts, etc.) change their structures and properties. For the research and development of materials, it is of vital importance to clarify mechanisms of solid-gas and liquid-gas reactions. Recently an in situ TEM system combined with an environmental holder, which has a gas injection nozzle close to a specimen-heating element, has been developed. The gas injection nozzle permits gas to flow around the specimens sitting on the heating element made of a fine W filament. The newly developed in situ TEM has a differential pumping system; therefore, the pressure in the specimen chamber is maintained in the range of higher than 1 Pa, while the pressure in the electron gun chamber can be kept in the range of 10 -5 Pa. This system was applied to in situ observation of chemical reactions of metals with gases: Observation of oxidation and reduction under a gas pressure ranging from 10 -5 Pa to 1 Pa at high temperatures (room temperature to ∼1473 K) were successfully carried out on pure metal and rare metal catalysts at near-atomic resolution. This in situ environmental TEM system is promising for clarifying mechanisms of many solid-gas and liquid-gas reactions that take place at high temperatures under a gas atmosphere.

  2. Short Communication on “In-situ TEM ion irradiation investigations on U{sub 3}Si{sub 2} at LWR temperatures”

    Energy Technology Data Exchange (ETDEWEB)

    Miao, Yinbin, E-mail: ymiao@anl.gov [Argonne National Laboratory, Lemont, IL 60439 (United States); Harp, Jason [Idaho National Laboratory, Idaho Fall, ID 83415 (United States); Mo, Kun [Argonne National Laboratory, Lemont, IL 60439 (United States); Bhattacharya, Sumit [Northwestern University, Evanston, IL 60208 (United States); Baldo, Peter; Yacout, Abdellatif M. [Argonne National Laboratory, Lemont, IL 60439 (United States)

    2017-02-15

    The radiation-induced amorphization of U{sub 3}Si{sub 2} was investigated by in-situ transmission electron microscopy using 1 MeV Kr ion irradiation. Both arc-melted and sintered U{sub 3}Si{sub 2} specimens were irradiated at room temperature to confirm the similarity in their responses to radiation. The sintered specimens were then irradiated at 350 °C and 550 °C up to 7.2 × 10{sup 15} ions/cm{sup 2} to examine their amorphization behavior under light water reactor (LWR) conditions. U{sub 3}Si{sub 2} remains crystalline under irradiation at LWR temperatures. Oxidation of the material was observed at high irradiation doses.

  3. 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.

  4. 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...

  5. TEM investigations of microstructures of combustion aerosols

    International Nuclear Information System (INIS)

    Marquardt, A.; Hackfort, H.; Borchardt, J.; Schober, T.; Friedrich, J.

    1992-12-01

    In the incineration of organic material, apart from a series of gaseous pollutants, particulate pollutants or combustion aerosols also arise. The latter frequently consist of particles with a solid core of carbon to which a large number of inorganic and organic compounds are attached. These primarily include the polycyclic aromatic hydrocarbons (PAH) and their nitro-derivatives (NPAH), whose mutagenic or carcinogenic effect is known. The invisible particle sizes in the nanometer range, whose retention in the incineration off-gas is not state of the art, are of increasing significance for man and environment. On the one hand, they are deposited almost completely in the human lung. On the other hand, due to their fine dispersity they have along residence time in the atmosphere where they participate in chemical reactions and climatically significant processes. Important insights about the formation process of combustion aerosols are to be expected from the imaging of their microstructures in the transmission electron microscope (TEM). The present contribution describes the development and application of a representative sampling procedure for aerosols from a partial flow of flue gas from a fluidized-bed furnace. The method developed consists of electrically charging aerosol particles in situ and subsequently selectively precipitating them onto a microscope slide in an electric field. TEM studies of aerosol microstructures on the microscope slides revealed that in the combustion of petrol and heating oil under different combustion conditions in principle the same particle structures result, whereas in the incineration of used lubricating oil quite different particle structures were found. Results from the literature on aerosol microstructures in exhaust gases from petrol and diesel engines demonstrate agreement with the results of this study in the basic structure of the particles. (orig.) [de

  6. TEM investigations of laser ablated particles

    International Nuclear Information System (INIS)

    Fliegel, D.; Dundas, S.; Kosler, J.; Klementova, M.

    2009-01-01

    Full text: Laser ablation inductively coupled plasma mass spectrometry suffers from fractionation effects hindering a non matrix matched calibration strategy. Different reasons for elemental fractionation that are related to the laser ablation, the transport and the vaporization in the plasma are discussed. One major question to be addressed linked to the vaporization yield in the ICP is in which of mineralogical phase the different ablated particle sizes enter the plasma. This contribution will investigate particles generated by a 213 nm laser from different samples such as minerals and alloys with respect to their chemical and phase compositions using high resolution TEM. (author)

  7. Silver Accumulation in the Green Microalga Coccomyxa actinabiotis: Toxicity, in Situ Speciation, and Localization Investigated Using Synchrotron XAS, XRD, and TEM.

    Science.gov (United States)

    Leonardo, Thomas; Farhi, Emmanuel; Pouget, Stéphanie; Motellier, Sylvie; Boisson, Anne-Marie; Banerjee, Dipanjan; Rébeillé, Fabrice; den Auwer, Christophe; Rivasseau, Corinne

    2016-01-05

    Microalgae are good candidates for toxic metal remediation biotechnologies. This study explores the cellular processes implemented by the green microalga Coccomyxa actinabiotis to take up and cope with silver over the concentration range of 10(-7) to 10(-2) M Ag(+). Understanding these processes enables us to assess the potential of this microalga for applications for bioremediation. Silver in situ speciation and localization were investigated using X-ray absorption spectroscopy, X-ray diffraction, and transmission electron microscopy. Silver toxicity was evaluated by monitoring microalgal growth and photochemical parameters. Different accumulation mechanisms were brought out depending on silver concentration. At low micromolar concentration, microalgae fixed all silver initially present in solution, trapping it inside the cells into the cytosol, mainly as unreduced Ag(I) bound with molecules containing sulfur. Silver was efficiently detoxified. When concentration increased, silver spread throughout the cell and particularly entered the chloroplast, where it damaged the photosystem. Most silver was reduced to Ag(0) and aggregated to form crystalline silver nanoparticles of face-centered cubic structure with a mean size of 10 nm. An additional minor interaction of silver with molecules containing sulfur indicated the concomitant existence of the mechanism observed at low concentration or nanoparticle capping. Nanoparticles were observed in chloroplasts, in mitochondria, on the plasma membrane, on cytosolic membrane structures, and in vacuoles. Above 10(-4) M Ag(+), damages were irreversible, and photosynthesis and growth were definitely inhibited. However, high silver amounts remained confined inside microalgae, showing their potential for the bioremediation of contaminated water.

  8. In-situ TEM characterization of nanomaterials and devices

    KAUST Repository

    Kim, Moon; Park, Seongyong; Cha, Dong Kyu; Kim, Jiyoung; Floresca, Herman Carlo; Lu, Ning; Wang, Jinguo

    2011-01-01

    Electrical properties of nano size devices were directly measured by TEM. Real time observation of phase transition behavior in PRAM revealed that the volume of the crystalline phase is the main factor in determining cell resistance. In the transistor device, we have identified the doping type and area by measuring the I-V curve at the individual nano contact on the specimen. The evolution of the graphene edge structure was controlled and monitored at and up to 1200°C in-situ. © 2011 IEEE.

  9. In-situ TEM characterization of nanomaterials and devices

    KAUST Repository

    Kim, Moon

    2011-10-01

    Electrical properties of nano size devices were directly measured by TEM. Real time observation of phase transition behavior in PRAM revealed that the volume of the crystalline phase is the main factor in determining cell resistance. In the transistor device, we have identified the doping type and area by measuring the I-V curve at the individual nano contact on the specimen. The evolution of the graphene edge structure was controlled and monitored at and up to 1200°C in-situ. © 2011 IEEE.

  10. Investigation of creep threshold stresses using in situ TEM straining experiment in an Al-5Y2O3-10SiC composite

    International Nuclear Information System (INIS)

    Deshmukh, S.P.; Mishra, R.S.; Robertson, I.M.

    2010-01-01

    Creep behavior of metal matrix composites is similar to dispersion strengthen alloys and characterized by the presence of a threshold stress below which the creep rate is negligible. This threshold stress is attributed, at least in dispersion-strengthened alloys, to dislocation particle interactions in which the detachment of the dislocations from the particle is the rate-limiting step. Creep experiments were performed on an Al-5Y 2 O 3 -10SiC composite in the temperature range of 473 and 573 K and the nature of the dislocation-particle interaction was determined by performing in situ straining experiments at elevated temperature in a transmission electron microscope. The threshold stress and the detachment stress are temperature dependent and the detachment stress is less than the threshold stress emphasizing the contribution of load transfer from the matrix to the reinforcement phase.

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

    International Nuclear Information System (INIS)

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

    2008-01-01

    In order to perform in situ investigations on the evolution of microstructures during ion irradiation for the evaluation of irradiation-resistance performance of advanced materials, we have established a transmission electron microscope (TEM)-implanter/accelerator interface facility at Wuhan University, the first of its kind in China. A Hitachi H800 TEM was linked to a 200 kV ion implanter and a 2x1.7 MV tandem accelerator through the interface system designed on the basis of ion beam transportation calculations. Effective steps were taken to isolate the TEM from mechanical vibration transmitted from the ion beam lines, and no significant degradation of microscope resolution was observed when the TEM operated under high zoom modes during the ion implantation. In the test experiments, ion beams of N + , He + , Ar + , and H + were successfully transported from the implanter into the TEM chamber through the interface system, and the ion currents measured at the entrance of the TEM column were between 20 and 80 nA. The amorphisation process of Si crystal irradiated by N + ion beams was successfully observed in the preliminary experiments, demonstrating that this interface facility is capable of in situ study of ion irradiated samples

  12. Analytical TEM investigations of nanoscale magnetic materials

    International Nuclear Information System (INIS)

    Meingast, A.

    2015-01-01

    Analytical transmission electron microscopy has been applied within this thesis to investigate several novel approaches to design and fabricate nanoscale magnetic materials. As the size of the features of interest rank in the sub-nanometer range, it is necessary to employ techniques with a resolution – both spatial and analytical – well below this magnitude. Only at this performance level it is possible to examine material properties, necessary for the further tailoring of materials. Within this work two key aspects have been covered: First, analytical TEM (transmission electron microscopy) investigations were carried out to get insight into novel magnetic materials with high detail. Second, new analytical and imaging possibilities enabled with the commissioning of the new ASTEM (Austrian scanning transmission electron microscope) were explored. The aberration corrected TITAN® microscope (© FEI Company) allows resolving features in scanning transmission mode (STEM) with 70 pm distance. Thereby, direct imaging of light elements in STEM mode by using the annular bright field method becomes possible. Facilitated through high beam currents within the electron probe, an increased acquisition speed of analytical signals is possible. For energy dispersive X-ray spectroscopy (EDXS) a new four detector disc geometry around the specimen was implemented, which increases the accessible collection angle. With the integration of the latest generation of image filter and electron spectrometer (GIF QuantumERS), electron energy loss spectroscopy (EELS) is boosted through the high acquisition speed and the dual spectroscopy mode. The high acquisition speed allows to record up to 1000 spectra per second and the possibility to record atomically resolved EELS maps is at hand. Hereby it is important to avoid beam damage and alteration of the material during imaging and analysis. With the simultaneous acquisition of the low and the high loss spectral region, an extended range for

  13. 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.

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

    NARCIS (Netherlands)

    Malladi, S.R.K.

    2014-01-01

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

  15. 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

  16. Microfabricated Nanofluidic cells for in situ liquid TEM

    DEFF Research Database (Denmark)

    Laganà, Simone

    Over the last decade, transmission electron microscopy (TEM) has been revolutionized not only by the introduction of new and very sophisticated hardware for improved resolution, such as aberration correctors and monochromators, but also by the improvement of new methods that have provided more than......, allowing quantitative and high-precision acquisition of liquid thickness maps, high resolution observations and meaningful information about synthesis of NPs from metal precursor solutions in confined space. Finally, a new concept device based on a Si3N4 membrane for plunge freezing fixation, which enables...

  17. 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.

  18. 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....

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

    Science.gov (United States)

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

    2014-05-01

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

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

    Directory of Open Access Journals (Sweden)

    Yibing Wang

    2015-01-01

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

  1. 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)

  2. 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.

  3. In situ TEM observations of unusual nanocrystallization in a Ti-based bulk metallic glass

    International Nuclear Information System (INIS)

    Yan, M.; Wang, D.J.; Shen, J.; Qian, M.

    2011-01-01

    In situ transmission electron microscopy (TEM) has been used to witness the nanocrystallization of amorphous Ti 42.5 Cu 40 Zr 10 Ni 5 Sn 2.5 . A crystallization front exists to separate the TEM sample into two parts with different thermal stabilities. The number density of the crystallization products varies significantly, with the precipitate sizes ranging from a few nanometres to ∼100 nm. Detailed TEM analysis suggests that oxygen is the most likely reason for realizing the unusual nanocrystallization. External thermal analysis also indicates that oxygen affects the crystallization.

  4. 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

  5. Soft nanomaterials analysed by in situ liquid TEM: Towards high resolution characterisation of nanoparticles in motion

    Directory of Open Access Journals (Sweden)

    Joseph P. Patterson

    2015-12-01

    Full Text Available In this article we present in situ transmission electron microscopy (TEM of soft, synthetic nanoparticles with a comparative analysis using conventional TEM methods. This comparison is made with the simple aim of describing what is an unprecedented example of in situ imaging by TEM. However, we contend the technique will quickly become essential in the characterisation of analogous systems, especially where dynamics are of interest in the solvated state. In this case, particles were studied which were obtained from the direct polymerisation of an oxaliplatin analogue, designed for an ongoing programme in novel chemotherapeutic delivery systems. The resulting nanoparticles provided sufficient contrast for facile imaging in situ, and point towards key design parameters that enable this new characterisation approach for organic nanomaterials. We describe the preparation of the synthetic nanoparticles together with their characterisation in liquid water. Finally, we provide a future perspective of this technique for the analysis of soft and dynamic nanomaterials and discussion the progress which needs to be made in order to bring in situ liquid TEM to its full potential.

  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. TEM in situ cube-corner indentation analysis using ViBe motion detection algorithm

    Science.gov (United States)

    Yano, K. H.; Thomas, S.; Swenson, M. J.; Lu, Y.; Wharry, J. P.

    2018-04-01

    Transmission electron microscopic (TEM) in situ mechanical testing is a promising method for understanding plasticity in shallow ion irradiated layers and other volume-limited materials. One of the simplest TEM in situ experiments is cube-corner indentation of a lamella, but the subsequent analysis and interpretation of the experiment is challenging, especially in engineering materials with complex microstructures. In this work, we: (a) develop MicroViBE, a motion detection and background subtraction-based post-processing approach, and (b) demonstrate the ability of MicroViBe, in combination with post-mortem TEM imaging, to carry out an unbiased qualitative interpretation of TEM indentation videos. We focus this work around a Fe-9%Cr oxide dispersion strengthened (ODS) alloy, irradiated with Fe2+ ions to 3 dpa at 500 °C. MicroViBe identifies changes in Laue contrast that are induced by the indentation; these changes accumulate throughout the mechanical loading to generate a "heatmap" of features in the original TEM video that change the most during the loading. Dislocation loops with b = ½ identified by post-mortem scanning TEM (STEM) imaging correspond to hotspots on the heatmap, whereas positions of dislocation loops with b = do not correspond to hotspots. Further, MicroViBe enables consistent, objective quantitative approximation of the b = ½ dislocation loop number density.

  8. Determination of the initial oxidation behavior of Zircaloy-4 by in-situ TEM

    International Nuclear Information System (INIS)

    Harlow, Wayne; Ghassemi, Hessam; Taheri, Mitra L.

    2016-01-01

    The corrosion behavior of Zircaloy-4 (Zry-4), specifically by oxidation, is a problem of great importance as this material is critical for current nuclear reactor cladding. The early formation behavior and structure of the oxide layer during oxidation was studied using in-situ TEM techniques that allowed for Zry-4 to be monitored during corrosion. These environmental exposure experiments were coupled with precession electron diffraction to identify and quantify the phases present in the samples before and after the oxidation. Following short-term, high temperature oxidation, the dominant phase was revealed to be monoclinic ZrO 2 in a columnar structure. These samples oxidized in-situ contained structures that correlated well with bulk Zry-4 subjected to autoclave treatment, which were used for comparison and validation of this technique. By using in-situ TEM the effect of microstructure features, such as grain boundaries, on oxidation behavior of an alloy can be studied. The technique presented herein holds the potential to be applied any alloy system to study these effects. - Highlights: • In-situ TEM was used to oxidize samples of Zircaloy-4. • Similar behavior was found in the in-situ oxidized and autoclave-oxidized samples. • Precession diffraction was used to characterize oxide phase and texture.

  9. 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

  10. 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.

  11. 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.

  12. TEM INVESTIGATIONS OF WC-Co ALLOYS AFTER CREEP EXPERIMENTS

    OpenAIRE

    Lay , S.; Osterstock , F.; Vicens , J.

    1986-01-01

    Carbide tungsten cobalt alloys were deformed in compression or in three point bending in a temperature range 1000-1350°C and in a stress domain 30-1000MPa. In these conditions, the stress exponent n of WC-Co alloys is a function of only the cobalt volumic ratio and tends towards n = 1 for pure carbide. The apparent activation energy is 550 kj mole-1. T.E.M. investigations on pure carbide deformed at 1450°C show an extensive intragranular deformation. Analysis of these defects have been perfor...

  13. 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.

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

    Science.gov (United States)

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

    2017-12-01

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

  15. 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....

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2017-09-29

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

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

    Directory of Open Access Journals (Sweden)

    Caitlin Anne Taylor

    2017-09-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-01-30

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

  19. TEM in situ micropillar compression tests of ion irradiated oxide dispersion strengthened alloy

    Energy Technology Data Exchange (ETDEWEB)

    Yano, K.H., E-mail: kaylayano@u.boisestate.edu [Boise State University, 1910 University Drive, Boise, ID, 83725 (United States); Swenson, M.J. [Boise State University, 1910 University Drive, Boise, ID, 83725 (United States); Wu, Y. [Boise State University, 1910 University Drive, Boise, ID, 83725 (United States); Center for Advanced Energy Studies, 995 University Blvd, Idaho Falls, ID, 83401 (United States); Wharry, J.P. [Boise State University, 1910 University Drive, Boise, ID, 83725 (United States); Purdue University, 400 Central Drive, West Lafayette, IN 47907 (United States)

    2017-01-15

    The growing role of charged particle irradiation in the evaluation of nuclear reactor candidate materials requires the development of novel methods to assess mechanical properties in near-surface irradiation damage layers just a few micrometers thick. In situ transmission electron microscopic (TEM) mechanical testing is one such promising method. In this work, microcompression pillars are fabricated from a Fe{sup 2+} ion irradiated bulk specimen of a model Fe-9%Cr oxide dispersion strengthened (ODS) alloy. Yield strengths measured directly from TEM in situ compression tests are within expected values, and are consistent with predictions based on the irradiated microstructure. Measured elastic modulus values, once adjusted for the amount of deformation and deflection in the base material, are also within the expected range. A pillar size effect is only observed in samples with minimum dimension ≤100 nm due to the low inter-obstacle spacing in the as received and irradiated material. TEM in situ micropillar compression tests hold great promise for quantitatively determining mechanical properties of shallow ion-irradiated layers.

  20. Cassette-based in-situ TEM sample inspection in the dual-beam FIB

    International Nuclear Information System (INIS)

    Kendrick, A B; Moore, T M; Zaykova-Feldman, L; Amador, G; Hammer, M

    2008-01-01

    A novel method is presented, combining site-specific TEM sample preparation and in-situ STEM analysis in a dual-beam microscope (FIB/SEM) fitted with a chamber mounted nano-manipulator. TEM samples are prepared using a modified in-situ, lift-out method, whereby the samples are thinned and oriented for immediate in-situ STEM analysis using the tilt, translation, and rotation capabilities of a FIB/SEM sample stage, a nano-manipulator, and a novel cassette. This cassette can provide a second tilt axis, orthogonal to the stage tilt axis, so that the STEM image contrast can be optimized to reveal the structural features of the sample (true STEM imaging in the FIB/SEM). The angles necessary for stage rotation and probe shaft rotation are calculated based on the position of the nano-manipulator relative to the stage and door and the stage tilt angle. A FIB/SEM instrument, equipped with a high resolution scanning electron column, can provide sufficiently high image resolution to enable many failure analysis and process control applications to be successfully carried out without requiring the use of a separate dedicated TEM/STEM instrument. The benefits of this novel approach are increased throughput and reduced cost per sample. Comparative analysis of different sample preparation methods is provided, and the STEM images obtained are shown.

  1. 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)

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

    International Nuclear Information System (INIS)

    Kaoumi, D.

    2011-01-01

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

  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. A tem investigation on intermetallic particles in zircaloy-2

    International Nuclear Information System (INIS)

    Sudarminto, Harini Sosiati; Kuwano, Noriyuki; Oki, Kensuke

    1996-01-01

    Tem investigation were conducted on the heat treated zircaloy-2 having the composition of Zr containing 1.6% Sn, 0.2% Fe, 0.1% Cr and 0.05% Ni (%wt) in order tostudy the characteristics of intermetallic particles related to the microstructural basis on the corrosion effect. Forged zircaloy-2 was annealed in the β-phase at 1050 C degrees for various isothermally in the α-phase region at 650 and 750 C degrees, followed by water quenching. The size precipates, the lower became their number. By increasing the annealing temperature, the growth of precipitates formed in this zircaloy-2 were of the Zr(Cr,Fe) 2 and Zr 2 (Fe,Cr,Ni) types. These kinds of precipitates and the ratios of Fe/Cr were independent of size and shape of precipitates and annealing time and temperature. (author), 16 refs, 2 tabs, 5 figs

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

    Science.gov (United States)

    1984-01-01

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

  6. Direct observation of shear–induced nanocrystal attachment and coalescence in CuZr-based metallic glasses: TEM investigation

    International Nuclear Information System (INIS)

    Hajlaoui, K.; Alrasheedi, Nashmi H.; Yavari, A.R.

    2016-01-01

    In-situ tensile straining tests were performed in a transmission electron microscope (TEM) to analyse the deformation processes in CuZr-based metallic glasses and to directly observe the phase transformation occurrence. We report evidence of shear induced coalescence of nanocrystals in the vicinity of deformed regions. Nanocrystals grow in shear bands, come into contact, being attached and progressively coalesce under applied shear stress. - Highlights: • In-situ tensile straining test in TEM was investigated on CuZr-Based metallic glass. • Strain induces nanocrystallization and subsequent attachment and coalescence of nanocrystals. • The coalescence of nanocrystals compensates strain softening in metallic glasses.

  7. In situ TEM observations of reverse dislocation motion upon unloading in tensile-deformed UFG aluminium

    International Nuclear Information System (INIS)

    Mompiou, Frédéric; Caillard, Daniel; Legros, Marc; Mughrabi, Haël

    2012-01-01

    Loading–unloading cycles have been performed on ultrafine-grained (UFG) aluminium inside a transmission electron microscope (TEM). The interaction of dislocations with grain boundaries, which is supposed to be at the origin of the inelastic behaviour of this class of materials, differs according to the main character of the dislocation segments involved in pile-ups. Pile-ups are formed by spiral sources and lead to the incorporation of dislocations into grain boundaries (GBs) during loading. Upon unloading, partial re-emission of dislocations from GBs can be observed. Stress and strain measurements performed during these in situ TEM loading–unloading experiments are in agreement with the rather large inelastic reverse strains observed during unloading in loading–unloading tests on bulk macroscopic UFG aluminium specimens.

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

    DEFF Research Database (Denmark)

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

    2017-01-01

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

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

    Science.gov (United States)

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

    2017-09-01

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

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

    DEFF Research Database (Denmark)

    Simonsen, Søren Bredmose

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

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

    Czech Academy of Sciences Publication Activity Database

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

    2013-01-01

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

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

    International Nuclear Information System (INIS)

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

    2011-01-01

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

  13. TEM investigation of plant-irradiated NPP bolt material

    International Nuclear Information System (INIS)

    Pakarinen, J.; Ehrnsten, U.; Keinaenen, H.; Karlsen, W.; Karlsen, T.

    2015-01-01

    Analytical transmission electron microscopy (ATEM) was used to examine irradiation-induced damage in material removed from two different bolts from two different nuclear power plants. One section came from a French PWR, was made of CW AISI 316, and included a section of the bolt that had accumulated a dose of approximately 15 dpa during 19 operation cycles at 350 - 390 C. degrees. Another section came from a VVER bolt that was removed from the plant due to indications found in non-destructive examinations (NDE). The VVER bolt was made of solution annealed titanium stabilized 0X18H10T (corresponding to Type AISI 321) and had accumulated a fluence of 2.9 dpa. During the removal of that bolt, it was found that the bolt washer had been inappropriately spot welded to the shielding plate during assembly. Destructive investigations showed that the bolt had two large intergranular cracks, and the TEM samples were prepared from the material adjacent to those cracks. The PWR bolt had not failed, although cracks in the bolts with a similar history had been found previously. The fluence for the cold-worked AISI 316 PWR bolt was estimated to be about 15 dpa. Both the examined bolts showed a clear radiation induced segregation of alloying elements at the grain boundaries (GB-RIS), the presence of dislocation loops, the formation of precipitates, and linear deformation microstructures. Additionally, voids were found from the PWR bolt and the VVER bolt had a high density of dislocations. (authors)

  14. In situ TEM experiments of electrochemical lithiation and delithiation of individual nanostructures

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Xiao Hua; Liu, Yang; Huang, Jian Yu [Center for Integrated Nanotechnologies (CINT), Sandia National Laboratories, Albuquerque, New Mexico (United States); Kushima, Akihiro; Li, Ju [Department of Nuclear Science and Engineering and Department of Materials Science and Engineering, Massachusetts Institute of Technology, Cambridge, Massachusetts (United States); Zhang, Sulin [Department of Engineering Science and Mechanics, Pennsylvania State University, University Park, Pennsylvania (United States); Zhu, Ting [Woodruff School of Mechanical Engineering, Georgia Institute of Technology, Atlanta, Georgia (United States)

    2012-07-15

    Understanding the microscopic mechanisms of electrochemical reaction and material degradation is crucial for the rational design of high-performance lithium ion batteries (LIBs). A novel nanobattery assembly and testing platform inside a transmission electron microscope (TEM) has been designed, which allows a direct study of the structural evolution of individual nanowire or nanoparticle electrodes with near-atomic resolution in real time. In this review, recent progresses in the study of several important anode materials are summarized. The consistency between in situ and ex situ results is shown, thereby validating the new in situ testing paradigm. Comparisons between a variety of nanostructures lead to the conclusion that electrochemical reaction and mechanical degradation are material specific, size dependent, and geometrically and compositionally sensitive. For example, a highly anisotropic lithiation in Si is observed, in contrast to the nearly isotropic response in Ge. The Ge nanowires can develop a spongy network, a unique mechanism for mitigating the large volume changes during cycling. The Si nanoparticles show a critical size of {proportional_to}150 nm below which fracture is averted during lithiation, and above which surface cracking, rather than central cracking, is observed. In carbonaceous nanomaterials, the lithiated multi-walled carbon nanotubes (MWCNTs) are drastically embrittled, while few-layer graphene nanoribbons remain mechanically robust after lithiation. This distinct contrast manifests a strong 'geometrical embrittlement' effect as compared to a relatively weak 'chemical embrittlement' effect. In oxide nanowires, discrete cracks in ZnO nanowires are generated near the lithiation reaction front, leading to leapfrog cracking, while a mobile dislocation cloud at the reaction front is observed in SnO{sub 2} nanowires. This contrast is corroborated by ab initio calculations that indicate a strong chemical embrittlement of Zn

  15. In Situ Environmental TEM in Imaging Gas and Liquid Phase Chemical Reactions for Materials Research.

    Science.gov (United States)

    Wu, Jianbo; Shan, Hao; Chen, Wenlong; Gu, Xin; Tao, Peng; Song, Chengyi; Shang, Wen; Deng, Tao

    2016-11-01

    Gas and liquid phase chemical reactions cover a broad range of research areas in materials science and engineering, including the synthesis of nanomaterials and application of nanomaterials, for example, in the areas of sensing, energy storage and conversion, catalysis, and bio-related applications. Environmental transmission electron microscopy (ETEM) provides a unique opportunity for monitoring gas and liquid phase reactions because it enables the observation of those reactions at the ultra-high spatial resolution, which is not achievable through other techniques. Here, the fundamental science and technology developments of gas and liquid phase TEM that facilitate the mechanistic study of the gas and liquid phase chemical reactions are discussed. Combined with other characterization tools integrated in TEM, unprecedented material behaviors and reaction mechanisms are observed through the use of the in situ gas and liquid phase TEM. These observations and also the recent applications in this emerging area are described. The current challenges in the imaging process are also discussed, including the imaging speed, imaging resolution, and data management. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. 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.

  17. 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.

  18. 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.

  19. In situ targeting TEM8 via immune response and polypeptide recognition by wavelength-modulated surface plasmon resonance biosensor

    Science.gov (United States)

    Wang, Yimin; Luo, Zewei; Liu, Kunping; Wang, Jie; Duan, Yixiang

    2016-01-01

    There is an increasing interest in real-time and in situ monitoring of living cell activities in life science and medicine. This paper reports a whole cell sensing protocol over the interface of Au film coupled in a wavelength-modulated surface plasmon resonance (WMSPR) biosensor. With dual parabolic mirrors integrated in the sensor, the compact and miniaturized instrument shows satisfactory refractive index sensitivity (2220 nm/RIU) and a high resolution of resonance wavelength shift of 0.3 nm to liquid samples. The affinity interactions between the biomarker of human tumor endothelial marker 8 (TEM8) and antibody (Ab) or specific polypeptide (PEP) were firstly introduced to WMSPR biosensor analysis. Both the interaction events of Ab-cell and PEP-cell over the Au film interface can be recognized by the sensor and the balance time of interactions is about 20 min. The concentration range of Ab for quantitative monitoring of the TEM8 expression on human colon carcinoma SW620 cells was investigated. The present low-cost and time-saving method provides a time resolution of binding specificity between Ab/PEP and TEM8 for real-time analysis of antigen on living tumor cell surface. PMID:26822761

  20. In situ EELS and TEM observation of Al implanted with nitrogen ions

    International Nuclear Information System (INIS)

    Hojou, K.; Furuno, S.; Kushita, K.N.; Otsu, H.; Izui, K.

    1995-01-01

    Formation processes of Aluminum nitride (AIN) in Aluminum (AI) implanted with nitrogen were examined by in situ EELS and TEM observations during nitrogen ion implantation in an electron microscope at room temperature and 400 deg C. AIN phase was identified both by EDP and EELS after nitrogen ion implantation to 6 x 10 20 (N + )/m 2 . The observed peak (20.8 eV) in EELS spectra was identified as plasmon loss peak of AIN formed in AI. The binding energy of N ls in AI was found to shift by about 4 eV to the lower side with increasing nitrogen-ion fluence. Unreacted AI was also found to remain in the AIN films after high fluence implantation both at room temperature and 400 deg C. (authors). 11 refs., 5 figs., 2 tabs

  1. Customizable in situ TEM devices fabricated in freestanding membranes by focused ion beam milling

    International Nuclear Information System (INIS)

    Lei, Anders; Petersen, Dirch Hjorth; Booth, Timothy John; Homann, Lasse Vinther; Kallesoe, Christian; Sukas, Ozlem Sardan; Molhave, Kristian; Boggild, Peter; Gyrsting, Yvonne

    2010-01-01

    Nano- and microelectromechanical structures for in situ operation in a transmission electron microscope (TEM) were fabricated with a turnaround time of 20 min and a resolution better than 100 nm. The structures are defined by focused ion beam (FIB) milling in 135 nm thin membranes of single crystalline silicon extending over the edge of a pre-fabricated silicon microchip. Four-terminal resistance measurements of FIB-defined nanowires showed at least two orders of magnitude increase in resistivity compared to bulk. We show that the initial high resistance is due to amorphization of silicon, and that current annealing recrystallizes the structure, causing the electrical properties to partly recover to the pristine bulk resistivity. In situ imaging of the annealing process revealed both continuous and abrupt changes in the crystal structure, accompanied by instant changes of the electrical conductivity. The membrane structures provide a simple way to design electron-transparent nanodevices with high local temperature gradients within the field of view of the TEM, allowing detailed studies of surface diffusion processes. We show two examples of heat-induced coarsening of gold on a narrow freestanding bridge, where local temperature gradients are controlled via the electrical current paths. The separation of device processing into a one-time batch-level fabrication of identical, generic membrane templates, and subsequent device-specific customization by FIB milling, provides unparalleled freedom in device layout combined with very short effective fabrication time. This approach significantly speeds up prototyping of nanodevices such as resonators, actuators, sensors and scanning probes with state-of-art resolution.

  2. Customizable in situ TEM devices fabricated in freestanding membranes by focused ion beam milling

    Energy Technology Data Exchange (ETDEWEB)

    Lei, Anders; Petersen, Dirch Hjorth; Booth, Timothy John; Homann, Lasse Vinther; Kallesoe, Christian; Sukas, Ozlem Sardan; Molhave, Kristian; Boggild, Peter [DTU Nanotech, Department of Nano- and Microtechnology, Technical University of Denmark, DK-2800 Kongens Lyngby (Denmark); Gyrsting, Yvonne, E-mail: Anders.Lei@nanotech.dtu.dk [DTU Danchip, National Center for Micro- and Nanofabrication, Technical University of Denmark, DK-2800 Kongens Lyngby (Denmark)

    2010-10-08

    Nano- and microelectromechanical structures for in situ operation in a transmission electron microscope (TEM) were fabricated with a turnaround time of 20 min and a resolution better than 100 nm. The structures are defined by focused ion beam (FIB) milling in 135 nm thin membranes of single crystalline silicon extending over the edge of a pre-fabricated silicon microchip. Four-terminal resistance measurements of FIB-defined nanowires showed at least two orders of magnitude increase in resistivity compared to bulk. We show that the initial high resistance is due to amorphization of silicon, and that current annealing recrystallizes the structure, causing the electrical properties to partly recover to the pristine bulk resistivity. In situ imaging of the annealing process revealed both continuous and abrupt changes in the crystal structure, accompanied by instant changes of the electrical conductivity. The membrane structures provide a simple way to design electron-transparent nanodevices with high local temperature gradients within the field of view of the TEM, allowing detailed studies of surface diffusion processes. We show two examples of heat-induced coarsening of gold on a narrow freestanding bridge, where local temperature gradients are controlled via the electrical current paths. The separation of device processing into a one-time batch-level fabrication of identical, generic membrane templates, and subsequent device-specific customization by FIB milling, provides unparalleled freedom in device layout combined with very short effective fabrication time. This approach significantly speeds up prototyping of nanodevices such as resonators, actuators, sensors and scanning probes with state-of-art resolution.

  3. Characterising ambient and vacuum performance of a miniaturised TEM nanoindenter for in-situ material deformation

    Energy Technology Data Exchange (ETDEWEB)

    Wang, J J; Lockwood, A J; Gay, R; Inkson, B J [Department of Engineering Materials, University of Sheffield, Sheffield SI 3JD (United Kingdom)], E-mail: beverley.inkson@Sheffield.ac.uk

    2008-08-15

    A miniaturised nanomanipulation and nanoindentation system has been designed and manufactured to perform sub-micron localised in-situ deformation studies in a high resolution transmission electron microscope (HRTEM). The nanomanipulation drive comprises two independent mechanisms for both coarse and fine positioning of sharp indenter tips. Small slip-stick inertial sliders are used to coarsely position a tip which fits inside a bespoke hollowed specimen holder for a JEOL (Japan) 2010/3010 series microscope. The coarse drive comprises three fully independent sliders which are set mutually perpendicular to one another (x, y and z) with a range > 1 mm and resolution {approx} 100 nm. Fine positioning is achieved with a quartered piezoelectric tube with range {approx} 2 {mu}m and resolution < 1 A. Optical displacement sensors have been used to characterise the nanomanipulation drive performance including total displacement rate and step size in ambient conditions. These are compared to the operation of the drive within a TEM under vacuum conditions. TEM observations at high magnification enable optimisation of the fine and coarse motion and overall drive stiffness.

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

    Science.gov (United States)

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

    2016-07-14

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

  5. TEM investigation of irradiation damage in single crystal CeO2

    International Nuclear Information System (INIS)

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

    2011-01-01

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

  6. In Situ TEM Scratch Testing of Perpendicular Magnetic Recording Multilayers with a Novel MEMS Tribometer

    Science.gov (United States)

    Hintsala, Eric D.; Stauffer, Douglas D.; Oh, Yunje; Asif, S. A. Syed

    2017-01-01

    Utilizing a newly developed two-dimensional (2D) transducer designed for in situ transmission electron microscope (TEM) nanotribology, deformation mechanisms of a perpendicular magnetic recording film stack under scratch loading conditions were evaluated. These types of films are widely utilized in storage devices, and loss of data by grain reorientation in the recording layers is of interest. The observed deformation was characterized by a stick-slip mechanism, which was induced by a critical ratio of lateral to normal force regardless of normal force. At low applied normal forces, the diamond-like carbon (DLC) coating and asperities in the recording layer were removed during scratching, while, at higher applied forces, grain reorientation and debonding of the recording layer was observed. As the normal force and displacement were increased, work for stick-slip deformation and contact stress were found to increase based upon an Archard's Law analysis. These experiments also served as an initial case study demonstrating the capabilities of this new transducer.

  7. The investigation of nanostructures of magnetic recording media by TEM

    International Nuclear Information System (INIS)

    Peng Yingguo; Ohkubo, Tadakatsu; Laughlin, David E.

    2003-01-01

    Diverse applications of transmission electron microscopy techniques used in investigating the nanostructures of magnetic recording materials are presented. Specimen preparation methods are discussed for the specific case of magnetic thin film recording media. Investigations of the crystallographic orientation, grain size and distribution, and interfacial nanostructures are presented

  8. In situ TEM observation of stress-induced martensitictransformations and twinning processes in CuAlNi single crystals

    Czech Academy of Sciences Publication Activity Database

    Zárubová, Niva; Gemperlová, Juliana; Gemperle, Antonín; Dlabáček, Zdeněk; Šittner, Petr; Novák, Václav

    2010-01-01

    Roč. 58, č. 15 (2010), s. 5109-5119 ISSN 1359-6454 R&D Projects: GA AV ČR(CZ) IAA200100627 Institutional research plan: CEZ:AV0Z10100520 Keywords : CuAlNi shape memory alloy * martensitic transformation * in situ TEM straining Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 3.781, year: 2010

  9. ANALISIS JARINGAN UMTS PADA MENARA ROOFTOP DENGAN MENGGUNAKAN SOFTWARE TEMS INVESTIGATION DAN G-NETTRACK PRO

    OpenAIRE

    Pande Putu Wahyu Pramanda; Pande Ketut Sudiarta; Ngurah Indra ER.

    2016-01-01

    Berkembangnya dunia teknologi telekomunikasi dan informasi sejalan dengan kebutuhan akan kecepatan dan kestabilan akses internet teknologi UMTS. Metode drive test adalah metode yang biasanya digunakan untuk pengukuran kualitas sebuah site. Pihak provider umumnya menggunakan software TEMS Investigation dalam melakukan drive test. Melakukan drive test dengan TEMS Investigation sangatlah tidak praktis dan memerlukan biaya yang besar. Berkembangnya teknologi smartphone membuat drive test dapat di...

  10. 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.

  11. Investigation of diversity of plasmids carrying the blaTEM-52 gene

    DEFF Research Database (Denmark)

    Bielak, Eliza Maria; Bergenholtz, Rikke D.; Jørgensen, Mikael Skaanning

    2011-01-01

    OBJECTIVES: To investigate the diversity of plasmids that carry blaTEM-52 genes among Escherichia coli and Salmonella enterica originating from animals, meat products and humans. METHODS: A collection of 22 blaTEM-52-encoding plasmids was characterized by restriction fragment length polymorphism...... of self-transfer to a plasmid-free E. coli recipient. CONCLUSIONS: The blaTEM-52 gene found in humans could have been transmitted on transferable plasmids originating from animal sources. Some of the blaTEM-52 plasmids carry replicons that differ from the classical ones. Two novel replicons were detected...

  12. In situ TEM study on elastic interaction between a prismatic loop and a gliding dislocation

    International Nuclear Information System (INIS)

    Matsukawa, Yoshitaka; Liu, Grace S.

    2012-01-01

    In situ straining in a transmission electron microscope was performed in order to investigate dislocation interactions with a prismatic loop, which as a mobile obstacle is expected to be displaced by the strain-field of dislocation prior to physical contact. It was found that when a gliding dislocation approached a critical distance, the prismatic loop was certainly attracted to the dislocation. The captured loop disrupted the dislocation motion and was not dragged along with the mobile dislocation. Instead, the dislocation bypassed the loop via cross-slip to another slip plane with a resolved shear stress estimated to be 40% lower than that of the original plane.

  13. 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.

  14. TEM investigation of the microstructural evolution in nickel during MeV helium implantation

    International Nuclear Information System (INIS)

    Gadalla, A.A.; Jaeger, W.; Ehrhart, P.

    1986-01-01

    In a recent TEM investigation of high energy He-implanted copper the low average helium density could be understood by the observation of the coexistence of two types of vacancy agglomerates i.e. relaxed vacancy agglomerates in the form of stacking fault tetrahedra (SFT) and small bubbles. In order to arrive at a more systematic understanding of the evolution of the microstructure during high energy helium implantation we extended these TEM investigations to nickel. Of particular interest was also the minimum implantation dose necessary to precipitate bubbles that are large enough to be visible in the TEM. (orig./RK)

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

    Energy Technology Data Exchange (ETDEWEB)

    Hsiung, L M

    2005-12-06

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

  16. ANALISIS JARINGAN UMTS PADA MENARA ROOFTOP DENGAN MENGGUNAKAN SOFTWARE TEMS INVESTIGATION DAN G-NETTRACK PRO

    Directory of Open Access Journals (Sweden)

    Pande Putu Wahyu Pramanda

    2016-03-01

    Full Text Available Berkembangnya dunia teknologi telekomunikasi dan informasi sejalan dengan kebutuhan akan kecepatan dan kestabilan akses internet teknologi UMTS. Metode drive test adalah metode yang biasanya digunakan untuk pengukuran kualitas sebuah site. Pihak provider umumnya menggunakan software TEMS Investigation dalam melakukan drive test. Melakukan drive test dengan TEMS Investigation sangatlah tidak praktis dan memerlukan biaya yang besar. Berkembangnya teknologi smartphone membuat drive test dapat dilakukan dengan menggunakan handphone yaitu dengan G-NetTrack Pro. Namun G-NetTrack Pro tidak memiliki kemampuan yang sama dengan TEMS Investigation. Software G-NetTrack Pro dapat digunakan sebagai bahan pembelajaran yaitu untuk pengenalan drivetest namun belum cocok digunakan secara profesional. G-NetTrack Pro dapat menampilkan data yang dibutuhkan dalam drive test namun tidak sedetail TEMS Investigation, sehingga dalam proses pembelajaran dapat digunakan untuk pengenalan karena efisien dan dapat di install pada handphone mahasiswa namun tidak dapat digunakan melakukan drive test misalnya dalam dunia kerja atau secara professional.

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

    Science.gov (United States)

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

    2014-01-24

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

  18. XRD, TEM, IR, Raman and NMR Spectroscopy of In Situ Crystallization of Lithium Disilicate Glass

    Science.gov (United States)

    Fuss, T.; Mogus-Milankovic, A.; Ray, C. S.; Lesher, C. E.; Youngman, R.; Day, D. E.

    2006-01-01

    The structure of a Li2O-2SiO2 (LS2) glass was investigated as a function of pressure and temperature up to 6 GPa and 750 C respectively, using XRD, TEM, IR, Raman and NMR spectroscopy. Glass densified at 6 GPa has an average Si-O-Si bond angle approx.7deg lower than that found in glass processed at 4.5 GPa. At 4.5 GPa, lithium disilicate crystallizes from the glass, while at 6 GPa a new high pressure form of lithium metasilicate crystallizes. The new phase, while having lithium metasilicate crystal symmetry, contains at least 4 different Si sites. NMR results for 6 GPa sample indicate the presence of Q4 species with (Q(sup 4))Si-O-Si(Q(sup 4)) bond angles of approx.157deg. This is the first reported occurrence of Q(sup 4) species with such large bond angles in alumina free alkali silicate glass. No five- or six- coordinated Si are found.

  19. ANALISIS PARAMETER JARINGAN HSDPA KONDISI INDOOR DENGAN TEMS INVESTIGATION DAN G-NETTRACK PRO

    Directory of Open Access Journals (Sweden)

    Dewa Made Mahendra Yudha

    2016-03-01

    Full Text Available Penggunaan teknologi dalam sistem komunikasi bergerak sudah berkembang cukup pesat. Salah satu contohnya ada teknologi HSDPA. Pihak provider biasanya melakukan metode walk test untuk mengecek kekuatan sinyal dengan menggunakan software TEMS Investigtions. Dengan kemajuannya Teknologi walk test dapat diterapkan dengan lebih mudah yaitu menggunakan perangkat android yang sudah terinstal aplikasi G-Net track Pro. Pada penelitian ini, akan menggunakan tahapan sesuai alur yang ada pada metode penelitian yaitu dimulai dengan melakukan pengukuran berdasarkan jarak dengan membandingkan software TEMS Investigations dan G-NET TRACK PRO dengan parameter RSCP dan Ec/No. Setelah dilakukan pengukuran kemudian akan dilanjutkan dengan menganalisa antara hubungan parameter RSCP dan Ec/No menggunakan TEMS Investigations dan G-Net Pro. kemudian dilanjutkan menggunakan perhitungan teoritis parameter RSCP. Dari hasil pengukuran diproleh pada lantai I antena 1-1 pada titik jarak 5 meter parameter RSCP dengan TEMS Investigation memiliki nilai -75 dBm sedangkan dari G-Net Track Pro memiliki nilai -83 dBm. Pada parameter Ec/No dengan TEMS Investigation memiliki nilai -6 dB dan G_Net Track memiliki nilai -5 dB. Dapat disimpulkan bahwa aplikasi G-NetTrack Pro mampu menampilkan parameter yang dibutuhkan akan tetapi tidak sedetail TEMS investigation sehingga untuk proses pembelajaran dan pengenalan walk test aplikasi G-Net track Pro dapat digunakan.

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

    International Nuclear Information System (INIS)

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

    2009-01-01

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

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

    Science.gov (United States)

    Harlow, Wayne

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

  2. 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.

  3. 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

  4. Minimum depth of investigation for grounded-wire TEM due to self-transients

    Science.gov (United States)

    Zhou, Nannan; Xue, Guoqiang

    2018-05-01

    The grounded-wire transient electromagnetic method (TEM) has been widely used for near-surface metalliferous prospecting, oil and gas exploration, and hydrogeological surveying in the subsurface. However, it is commonly observed that such TEM signal is contaminated by the self-transient process occurred at the early stage of data acquisition. Correspondingly, there exists a minimum depth of investigation, above which the observed signal is not applicable for reliable data processing and interpretation. Therefore, for achieving a more comprehensive understanding of the TEM method, it is necessary to perform research on the self-transient process and moreover develop an approach for quantifying the minimum detection depth. In this paper, we first analyze the temporal procedure of the equivalent circuit of the TEM method and present a theoretical equation for estimating the self-induction voltage based on the inductor of the transmitting wire. Then, numerical modeling is applied for building the relationship between the minimum depth of investigation and various properties, including resistivity of the earth, offset, and source length. It is guide for the design of survey parameters when the grounded-wire TEM is applied to the shallow detection. Finally, it is verified through applications to a coal field in China.

  5. In-Situ TEM-STM Observations of SWCNT Ropes/Tubular Transformations

    Science.gov (United States)

    Sola, F.; Lebron-Colon, M.; Ferreira, P. J.; Fonseca, L. F.; Meador, M. A.; Marin, C.

    2010-01-01

    Single-walled carbon nanotubes (SWCNTs) prepared by the HiPco process were purified using a modified gas phase purification technique. A TEM-STM holder was used to study the morphological changes of SWCNT ropes as a function of applied voltage. Kink formation, buckling behavior, tubular transformation and eventual breakdown of the system were observed. The tubular formation was attributed to a transformation from SWCNT ropes to multi-walled carbon nanotube (MWCNT) structures. It is likely mediated by the patching and tearing mechanism which is promoted primarily by the mobile vacancies generated due to current-induced heating and, to some extent, by electron irradiation.

  6. Environmental TEM in the in situ Toolbox

    DEFF Research Database (Denmark)

    Wagner, Jakob Birkedal

    on complementary experiments and characterization techniques. Normally, this is done in parallel with experiments separated in time and space [1] or mimicking a reaction by changing the conditions according to e.g. reactivity and conversion measured in dedicated catalyst set-ups [2]. Furthermore, dedicated...... the techniques to the microscope. A dedicated custom TEM specimen holder containing two optical fibres, five electrical contacts, a fixed miniaturized optical bench for light handling and a heating element has been designed. A system of pre-aligned mirrors and a MEMS heater are implemented in the holder...

  7. 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.

  8. 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.

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

    NARCIS (Netherlands)

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

    2011-01-01

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

  10. Insights from in situ and environmental TEM on the oriented attachment of α-Fe2O3 nanoparticles during α-Fe2O3 nanorod formation

    DEFF Research Database (Denmark)

    Almeida, Trevor P.; Fay, Michael W.; Hansen, Thomas Willum

    2014-01-01

    Acicular α-Fe2O3 nanorods (NRs), at an intermediate stage of development, were isolated using a snapshot valve-assisted hydrothermal synthesis (HS) technique, for the purpose of complementary in situ transmission electron microscopy (iTEM) and environmental TEM (ETEM) investigations of the effect......’ with the developing NR to adopt a perfect single crystal. Conversely, the heating of partially developed α-Fe2O3 NRs up to 250 °C, under vacuum, during iTEM, demonstrated the progressive coalescence of loosely packed α-Fe2O3 NPs and the coarsening of α-Fe2O3 NRs, without any direct evidence for an intermediate OA...... stage. Direct evidence was obtained for the action of an OA mechanism prior to the consumption of α-Fe2O3 NPs at the tips of developing α-Fe2O3 NRs during ETEM investigation, under an He pressure of 5 mbar at 500 °C. However, α-Fe2O3 NPs more strongly attached to the side-walls of developing α-Fe2O3 NRs...

  11. In-situ TEM imaging of the anisotropic etching of graphene by metal nanoparticles.

    Science.gov (United States)

    Wei, Jiake; Xu, Zhi; Wang, Hao; Tian, Xuezeng; Yang, Shize; Wang, Lifen; Wang, Wenlong; Bai, Xuedong

    2014-11-21

    Few-layer graphene was successfully tailored with smooth edges along crystallographic directions by Joule heating-driven tungsten nanoparticles inside a transmission electron microscope. The dynamic process was monitored in real time at the atomic resolution level. These high-resolution in-situ observations show that the neighboring graphene layers joined together to form closed edges, which is in contrast to the supposed open edges formed with hydrogen passivation. The tungsten nanoparticles transformed to W₂C in the intermediate stage of etching and to WC after etching, suggesting that carbon dissolution helped the continuous action of the metal nanoparticles in the catalytic anisotropic etching reaction.

  12. 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...

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

    Science.gov (United States)

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

    2017-09-01

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

  14. Low-temperature plasticity of olivine revisited with in situ TEM nanomechanical testing.

    Science.gov (United States)

    Idrissi, Hosni; Bollinger, Caroline; Boioli, Francesca; Schryvers, Dominique; Cordier, Patrick

    2016-03-01

    The rheology of the lithospheric mantle is fundamental to understanding how mantle convection couples with plate tectonics. However, olivine rheology at lithospheric conditions is still poorly understood because experiments are difficult in this temperature range where rocks and mineral become very brittle. We combine techniques of quantitative in situ tensile testing in a transmission electron microscope and numerical modeling of dislocation dynamics to constrain the low-temperature rheology of olivine. We find that the intrinsic ductility of olivine at low temperature is significantly lower than previously reported values, which were obtained under strain-hardened conditions. Using this method, we can anchor rheological laws determined at higher temperature and can provide a better constraint on intermediate temperatures relevant for the lithosphere. More generally, we demonstrate the possibility of characterizing the mechanical properties of specimens, which can be available in the form of submillimeter-sized particles only.

  15. 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.

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

    Science.gov (United States)

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

    2018-05-01

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

  17. A novel tripod-driven platform for in-situ positioning of samples and electrical probes in a TEM

    International Nuclear Information System (INIS)

    Medford, B D; Rogers, B L; Laird, D; Berdunov, N; Beton, P H; Lockwood, A J; Gnanavel, T; Guan, W; Wang, J; Moebus, G; Inkson, B J

    2010-01-01

    We present a design for a novel coarse positioning system based on a tilting platform which is positioned using linear slip/stick motors. The design differs from common arrangements of stacked x, y, and z motors, and also ball mounted slip/stick motors, by allowing easy access along the central axis of the microscope holder. The drive motors are highly compact and co-linear and may be easily incorporated in an off-axis configuration, leaving a central cylindrical region with an approximate diameter of 3mm which is available to accommodate screened electrical wiring and optical fibres. We show that the tripod can be used to manoeuvre two metallic tips towards each other in-situ in a TEM in nanometre-scale lateral steps.

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

    International Nuclear Information System (INIS)

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

    2010-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2010-08-15

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

  20. In-situ heating TEM observation of microscopic structural changes of size-controlled metallic copper/gelatin composite.

    Science.gov (United States)

    Narushima, Takashi; Hyono, Atsushi; Nishida, Naoki; Yonezawa, Tetsu

    2012-10-01

    Copper/gelatin composite particles with controlled sizes were prepared at room temperature from cupric sulfate pentahydrate in the presence of gelatin as a protective reagent by using hydrazine monohydrate as a reducing agent. The formed particles with the size between 190-940 nm were secondary aggregated particles which were composed of smaller nanosized particles ("particle-in-particle"), the presence of which was established by XRD patterns and a cross-sectional TEM image. The sintering behavior of these copper/gelatin composite particles was demonstrated by in-situ heating TEM under a high vacuum (approximately 10(-5) Pa) and separately with the oxygen partial pressure controlled at the 10(-4) Pa level. It was established that the particles began to sinter at about 330 degrees C with the oxygen and that they sublimate above 450 degrees C both in the vacuum and oxygen conditions. This result shows that the introduction of an adequate amount of oxygen was effective to remove the gelatin surrounding the particles. It can also be concluded that the sintering of the copper/gelatin composite particles occurred even in the absence of a reducing agent such as hydrogen gas.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-01-05

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

  2. Assessing phase stability and element distribution in Co-base superalloys at elevated temperatures by in situ TEM heating experiments

    Energy Technology Data Exchange (ETDEWEB)

    Eggeler, Yolita; Mueller, Julian; Spiecker, Erdmann [Lehrstuhl fuer Mikro- und Nanostrukturforschung and Center for Nanoanalysis and Electron Microscopy (CENEM), Department Werkstoffwissenschaften, Universitaet Erlangen-Nuernberg, Erlangen (Germany)

    2016-07-01

    Co-based alloys, of a composition of Co-12Al-9W, form a stable two phase γ/γ{sup '} microstructure at 900 C. γ{sup '} cubes, consisting of the L12 crystal structure are coherently embedded in a solid solution fcc (A1) γ matrix. To ensure precipitate hardening at temperatures, which are relevant to practical applications, 700-1100 C, as experienced in gas turbine applications, the stability of the γ/γ{sup '} phases is of fundamental importance. In this analysis in situ TEM studies with chip-based heating systems (by DENS solution) are applied on new Co-based superalloys. After in situ heating at apr. 900 C and controlled quenching with different quenching rates the elemental distribution at the γ/γ{sup '} interface is measured using ChemiSTEM EDX. Exploiting the driving force for interface movement resulting from temperature-dependent volume fraction of γ and γ{sup '} insight into the diffusion of individual alloying elements and the relationship between local chemistry and ordering can be gained from transient phenomena. The experimental results will be compared with theoretical calculations. This work has been carried out within the framework of the SFB-TR 103 ''Single Crystal Superalloys''.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1966-03-01

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

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

    International Nuclear Information System (INIS)

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

    1966-03-01

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

  5. In situ oxidation of zirconium binary alloys by environmental SEM and analysis by AFM, FIB, and TEM

    International Nuclear Information System (INIS)

    Proff, C.; Abolhassani, S.; Dadras, M.M.; Lemaignan, C.

    2010-01-01

    Binary Zr-alloys containing 1%Fe and 1% Ni (large precipitates) and 1% Cr and 0.6% Nb (small precipitates), as well as a pure Zr sample were exposed in situ at 130 Pa water vapour pressure at 415 o C in an environmental SEM. The surface topography and composition of each sample was characterised before in situ experiments, during and after oxidation. After oxidation the surface was characterised by SEM and EDS, AFM and TEM combined with EDS. Focused ion beam was used to prepare cross sections of the metal-oxide interface and for the preparation of TEM thin foils. The oxidation behaviour of precipitates for these alloying elements can be characterised into two large families, those which show a rapid oxidation and those which induce a delayed oxidation in comparison with the Zr-matrix. At 415 o C after 1 h of oxidation for Zr1%Fe and Zr1%Ni, the formation of protrusions could be detected at the surface, being related to underlying SPP in the oxide. On Zr1%Cr and Zr0.6%Nb unoxidised SPPs were observed in the oxide, close to the metal-oxide interface. These SPPs were, however, oxidised close to the outer surface of the oxide. The surface roughness was increased for all materials after in situ oxidation, however, only for Zr1%Fe and Zr1%Ni protrusions appeared on the surface during oxidation. It was subsequently demonstrated that these latter correspond to the position of SPPs. For Zr1%Fe the surface roughness increased more than in the other materials and on these protrusions small iron oxide crystals have been observed at the surface. These observations confirm that Fe has a different behaviour compared to the other SPP forming elements, and it diffuses out to the free surface of the material. These alloying elements being the constituents of the commercial alloys (Fe and Cr for Zircaloy-4; Fe, Cr and Ni for Zircaloy-2 and Nb for all Nb-containing alloys), this study allows to separate their individual influence and can allow a subsequent comparison to the behaviour

  6. In situ TEM and synchrotron characterization of U–10Mo thin specimen annealed at the fast reactor temperature regime

    International Nuclear Information System (INIS)

    Yun, Di; Mo, Kun; Mohamed, Walid; Ye, Bei; Kirk, Marquis A.; Baldo, Peter; Xu, Ruqing; Yacout, Abdellatif M.

    2015-01-01

    U–Mo metallic alloys have been extensively used for the Reduced Enrichment for Research and Test Reactors (RERTR) program, which is now known as the Office of Material Management and Minimization under the Conversion Program. This fuel form has also recently been proposed as fast reactor metallic fuels in the recent DOE Ultra-high Burnup Fast Reactor project. In order to better understand the behavior of U–10Mo fuels within the fast reactor temperature regime, a series of annealing and characterization experiments have been performed. Annealing experiments were performed in situ at the Intermediate Voltage Electron Microscope (IVEM-Tandem) facility at Argonne National Laboratory (ANL). An electro-polished U–10Mo alloy fuel specimen was annealed in situ up to 700 °C. At an elevated temperature of about 540 °C, the U–10Mo specimen underwent a relatively slow microstructure transition. Nano-sized grains were observed to emerge near the surface. At the end temperature of 700 °C, the near-surface microstructure had evolved to a nano-crystalline state. In order to clarify the nature of the observed microstructure, Laue diffraction and powder diffraction experiments were carried out at beam line 34-ID of the Advanced Photon Source (APS) at ANL. Phases present in the as-annealed specimen were identified with both Laue diffraction and powder diffraction techniques. The U–10Mo was found to recrystallize due to thermally-induced recrystallization driven by a high density of pre-existing dislocations. A separate in situ annealing experiment was carried out with a Focused Ion Beam processed (FIB) specimen. A similar microstructure transition occurred at a lower temperature of about 460 °C with a much faster transition rate compared to the electro-polished specimen. - Highlights: • TEM annealing experiments were performed in situ at the IVEM facility up to fast reactor temperature. • At 540 °C, the U-10Mo specimen underwent a slow microstructure transition

  7. In situ TEM and synchrotron characterization of U–10Mo thin specimen annealed at the fast reactor temperature regime

    Energy Technology Data Exchange (ETDEWEB)

    Yun, Di, E-mail: diyun1979@xjtu.edu.cn [Argonne National Laboratory, 9700 South Cass Avenue, Argonne, IL 60439 (United States); Xi' an Jiao Tong University, 28 Xian Ning West Road, Xi' an 710049 (China); Mo, Kun; Mohamed, Walid; Ye, Bei; Kirk, Marquis A.; Baldo, Peter; Xu, Ruqing; Yacout, Abdellatif M. [Argonne National Laboratory, 9700 South Cass Avenue, Argonne, IL 60439 (United States)

    2015-12-15

    U–Mo metallic alloys have been extensively used for the Reduced Enrichment for Research and Test Reactors (RERTR) program, which is now known as the Office of Material Management and Minimization under the Conversion Program. This fuel form has also recently been proposed as fast reactor metallic fuels in the recent DOE Ultra-high Burnup Fast Reactor project. In order to better understand the behavior of U–10Mo fuels within the fast reactor temperature regime, a series of annealing and characterization experiments have been performed. Annealing experiments were performed in situ at the Intermediate Voltage Electron Microscope (IVEM-Tandem) facility at Argonne National Laboratory (ANL). An electro-polished U–10Mo alloy fuel specimen was annealed in situ up to 700 °C. At an elevated temperature of about 540 °C, the U–10Mo specimen underwent a relatively slow microstructure transition. Nano-sized grains were observed to emerge near the surface. At the end temperature of 700 °C, the near-surface microstructure had evolved to a nano-crystalline state. In order to clarify the nature of the observed microstructure, Laue diffraction and powder diffraction experiments were carried out at beam line 34-ID of the Advanced Photon Source (APS) at ANL. Phases present in the as-annealed specimen were identified with both Laue diffraction and powder diffraction techniques. The U–10Mo was found to recrystallize due to thermally-induced recrystallization driven by a high density of pre-existing dislocations. A separate in situ annealing experiment was carried out with a Focused Ion Beam processed (FIB) specimen. A similar microstructure transition occurred at a lower temperature of about 460 °C with a much faster transition rate compared to the electro-polished specimen. - Highlights: • TEM annealing experiments were performed in situ at the IVEM facility up to fast reactor temperature. • At 540 °C, the U-10Mo specimen underwent a slow microstructure transition

  8. Space Plasma Ion Processing of Ilmenite in the Lunar Soil: Insights from In-Situ TEM Ion Irradiation Experiments

    Science.gov (United States)

    Christoffersen, R.; Keller, L. P.

    2007-01-01

    Space weathering on the moon and asteroids results largely from the alteration of the outer surfaces of regolith grains by the combined effects of solar ion irradiation and other processes that include deposition of impact or sputter-derived vapors. Although no longer considered the sole driver of space weathering, solar ion irradiation remains a key part of the space weathering puzzle, and quantitative data on its effects on regolith minerals are still in short supply. For the lunar regolith, previous transmission electron microscope (TEM) studies performed by ourselves and others have uncovered altered rims on ilmenite (FeTiO3) grains that point to this phase as a unique "witness plate" for unraveling nanoscale space weathering processes. Most notably, the radiation processed portions of these ilmenite rims consistently have a crystalline structure, in contrast to radiation damaged rims on regolith silicates that are characteristically amorphous. While this has tended to support informal designation of ilmenite as a "radiation resistant" regolith mineral, there are to date no experimental data that directly and quantitatively compare ilmenite s response to ion radiation relative to lunar silicates. Such data are needed because the radiation processed rims on ilmenite grains, although crystalline, are microstructurally and chemically complex, and exhibit changes linked to the formation of nanophase Fe metal, a key space weathering process. We report here the first ion radiation processing study of ilmenite performed by in-situ means using the Intermediate Voltage Electron Microscope- Tandem Irradiation facility (IVEM-Tandem) at Argonne National Laboratory. The capability of this facility for performing real time TEM observations of samples concurrent with ion irradiation makes it uniquely suited for studying the dose-dependence of amorphization and other changes in irradiated samples.

  9. In situ investigation of catalysts for alcohol synthesis

    DEFF Research Database (Denmark)

    Duchstein, Linus Daniel Leonhard; Sharafutdinov, Irek; Wu, Qiongxiao

    consists of three complimentary in situ techniques: (1) Activity measurements based on a reactor connected to a gas chromatograph (GC), (2) In situ x-ray diffractometer (XRD) measurements based on a reactor cell connected to a mass spectrometer (MS), and (3) environmental TEM (ETEM) that allows...... distribution, measured both macroscopically (XRD) and microscopically (ETEM), with the catalytic activity....

  10. Geological Hypothesis Testing and Investigations of Coupling with Transient Electromagnetics (TEM)

    Science.gov (United States)

    Adams, A. C.; Moeller, M. M.; Snyder, E.; Workman, E. J.; Urquhart, S.; Bedrosian, P.; Pellerin, L.

    2014-12-01

    Transient electromagnetic (TEM) data were acquired in Borrego Canyon within the Santo Domingo Basin of the Rio Grande Rift, central New Mexico, during the 2014 Summer of Applied Geophysical Experience (SAGE) field program. TEM surveys were carried out in several regions both to investigate geologic structure and to illustrate the effects of coupling to anthropogenic structures. To determine an optimal survey configuration, 50, 100 and 200 m square transmitter loops were deployed; estimates of depth-of-investigation and logistical considerations determined that 50 m loops were sufficient for production-style measurements. A resistive (100s of ohm-m) layer was identified at a depth of 25-75 m at several locations, and interpreted as dismembered parts of one or more concealed volcanic flows, an interpretation consistent with Tertiary volcanic flows that cap the Santa Anna Mesa immediately to the south. TEM soundings were also made across an inferred fault to investigate whether fault offset is accompanied by lateral changes in electrical resistivity. Soundings within several hundred meters of the inferred fault strand were identical, indicating no resistivity contrast across the fault, and possibly an absence of recent activity. An old windmill and water tank, long-abandoned, offered an excellent laboratory to study the effect of coupling to metallic anthropogenic structures. The character of the measured data strongly suggests the water tank is in electrical contact with the earth (galvanic coupling), and an induced response was persistent to more than 1 second after current turn-off. Coupling effects could be identified at least 150 meters from the tank. Understanding the mechanism behind such coupling and the ability to identify coupled data are critical skills, as one-dimensional modeling of data is affected by such coupling producing artificial conductive layers at depth.

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

    International Nuclear Information System (INIS)

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

    2013-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-09-15

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

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

    Science.gov (United States)

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

    2015-09-01

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

  14. In situ TEM annealing of ion-amorphized Hi Nicalon S and Tyranno SA3 SiC fibers

    Energy Technology Data Exchange (ETDEWEB)

    Huguet-Garcia, J., E-mail: juan.huguet-garcia@cea.fr [CEA, DEN, Service de Recherches Métallurgiques Appliquées, F-91191 Gif-sur-Yvette (France); Jankowiak, A. [CEA, DEN, Service de Recherches Métallurgiques Appliquées, F-91191 Gif-sur-Yvette (France); Miro, S. [CEA, DEN, Service de Recherches en Métallurgie Physique, F-91191 Gif-sur-Yvette (France); Meslin, E. [CEA, DEN, Service de Recherches en Métallurgie Physique, Laboratoire JANNUS, F-91191 Gif-sur-Yvette (France); Serruys, Y. [CEA, DEN, Service de Recherches en Métallurgie Physique, F-91191 Gif-sur-Yvette (France); Costantini, J.-M. [CEA, DEN, Service de Recherches Métallurgiques Appliquées, F-91191 Gif-sur-Yvette (France)

    2016-05-01

    In this work, recrystallization of ion-amorphized Hi Nicalon Type S and Tyranno SA3 SiC fibers (4 MeV Au{sup 3+}, 2 × 10{sup 15} cm{sup −2}) has been studied via in situ TEM annealing. Both fibers show a two-step recovery process of the radiation damage. First recovery stage starts at temperatures as low as 250 °C and implies recovery of the radiation swelling. Eventually the amorphous layer recrystallizes with no signs of polytype change (3C-SiC). Recrystallization temperatures yield 900–920 °C and 930 °C for the HNS and the TSA3 respectively. HNS fiber shows columnar recrystallization perpendicular to the amorphous–crystalline interphase with a grain growth rate of ∼20 nm min{sup −1}. On the other hand, recrystallization of TSA3 fiber is rather “spontaneous” with no preferential growth direction. The different recrystallization is attributed to the different microstructure of the fibers.

  15. In situ TEM annealing of ion-amorphized Hi Nicalon S and Tyranno SA3 SiC fibers

    International Nuclear Information System (INIS)

    Huguet-Garcia, J.; Jankowiak, A.; Miro, S.; Meslin, E.; Serruys, Y.; Costantini, J.-M.

    2016-01-01

    In this work, recrystallization of ion-amorphized Hi Nicalon Type S and Tyranno SA3 SiC fibers (4 MeV Au"3"+, 2 × 10"1"5 cm"−"2) has been studied via in situ TEM annealing. Both fibers show a two-step recovery process of the radiation damage. First recovery stage starts at temperatures as low as 250 °C and implies recovery of the radiation swelling. Eventually the amorphous layer recrystallizes with no signs of polytype change (3C-SiC). Recrystallization temperatures yield 900–920 °C and 930 °C for the HNS and the TSA3 respectively. HNS fiber shows columnar recrystallization perpendicular to the amorphous–crystalline interphase with a grain growth rate of ∼20 nm min"−"1. On the other hand, recrystallization of TSA3 fiber is rather “spontaneous” with no preferential growth direction. The different recrystallization is attributed to the different microstructure of the fibers.

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

    Science.gov (United States)

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

    2017-09-07

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

  17. 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

  18. APFIM and TEM investigations of precipitation in rapidly solidified 316 stainless steel

    International Nuclear Information System (INIS)

    Wisutmethangoon, S.; Kelly, T.F.; Flinn, J.E.; Camus, P.P.

    1998-01-01

    316 stainless steel has been rapid solidification-processed (RSP) by gas atomization and hot extrusion of the powder with the intent of improving the mechanical properties through fine-scale precipitation. Vanadium, nitrogen and oxygen have been introduced intentionally as alloying elements for this purpose. The yield strength after solution heat treatment of the RSP alloy is 450 MPa. By ageing at 600 C for 1000 h, the yield strength increases to 615 MPa with little loss of ductility (53% reduction of area). The ultimate tensile strength after cold work and ageing is 922 MPa. The morphology and composition of the precipitates in this steel have been investigated using APFIM and TEM techniques in order understand the origin of the high strength. A high numbered density (∼2 x 10 21 m -3 ) of 25 nm plate-like precipitates was observed with TEM in an aged specimen. The composition of these precipitates was analyzed using APFIM techniques, and was found to be a complex nitride of Cr, V, Fe, Ni and Mo. This nitride precipitate was not found in an unaged specimen of this alloy. These precipitates are responsible for improving mechanical properties by dispersion strengthening. (orig.)

  19. ANALISIS KUAT SINYAL DAN KUALITAS PANGGILAN JARINGAN GSM INDOOR DENGAN TEMS INVESTIGATION DAN G-NETTRACK PRO

    OpenAIRE

    Ida Bagus Ari Budiarta; Pande Ketut Sudiarta; IGAK. Diafari Djuni H.

    2016-01-01

    Kebutuhan akan teknologi GSM merupakan tantangan bagi provider untuk memberikan pelayanan terbaik bagi pengguna layanannya. Dalam proses layanan tersebut kemungkinan besar terdapat masalah yang terjadi. Pihak provider biasanya melakukan walk test untuk mengecek kekuatan sinyal yang dipancarkan oleh antena pemancar di dalam ruangan. Kebanyakan pihak provider menggunakan TEMS Investigation dalam melakukan walk test. Biaya walk test dengan TEMS Investigation bisa dikatakan cukup mahal. Namun den...

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

    International Nuclear Information System (INIS)

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

    2006-01-01

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

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

    International Nuclear Information System (INIS)

    Van den Berghe, S.

    2009-01-01

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

  2. TEM and XAS investigation of fission gas behaviors in U-Mo alloy fuels through ion beam irradiation

    Science.gov (United States)

    Zang, Hang; Yun, Di; Mo, Kun; Wang, Kunpeng; Mohamed, Walid; Kirk, Marquis A.; Velázquez, Daniel; Seibert, Rachel; Logan, Kevin; Terry, Jeffrey; Baldo, Peter; Yacout, Abdellatif M.; Liu, Wenbo; Zhang, Bo; Gao, Yedong; Du, Yang; Liu, Jing

    2017-10-01

    In this study, smaller-grained (hundred nano-meter size grain) and larger-grained (micro-meter size grain) U-10Mo specimens have been irradiated (implanted) with 250 keV Xe+ beam and were in situ characterized by TEM. Xe bubbles were not seen in the specimen after an implantation fluence of 2 × 1020 ions/m2 at room temperature. Nucleation of Xe bubbles happened during heating of the specimen to a final temperature of 300 °C. By comparing measured Xe bubble statistics, the nucleation and growth behaviors of Xe bubbles were investigated in smaller-grained and larger-grained U-10Mo specimens. A multi-atom kind of nucleation mechanism has been observed in both specimens. X-ray Absorption spectroscopy showed the edge position in the bubbles to be the same as that of Xe gas. The size of Xe bubbles has been shown to be bigger in larger-grained specimens than in smaller-grained specimens at the same implantation conditions.

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

    NARCIS (Netherlands)

    JONGEBLOED, WL; KALICHARAN, D; WORST, JGF

    1993-01-01

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

  4. Oxidation in ceria infiltrated metal supported SOFCs – A TEM investigation

    DEFF Research Database (Denmark)

    Knibbe, Ruth; Wang, Hsiang-Jen; Blennow Tullmar, Peter

    2013-01-01

    electron microscopy (TEM) techniques including energy-dispersive X-ray spectroscopy and electron energy-loss spectroscopy of focus ion beamed TEM samples. The infiltrated CGO is predominately converted into CeFeO3 after high temperature processing, protecting the alloy. A thin layer of Cr-oxide is observed...

  5. 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.

  6. 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"

  7. Phenomenological in-situ TEM gas exposure studies of palladium particles on MgO at room temperature

    Science.gov (United States)

    Heinemann, K.; Poppa, H.; Osaka, T.

    1983-01-01

    It has been found that very small vapor-deposited catalytically active metal particles in the 1-2 nm size range on metal oxide substrates can undergo significant changes when they are exposed to gases such as oxygen or air, or even when allowed to 'anneal' at room temperature (RT) under vacuum conditions. The present investigation is concerned with continued in-situ gas exposures of as-deposited, 1 to 2 nm size palladium particles on MgO to air, oxygen, nitrogen, hydrogen, CO, and water vapor at RT. It is found that the low-pressure exposure to various gases at RT can significantly affect small palladium particles supported on MgO surfaces. Exposure to oxygen for 3 min at 0.0002 m bar produces a considerable amount of coalescence, flattening of the particles, and some distinct crystallographic particle shapes.

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

    Science.gov (United States)

    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. Copyright © 2011 Elsevier B.V. All rights reserved.

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

    International Nuclear Information System (INIS)

    Rao, J. C.

    2017-01-01

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

  10. TEM investigation of the topotactic reaction of (001) and (111) Ag films and Te

    International Nuclear Information System (INIS)

    Safran, G.; Geszti, O.; Radnoczi, G.

    2002-01-01

    The formation, structure and morphology of Ag 2 Te phase developed by the reaction of single crystalline Ag films with subsequently vacuum deposited Te vapour was investigated. Silver films 30-40 nm in thickness were deposited at 85-120 grad C by thermal evaporation in vacuum at a base pressure of 4x10 -5 mbar. The NaCl substrates were cleaved and saw-cut in order to achieve (001) and (111) surfaces, respectively. The surfaces were treated with water and chlorine prior to Ag deposition. This preparation resulted in single crystalline Ag films of (001) and (111) orientation. Tellurium was deposited onto the silver at a rate about 0.1 nm/s at 200 grad C i.e. above the temperature of the polymorphic phase transformation from monoclinic to fcc (T c =150 grad C). The Ag-Te reaction occurred during the Te deposition. The samples were investigated by TEM and SAED in a 200 kV Philips CM 20 electron microscope equipped with a Ge detector Noran EDS system. In the fully tellurized layers, however, the monoclinic (low temperature) Ag 2 Te phase was found. It exhibited large single crystals consisting of strictly oriented mosaic grains of 1-2 mm size. Surprisingly, the orientation of the telluride was identical (010) on both the (001) and (111) Ag parent films. It is suggested that the final orientation appears during the polymorphic phase transition while cooling to room temperature, regardless to Ag orientation, due to the lower surface energy of the (010) orientation of monoclinic phase nuclei. (Authors)

  11. In-situ TEM observation of the response of ultrafine- and nanocrystalline-grained tungsten to extreme irradiation environments.

    Science.gov (United States)

    El-Atwani, O; Hinks, J A; Greaves, G; Gonderman, S; Qiu, T; Efe, M; Allain, J P

    2014-05-06

    The accumulation of defects, and in particular He bubbles, can have significant implications for the performance of materials exposed to the plasma in magnetic-confinement nuclear fusion reactors. Some of the most promising candidates for deployment into such environments are nanocrystalline materials as the engineering of grain boundary density offers the possibility of tailoring their radiation resistance properties. In order to investigate the microstructural evolution of ultrafine- and nanocrystalline-grained tungsten under conditions similar to those in a reactor, a transmission electron microscopy study with in situ 2 keV He(+) ion irradiation at 950 °C has been completed. A dynamic and complex evolution in the microstructure was observed including the formation of defect clusters, dislocations and bubbles. Nanocrystalline grains with dimensions less than around 60 nm demonstrated lower bubble density and greater bubble size than larger nanocrystalline (60-100 nm) and ultrafine (100-500 nm) grains. In grains over 100 nm, uniform distributions of bubbles and defects were formed. At higher fluences, large faceted bubbles were observed on the grain boundaries, especially on those of nanocrystalline grains, indicating the important role grain boundaries can play in trapping He and thus in giving rise to the enhanced radiation tolerance of nanocrystalline materials.

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

    Science.gov (United States)

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

    2014-11-01

    IntroductionCu is always present in the matrix when ferritic steels were prepared from ferrous scrap. When the ferritic steels are aged thermally, Cu precipitates start appear and disperse finely and homogeneously [1], which may make the steels strengthened by precipitation hardening. In this study, the interaction between Cu precipitates and dislocations was exmined via high-temperature in-situ TEM straining. ExperimentalCu-added ferritic stainless steel (Fe-18.4%Cr-1.5%Cu) was used in the present study. Specimen was aged at1073 K for 360 ks. Samples for TEM observation were prepared by focused ion beam (FIB; Quanta 3D 200i) method. Microstructure of specimen was analyzed by JEM-3200FSK and high-temperature in-situ TEM straining was conducted using JEM-1300NEF. Results and discussionInteraction between Cu precipitates and dislocation is seen from consecutive TEM images acquired by in-situ TEM straining at 1073 K, as shown in Fig.1. The size of Cu precipitates was about 70 nm and several dislocations were present within the field of view. In particular, progressing dislocations contacted with the Cu precipitate at right angle, as indicated by arrows in Fig.1 (b) to (d). This result implies that there is an attractive interaction between dislocations and the Cu precipitate. This is attributed to the fact that Stress field of dislocations was easily relaxed in interface between the Cu precipitate and matrix because of lattice and interface diffusion as well as slip in the interface [2,3]. Furthermore, dislocations pass through the particle after contacting it, so that the interaction with dislocations and particles should be explained by Srolovitz mechanism [4].jmicro;63/suppl_1/i28/DFU083F1F1DFU083F1Fig. 1.TEM images foucused on interaction with dislocations and partticles. © The Author 2014. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

  13. Investigating Processes of Nanocrystal Formation and Transformation via Liquid Cell TEM

    DEFF Research Database (Denmark)

    Nielsen, Michael H.; Li, Dongsheng; Zhang, Hengzhong

    2014-01-01

    and spatial resolution of experimental techniques that can observe dynamic processes in a bulk solution. Here we report results from liquid cell transmission electron microscopy studies of nucleation and growth of Au, CaCO3, and iron oxide nanoparticles. We show how these in situ data can be used to obtain...... direct evidence for the mechanisms underlying nanoparticle crystallization as well as dynamic information that provide constraints on important energetic parameters not available through ex situ methods....

  14. Investigation of C3 S hydration mechanism by transmission electron microscope (TEM) with integrated Super-XTM EDS system.

    Science.gov (United States)

    Sakalli, Y; Trettin, R

    2017-07-01

    Tricalciumsilicate (C 3 S, Alite) is the major component of the Portland cement clinker. Hydration of Alite is decisive in influencing the properties of the resulting material. This is due to its high content in cement. The mechanism of the hydration of C 3 S is very complicated and not yet fully understood. There are different models describing the hydration of C 3 S in various ways. In this work for a better understanding of hydration mechanism, the hydrated C 3 S was investigated by using the transmission electron microscope (TEM) and for the first time, the samples for the investigations were prepared by using of focused ion beam from sintered pellets of C 3 S. Also, an FEI Talos F200x with an integrated Super-X EDS system was used for the investigations. FEI Talos F200X combines outstanding high-resolution S/TEM and TEM imaging with energy dispersive X-ray spectroscopy signal detection, and 3D chemical characterization with compositional mapping. TEM is a very powerful tool for material science. A high energy beam of electrons passes through a very thin sample, and the interactions between the electrons and the atoms can be used to observe the structure of the material and other features in the structure. TEM can be used to study the growth of layers and their composition. TEM produces high-resolution, two-dimensional images and will be used for a wide range of educational, science and industry applications. Chemical analysis can also be performed. The purpose of these investigations was to get the information about the composition of the C-S-H phases and some details of the nanostructure of the C-S-H phases. © 2017 The Authors Journal of Microscopy © 2017 Royal Microscopical Society.

  15. ANALISIS PARAMETER JARINGAN HSDPA KONDISI INDOOR DENGAN TEMS INVESTIGATION DAN G-NETTRACK PRO

    OpenAIRE

    Dewa Made Mahendra Yudha; Pande Ketut Sudiarta; Ngurah Indra ER

    2016-01-01

    Penggunaan teknologi dalam sistem komunikasi bergerak sudah berkembang cukup pesat. Salah satu contohnya ada teknologi HSDPA. Pihak provider biasanya melakukan metode walk test untuk mengecek kekuatan sinyal dengan menggunakan software TEMS Investigtions. Dengan kemajuannya Teknologi walk test dapat diterapkan dengan lebih mudah yaitu menggunakan perangkat android yang sudah terinstal aplikasi G-Net track Pro. Pada penelitian ini, akan menggunakan tahapan sesuai alur yang ada pada metode pene...

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-10-01

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

  17. "Rinse and trickle": a protocol for TEM preparation and investigation of inorganic fibers from biological material.

    Science.gov (United States)

    Vigliaturo, Ruggero; Capella, Silvana; Rinaudo, Caterina; Belluso, Elena

    2016-07-01

    The purpose of this work is to define a sample preparation protocol that allows inorganic fibers and particulate matter extracted from different biological samples to be characterized morphologically, crystallographically and chemically by transmission electron microscopy-energy dispersive spectroscopy (TEM-EDS). The method does not damage or create artifacts through chemical attacks of the target material. A fairly rapid specimen preparation is applied with the aim of performing as few steps as possible to transfer the withdrawn inorganic matter onto the TEM grid. The biological sample is previously digested chemically by NaClO. The salt is then removed through a series of centrifugation and rinse cycles in deionized water, thus drastically reducing the digestive power of the NaClO and concentrating the fibers for TEM analysis. The concept of equivalent hydrodynamic diameter is introduced to calculate the settling velocity during the centrifugation cycles. This technique is applicable to lung tissues and can be extended to a wide range of organic materials. The procedure does not appear to cause morphological damage to the fibers or modify their chemistry or degree of crystallinity. The extrapolated data can be used in interdisciplinary studies to understand the pathological effects caused by inorganic materials.

  18. ANALISIS KUAT SINYAL DAN KUALITAS PANGGILAN JARINGAN GSM INDOOR DENGAN TEMS INVESTIGATION DAN G-NETTRACK PRO

    Directory of Open Access Journals (Sweden)

    Ida Bagus Ari Budiarta

    2016-03-01

    Full Text Available Kebutuhan akan teknologi GSM merupakan tantangan bagi provider untuk memberikan pelayanan terbaik bagi pengguna layanannya. Dalam proses layanan tersebut kemungkinan besar terdapat masalah yang terjadi. Pihak provider biasanya melakukan walk test untuk mengecek kekuatan sinyal yang dipancarkan oleh antena pemancar di dalam ruangan. Kebanyakan pihak provider menggunakan TEMS Investigation dalam melakukan walk test. Biaya walk test dengan TEMS Investigation bisa dikatakan cukup mahal. Namun dengan berkembangnya teknologi, walk test juga bisa dilakukan menggunakan smartphone Android dengan menggunakan G-NetTrack Pro. Dalam penelitian ini dibandingkan kualitas hasil pengukuran parameter kuat sinyal yaitu RSL dan parameter kualitas panggilan yaitu RxQual, CSSR, dan DCR antara software TEMS Investigation dengan G-NetTrack Pro berdasarkan metode walk test pada jaringan GSM indoor 1800 MHz di Matahari Duta Plaza. Secara keseluruhan, G-NetTrack Pro mampu menampilkan data yang dibutuhkan pada penelitian tetapi tidak sedetail TEMS Investigation, sehingga untuk pengenalan awal walk test, software G-NetTrack Pro bisa digunakan sebagai bahan pembelajaran.

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

    International Nuclear Information System (INIS)

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

    1997-01-01

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

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

    DEFF Research Database (Denmark)

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

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

  1. Resistive switching mechanism in the one diode-one resistor memory based on p+-Si/n-ZnO heterostructure revealed by in-situ TEM

    Science.gov (United States)

    Zhang, Lei; Zhu, Liang; Li, Xiaomei; Xu, Zhi; Wang, Wenlong; Bai, Xuedong

    2017-03-01

    One diode-one resistor (1D1R) memory is an effective architecture to suppress the crosstalk interference, realizing the crossbar network integration of resistive random access memory (RRAM). Herein, we designed a p+-Si/n-ZnO heterostructure with 1D1R function. Compared with the conventional multilayer 1D1R devices, the structure and fabrication technique can be largely simplified. The real-time imaging of formation/rupture process of conductive filament (CF) process demonstrated the RS mechanism by in-situ transmission electron microscopy (TEM). Meanwhile, we observed that the formed CF is only confined to the outside of depletion region of Si/ZnO pn junction, and the formation of CF does not degrade the diode performance, which allows the coexistence of RS and rectifying behaviors, revealing the 1D1R switching model. Furthermore, it has been confirmed that the CF is consisting of the oxygen vacancy by in-situ TEM characterization.

  2. Resistive switching mechanism in the one diode-one resistor memory based on p+-Si/n-ZnO heterostructure revealed by in-situ TEM.

    Science.gov (United States)

    Zhang, Lei; Zhu, Liang; Li, Xiaomei; Xu, Zhi; Wang, Wenlong; Bai, Xuedong

    2017-03-21

    One diode-one resistor (1D1R) memory is an effective architecture to suppress the crosstalk interference, realizing the crossbar network integration of resistive random access memory (RRAM). Herein, we designed a p + -Si/n-ZnO heterostructure with 1D1R function. Compared with the conventional multilayer 1D1R devices, the structure and fabrication technique can be largely simplified. The real-time imaging of formation/rupture process of conductive filament (CF) process demonstrated the RS mechanism by in-situ transmission electron microscopy (TEM). Meanwhile, we observed that the formed CF is only confined to the outside of depletion region of Si/ZnO pn junction, and the formation of CF does not degrade the diode performance, which allows the coexistence of RS and rectifying behaviors, revealing the 1D1R switching model. Furthermore, it has been confirmed that the CF is consisting of the oxygen vacancy by in-situ TEM characterization.

  3. In-situ TEM visualization of vacancy injection and chemical partition during oxidation of Ni-Cr nanoparticles.

    Science.gov (United States)

    Wang, Chong-Min; Genc, Arda; Cheng, Huikai; Pullan, Lee; Baer, Donald R; Bruemmer, Stephen M

    2014-01-14

    Oxidation of alloy often involves chemical partition and injection of vacancies. Chemical partition is the consequence of selective oxidation, while injection of vacancies is associated with the differences of diffusivity of cations and anions. It is far from clear as how the injected vacancies behave during oxidation of metal. Using in-situ transmission electron microscopy, we captured unprecedented details on the collective behavior of injected vacancies during oxidation of metal, featuring an initial multi-site oxide nucleation, vacancy supersaturation, nucleation of a single cavity, sinking of vacancies into the cavity and accelerated oxidation of the particle. High sensitive energy dispersive x-ray spectroscopy mapping reveals that Cr is preferentially oxidized even at the initial oxidation, leading to a structure that Cr oxide is sandwiched near the inner wall of the hollow particle. The work provides a general guidance on tailoring of nanostructured materials involving multi-ion exchange such as core-shell structured composite nanoparticles.

  4. Investigations of oxide particles in unirradiated ODS-Eurofer by TEM and 3D atom probe methods

    International Nuclear Information System (INIS)

    Aleev, A.A.; Iskandarov, N.A.; Nikitin, A.A.; Rogizhkin, S.V.; Zaluzhny, A.G.; Klimenkov, M.; Lindau, R.; Moeslang, A.; Vladimirov, P.

    2009-01-01

    Oxide dispersion strengthened steels possess better high-temperature creep and radiation resistance than conventionally produced ferritic/martensitic steels. This behavior is mainly caused by the presence of highly dispersed and extremely stable oxide particles with sizes of few nanometers. One of the promising oxides used for dispersion strengthening was yttria (Y 2 O 3 ), which was introduced into EUROFER by mechanical alloying followed by the hot isostatic pressing at temperature around 1000-1200 dg. C and pressure ∼100 MPa. It was found that mechanical properties were strongly depended on size and spatial distribution of the precipitates. Therefore considerable efforts are focused on the investigation of the chemical composition and orientation of precipitates with respect to the steel matrix. Recent studies of Eurofer ODS steel (9%-CrWVTa) by SANS revealed the presence of high number density structural features with a size of approximately one nanometer. At the same time, previous studies by TEM identified only high number of small (6-40 nm) Y 2 O 3 particles. In this work we tried to get a deeper inside into the nanostructure of this material by means of tomographic atom probe and to correlate the results with the picture obtained by TEM. The present investigations revealed fine (∼2 nm) enrichments containing not only yttrium and oxygen but also vanadium and nitrogen. Concentration of vanadium was found to be approximately at the same level as yttrium. Some of the enrichments contained only three or even two elements mentioned above. Estimated number density of enrichments is about (1/5) x 10 23 m -3 . We suppose that these enriched zones might be precursors of the larger precipitates observed by TEM. The thesis seems to be supported by the similarities of the chemical composition and spatial distribution of elements inside enriched zones and nano precipitates studied by atomic probe and analytical TEM methods. (author)

  5. Nanomechanical and in situ TEM characterization of boron carbide thin films on helium implanted substrates: Delamination, real-time cracking and substrate buckling

    Energy Technology Data Exchange (ETDEWEB)

    Framil Carpeño, David, E-mail: david.framil-carpeno@auckland.ac.nz [Department of Chemical and Materials Engineering, The University of Auckland, 20 Symonds Street, Auckland 1010 (New Zealand); Ohmura, Takahito; Zhang, Ling [Strength Design Group, Structural Materials Unit, National Institute for Materials Science, 1-2-1 Sengen, Tsukuba, Ibaraki 305-0047 (Japan); Leveneur, Jérôme [National Isotope Centre, GNS Science, 30 Gracefield Road, Gracefield, Lower Hutt 5010 (New Zealand); Dickinson, Michelle [Department of Chemical and Materials Engineering, The University of Auckland, 20 Symonds Street, Auckland 1010 (New Zealand); Seal, Christopher [International Centre for Advanced Materials, The University of Manchester, Oxford Road, Manchester M13 9PL (United Kingdom); Kennedy, John [National Isotope Centre, GNS Science, 30 Gracefield Road, Gracefield, Lower Hutt 5010 (New Zealand); Hyland, Margaret [Department of Chemical and Materials Engineering, The University of Auckland, 20 Symonds Street, Auckland 1010 (New Zealand)

    2015-07-15

    Boron carbide coatings deposited on helium-implanted and unimplanted Inconel 600 were characterized using a combination of nanoindentation and transmission electron microscopy. Real-time coating, cracking and formation of slip bands were recorded using in situ TEM-nanoindentation, allowing site specific events to be correlated with specific features in their load–displacement curves. Cross-sections through the residual indent impression showed a correlation between pop-outs in the load–displacement curves and coating delamination, which was confirmed with cyclic indentation experiments. Inconel exhibits (-11-1) and (1-1-1) twin variants in its deformed region beneath the indenter, organized in bands with a ladder-like arrangement. The nanomechanical properties of the metal–ceramic coating combinations exhibit a marked substrate effect as a consequence of helium implantation.

  6. Nanomechanical and in situ TEM characterization of boron carbide thin films on helium implanted substrates: Delamination, real-time cracking and substrate buckling

    International Nuclear Information System (INIS)

    Framil Carpeño, David; Ohmura, Takahito; Zhang, Ling; Leveneur, Jérôme; Dickinson, Michelle; Seal, Christopher; Kennedy, John; Hyland, Margaret

    2015-01-01

    Boron carbide coatings deposited on helium-implanted and unimplanted Inconel 600 were characterized using a combination of nanoindentation and transmission electron microscopy. Real-time coating, cracking and formation of slip bands were recorded using in situ TEM-nanoindentation, allowing site specific events to be correlated with specific features in their load–displacement curves. Cross-sections through the residual indent impression showed a correlation between pop-outs in the load–displacement curves and coating delamination, which was confirmed with cyclic indentation experiments. Inconel exhibits (-11-1) and (1-1-1) twin variants in its deformed region beneath the indenter, organized in bands with a ladder-like arrangement. The nanomechanical properties of the metal–ceramic coating combinations exhibit a marked substrate effect as a consequence of helium implantation

  7. 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.

  8. Anomalous Resistance Hysteresis in Oxide ReRAM: Oxygen Evolution and Reincorporation Revealed by In Situ TEM.

    Science.gov (United States)

    Cooper, David; Baeumer, Christoph; Bernier, Nicolas; Marchewka, Astrid; La Torre, Camilla; Dunin-Borkowski, Rafal E; Menzel, Stephan; Waser, Rainer; Dittmann, Regina

    2017-06-01

    The control and rational design of redox-based memristive devices, which are highly attractive candidates for next-generation nonvolatile memory and logic applications, is complicated by competing and poorly understood switching mechanisms, which can result in two coexisting resistance hystereses that have opposite voltage polarity. These competing processes can be defined as regular and anomalous resistive switching. Despite significant characterization efforts, the complex nanoscale redox processes that drive anomalous resistive switching and their implications for current transport remain poorly understood. Here, lateral and vertical mapping of O vacancy concentrations is used during the operation of such devices in situ in an aberration corrected transmission electron microscope to explain the anomalous switching mechanism. It is found that an increase (decrease) in the overall O vacancy concentration within the device after positive (negative) biasing of the Schottky-type electrode is associated with the electrocatalytic release and reincorporation of oxygen at the electrode/oxide interface and is responsible for the resistance change. This fundamental insight presents a novel perspective on resistive switching processes and opens up new technological opportunities for the implementation of memristive devices, as anomalous switching can now be suppressed selectively or used deliberately to achieve the desirable so-called deep Reset. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. TEM and TED investigation of Ag/PbTe thin film bilayers.

    Science.gov (United States)

    Mandrino, Đorđe; Marinković, V.

    Morphology and phase structure of Ag/PbTe thin film bilayers were investigated. This system was of particular interest because of interfacial reaction observed previously in an analogous Ag/SnTe system. Reaction products due to the interdiffusion of Ag with the substrate were determined as well as their orientations. They were discussed in view of the reaction products' structural relations to the PbTe.

  10. Environmental TEM investigation of the reduction of α-Fe2O3 nanorods under H2 atmosphere

    DEFF Research Database (Denmark)

    Almeida, Trevor P.; Fay, Michael W.; Zhu, Yanqiu

    2012-01-01

    The thermal reduction of hydrothermally synthesised α-Fe2O3 nanorods (NRs) to Fe3O4 NRs under hydrogen is investigated. Complete reduction of α-Fe2O3 NRs to Fe3O4 NRs was achieved during in situ XRD under 1 bar H2 atmosphere at 360°C. Complementary environmental transmission electron microscope...... investigation at high resolution, during in situ heating under an H2 pressure of 5 mbar at 500°C, provided evidence for the very first stages of transformation, supporting a model for the migration of oxygen along favoured α-Fe2O3 lattice planes during the templated thermal reduction of α-Fe2O3 NRs to Fe3O4 NRs....

  11. A review of in situ investigations in salt

    International Nuclear Information System (INIS)

    Kuehn, K.

    1985-01-01

    In situ investigations for the disposal of radioactive wastes in rock salt formations have the longest history in the field. Well known names are Project Salt Vault (PSV) which was performed in the Lyons Mine, Kansas/USA, and the Asse salt mine in Germany. The overall objective for in situ investigations is twofold: 1. To produce all necessary data for the construction and operation of repositories and 2. to produce all necessary data for a performance assessment for repositories

  12. In situ X-ray investigations of oxygen precipitation in semiconductor silicon; In-situ-Roentgenuntersuchungen der Sauerstoffpraezipitation in Halbleitersilizium

    Energy Technology Data Exchange (ETDEWEB)

    Grillenberger, Hannes

    2011-03-04

    The precipitation of oxygen in Czochralski grown semiconductor silicon is investigated in situ during thermal treatments up to 1000 C with high energy X-rays. All investigations are performed with a focusing Laue diffractometer. The parameters of the diffraction curve are the relative full width at half maximum (rFHWM) and the enhancement of the integral intensity (EII). A readout software has been developed to extract these automatically from the detector image for the measured 220, -220 and 040 Bragg peaks. The sample thickness is set to 15 mm as this enhances the sensitivity of the method and the samples are processed after the strain-field diffraction (SFD) experiments to wafers for an ex situ characterization demanding wafers. Three experimental series with a total of 21 in situ SFD experiments with different thermal treatments have been performed. The slope of the initial temperature ramp is set to 1 K/min in the first and the third series to generate a high precipitate (Bulk Micro Defect, BMD) density. In the second series the slope is chosen as 10 K/min to generate a lower density in the same silicon material. It is shown with all experiments and with preliminary works that the built up of strain during the heat treatment is caused by BMDs during the high temperature period of the treatment. The detection limit of series 1 is found at 7 nm at a density of 10{sup 13}/cm{sup 3}, of series 2 at 40 nm at a density of 2 x 10{sup 8}/cm{sup 3}, and at 8 nm at a density of 4.8 x 10{sup 12}/cm{sup 3} for series 3. The local maximum of the EII at 450 C, which emerges coincident with a local minimum of the rFWHM in series 2 may be caused by thermal donors (TD). With the experiments is shown that SFD operates in the infrared-laser scattering tomography detection range, but also reaches in a region covered only by transmission electron microscopy (TEM) so far. In contrast to these methods SFD is not limited to low temperatures and in situ experiments can be done. Thus

  13. Biomimetic Proteoglycan Interactions with Type I Collagen Investigated via 2D and 3D TEM

    Science.gov (United States)

    Moorehead, Carli

    Collagen is one of the leading components in extracellular matrix (ECM), providing durability, structural integrity, and functionality for many tissues. Regulation of collagen fibrillogenesis and degradation is important in the treatment of a number of diseases from orthopedic injuries to genetic deficiencies. Recently, novel, biocompatible, semi-synthetic biomimetic proteoglycans (BPGs) were developed, which consist of an enzymatically resistant synthetic polymer core and natural chondroitin sulfate bristles. It was demonstrated that BPGs affect type I collagen fibrillogenesis in vitro, as reflected by their impact delaying the kinetic formation of gels similar to native PGs. This indicates that the morphology of collagen scaffolds as well as endogenous ECM could also be modulated by these proteoglycan mimics. However, the imaging modality used previously, reflectance confocal microscopy, did not yield the resolution necessary to spatially localize BPGs within the collagen network or investigate the effect of BPGs on the quality of collagen fibrils produced in an in vitro fibrillogenesis model which is important for understanding the method of interaction. Consequently, a histological technique, electron tomography, was adapted and utilized to 3D image the nano-scale structures within this simplified tissue model. BPGs were found to aid in lateral growth and enhance fibril banding periodicity resulting in structures more closely resembling those in tissue, in addition to attaching to the collagen surface despite the lack of a protein core.

  14. Shallow groundwater investigation using time-domain electromagnetic (TEM) method at Itay El-Baroud, Nile Delta, Egypt

    Science.gov (United States)

    Shaaban, H.; El-Qady, G.; Al-Sayed, E.; Ghazala, H.; Taha, A. I.

    2016-12-01

    The Nile Delta is one of the oldest known ancient delta, largest and most important depositional complex in the Mediterranean sedimentary basin. Furthermore, it is a unique site in Egypt that is suitable for accumulation and preservation of the Quaternary sediments. In this work we applied time-domain electromagnetic (TEM) method to investigate the Quaternary sediments sequence as well as detecting the groundwater aquifer in the area of study. A suite of 232 TEM sounding at 43 stations were carried out using a ;SIROTEM MK-3; time-domain electromagnetic system. A simple coincident loop configuration, in which the same loop transmits and receives signals, was employed with loop side length of 25 m. The 1-D modeling technique was applied to estimate the depth and the apparent resistivity of the interpreted geoelectrical data. Based on the interpretation of the acquired geophysical data, four geoelectric cross-sections were constructed. These sections show that the Upper Quaternary sequence consists of three geoelectric layers. The Holocene Nile mud is separated into two layers: the agricultural root zone (Layer 1) and thick water saturated mud (Layer 2). The Upper Pleistocene sandy aquifer (Layer 3) is very complicated non-linear boundary. This aquifer is the most important unit since it is considered as the main water bearing unit in the study area.

  15. TEM of nanostructured metals and alloys

    International Nuclear Information System (INIS)

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

    2004-01-01

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

  16. INVESTIGATION ON THE MORPHOLOGY AND PROPERTIES OF AGGREGATE STRUCTURES OF NATURAL PHOSPHOLIPIDS IN AQUEOUS SYSTEM USING CRYO-TEM

    Directory of Open Access Journals (Sweden)

    Dwi Hudiyanti

    2012-02-01

    Full Text Available Cryogenic transmission electron microscopy (Cryo-TEM was used to investigate the aggregates morphology and properties of candle tree (Aleurites moluccana endosperm, sesame (Sesamum indicum L. syn. seeds, and coconut (Cocos nucifera endosperm phospholipids in dilute aqueous system. The micrographs showed that candle tree phospholipids formed planar bilayer and cluster of vesicles with lipid droplets, while coconut and sesame phospholipids formed well-defined unilamellar vesicles. The vesicles size could be as small as 50 nm in diameter. Coconut phospholipids also showed a good bending ability. Formation of clusters of vesicles was also found in coconut phospholipids dispersion, but this cluster was easily broken by extrusion through a small pore membrane.

  17. Moessbauer, TEM/SAED and XRD investigation on waste dumps of the Valea lui Stan gold mines

    Energy Technology Data Exchange (ETDEWEB)

    Constantinescu, Serban Grigore, E-mail: sconst@infim.ro [National Institute of Materials Physics, Bucharest-Magurele (Romania); Udubasa, Sorin S.; Udubasa, Gheorghe [University of Bucharest, Fac. of Geology and Geophysics (Romania); Kuncser, Victor; Popescu-Pogrion, Nicoleta; Mercioniu, Ionel; Feder, Marcel [National Institute of Materials Physics, Bucharest-Magurele (Romania)

    2012-03-15

    The complementary investigation techniques, Moessbauer spectroscopy, transmission electron microscopy with selected area electron diffraction (TEM/SAED), X-ray diffraction (XRD) have been used to investigate the fate of the Valea lui Stan, Romania, gold-ore nanoscale-minerals during the long time of residence in the waste dumps. The preliminary investigations showed such waste dumps to contain significant amount of metals which cannot be identified by conventional methods. An intense research activity started up in order to evaluate the possibilities to recycle Valea lui Stan waste dumps and to recover metals by chemical or phytoextraction procedures. The waste dumps naturally show different mineral constituents with clay minerals as major phases, observed by XRD-technique. Although the waste dumps materials have whitish-yellowish colours, MOeSSBAUER technique evidences the presence of the finely dispersed iron bearing minerals. The authors are focusing to inspect and analyze Fe-compounds in the samples collected from Valea lui Stan's waste dumps in order to identify the magnetic phases by Moessbauer technique.

  18. Aggregation and Fibril Morphology of the Arctic Mutation of Alzheimer’s Aβ peptide by CD, TEM, STEM and in situ AFM

    Science.gov (United States)

    Norlin, Nils; Hellberg, Magnus; Filippov, Andrei; Sousa, Alioscka A.; Gröbner, Gerhard; Leapman, Richard D.; Almqvist, Nils; Antzutkin, Oleg N.

    2012-01-01

    Morphology of aggregation intermediates, polymorphism of amyloid fibrils and aggregation kinetics of the “Arctic” mutant of the Alzheimer’s amyloid β-peptide, Aβ(1-40)(E22G), in a physiologically relevant TRIS buffer (pH 7.4) were thoroughly explored in comparison with the human wild type Alzheimer’s amyloid peptide, wt-Aβ(1-40), using both in situ atomic force and electron microscopy, circular dichroism and thioflavin T fluorescence assays. For arc-Aβ(1-40) at the end of the ‘lag’-period of fibrillization an abrupt appearance of ~3 nm size ‘spherical aggregates’ with a homogeneous morphology, was identified. Then, the aggregation proceeds with a rapid growth of amyloid fibrils with a variety of morphologies, while the spherical aggregates eventually disappeared during in situ measurements. Arc-Aβ(1-40) was also shown to form fibrils at much lower concentrations than wt-Aβ(1-40): ≤2.5 μM and 12.5 μM, respectively. Moreover, at the same concentration, 50 μM, the aggregation process proceeds more rapidly for arc-Aβ(1-40): The first amyloid fibrils were observed after ca 72 hours from the onset of incubation as compared to approximately 7 days for wt-Aβ(1-40). Amyloid fibrils of arc-Aβ(1-40) exhibit a large variety of polymorphs, at least five, both coiled and non-coiled distinct fibril structures were recognized by AFM, while at least four types of arc-Aβ(1-40) fibrils were identified by TEM and STEM and their mass-per-length statistics were collected suggesting supramolecular structures with two, four and six β-sheet laminae. Our results suggest a pathway of fibrillogenesis for full-length Alzheimer’s peptides with small and structurally ordered transient spherical aggregates as on-pathway immediate precursors of amyloid fibrils. PMID:22750418

  19. Experimental investigation of in situ cleanable HEPA filters

    International Nuclear Information System (INIS)

    Adamson, D.J.

    2000-01-01

    Savannah River Technology Center (SRTC), High Level Waste Division, Tanks Focus Area, and the Federal Energy Technology Center (FETC) have been investigating high efficiency particulate air (HEPA) filters which can be regenerated or cleaned in situ as an alternative to conventional disposable HEPA filters. This technical report documents concerns pertaining to conventional HEPA filters

  20. In situ research and investigations in OECD countries

    International Nuclear Information System (INIS)

    1988-01-01

    This report explains why deep geological disposal is the most favoured option for the disposal of high level waste and spent fuel, as well as some alpha bearing wastes. It also gives an overview of the main aim and elements of in-situ research and investigation activities in OECD countries, as well as of initiatives taken at an international level

  1. In situ TEM study of the effect of M/A films at grain boundaries on crack propagation in an ultra-fine acicular ferrite pipeline steel

    International Nuclear Information System (INIS)

    Zhong Yong; Xiao Furen; Zhang Jingwu; Shan Yiyin; Wang Wei; Yang Ke

    2006-01-01

    Microstructural refinement of structural materials generally improves their tensile properties but deteriorates their fatigue properties. However, pipeline steels with ultra-fine acicular ferrite (UFAF) possess not only high strength and toughness, but also a low fatigue-crack-growth rate (FCGR) and long fatigue-propagation life. In this paper, the micro-fracture mechanisms of an UFAF pipeline steel are investigated by in situ tensile testing in a transmission electron microscope. The results indicate that a grain-boundary-film structure composed of martensite/austenite could significantly influence the crack propagating behavior in the UFAF steel, consequently lowering the FCGR by enhancing roughness-induced crack closure during cyclic loading

  2. Experimental investigation of in situ cleanable HEPA filter

    International Nuclear Information System (INIS)

    Adamson, D.J.

    1999-01-01

    The Westinghouse Savannah River Company located at the Savannah River Site (SRS) in Aiken, South Carolina is currently testing the feasibility of developing an in situ cleanable high efficiency particulate air (HEPA) filter system. Sintered metal filters are being tested for regenerability or cleanability in simulated conditions found in a high level waste (HLW) tank ventilation system. The filters are being challenged using materials found in HLW tanks. HLW simulated salt, HLW simulated sludge and South Carolina road dust. Various cleaning solutions have been used to clean the filters in situ. The tanks are equipped with a ventilation system to maintain the tank contents at negative pressure to prevent the release of radioactive material to the environment. This system is equipped with conventional disposable glass-fiber HEPA filter cartridges. Removal and disposal of these filters is not only costly, but subjects site personnel to radiation exposure and possible contamination. A test apparatus was designed to simulate the ventilation system of a HLW tank with an in situ cleaning system. Test results indicate that the Mott sintered metal HEPA filter is suitable as an in situ cleanable or regenerable HEPA filter. Data indicates that high humidity or water did not effect the filter performance and the sintered metal HEPA filter was easily cleaned numerous times back to new filter performance by an in situ spray system. The test apparatus allows the cleaning of the soiled HEPA filters to be accomplished without removing the filters from process. This innovative system would eliminate personnel radiation exposure associated with removal of contaminated filters and the high costs of filter replacement and disposal. The results of these investigations indicate that an in situ cleanable HEPA filter system for radioactive and commercial use could be developed and manufactured

  3. Removal of industrial dyes and heavy metals by Beauveria bassiana: FTIR, SEM, TEM and AFM investigations with Pb(II).

    Science.gov (United States)

    Gola, Deepak; Malik, Anushree; Namburath, Maneesh; Ahammad, Shaikh Ziauddin

    2017-10-01

    Presence of industrial dyes and heavy metal as a contaminant in environment poses a great risk to human health. In order to develop a potential technology for remediation of dyes (Reactive remazol red, Yellow 3RS, Indanthrene blue and Vat novatic grey) and heavy metal [Cu(II), Ni(II), Cd(II), Zn(II), Cr(VI) and Pb(II)] contamination, present study was performed with entomopathogenic fungi, Beauveria bassiana (MTCC no. 4580). High dye removal (88-97%) was observed during the growth of B. bassiana while removal percentage for heavy metals ranged from 58 to 75%. Further, detailed investigations were performed with Pb(II) in terms of growth kinetics, effect of process parameters and mechanism of removal. Growth rate decreased from 0.118 h -1 (control) to 0.031 h -1 , showing 28% reduction in biomass at 30 mg L -1 Pb(II) with 58.4% metal removal. Maximum Pb(II) removal was observed at 30 °C, neutral pH and 30 mg L -1 initial metal concentration. FTIR analysis indicated the changes induced by Pb(II) in functional groups on biomass surface. Further, microscopic analysis (SEM and atomic force microscopy (AFM)) was performed to understand the changes in cell surface morphology of the fungal cell. SEM micrograph showed a clear deformation of fungal hyphae, whereas AFM studies proved the increase in surface roughness (RSM) in comparison to control cell. Homogenous bioaccumulation of Pb(II) inside the fungal cell was clearly depicted by TEM-high-angle annular dark field coupled with EDX. Present study provides an insight into the mechanism of Pb(II) bioremediation and strengthens the significance of using entomopathogenic fungus such as B. bassiana for metal and dye removal.

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

    International Nuclear Information System (INIS)

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

    2007-01-01

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

  5. Polymeric nanoparticles stabilized by surfactants investigated by light scattering, small-angle neutron scattering, and Cryo-TEM methods

    Czech Academy of Sciences Publication Activity Database

    Pánek, Jiří; Filippov, Sergey K.; Koňák, Čestmír; Nallet, F.; Noirez, L.; Karlsson, G.; Štěpánek, Petr

    2011-01-01

    Roč. 32, č. 6 (2011), s. 888-897 ISSN 0193-2691 R&D Projects: GA ČR GA202/09/2078 Institutional research plan: CEZ:AV0Z40500505 Keywords : Cryo-TEM * DLS * nanoparticles Subject RIV: BO - Biophysics Impact factor: 0.560, year: 2011

  6. 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...

  7. Investigation of the agglomeration and amorphous transformation effects of neutron irradiation on the nanocrystalline silicon carbide (3C-SiC) using TEM and SEM methods

    Energy Technology Data Exchange (ETDEWEB)

    Huseynov, Elchin M., E-mail: elchin.h@yahoo.com [Department of Nanotechnology and Radiation Material Science, National Nuclear Research Center, Inshaatchilar pr. 4, AZ 1073 Baku (Azerbaijan); Institute of Radiation Problems of Azerbaijan National Academy of Sciences, B.Vahabzade 9, AZ 1143 Baku (Azerbaijan)

    2017-04-01

    Nanocrystalline 3C-SiC particles irradiated by neutron flux during 20 h in TRIGA Mark II light water pool type research reactor. Silicon carbide nanoparticles were analyzed by Scanning Electron Microscope (SEM) and Transmission Electron Microscopy (TEM) devices before and after neutron irradiation. The agglomeration of nanoparticles was studied comparatively before and after neutron irradiation. After neutron irradiation the amorphous layer surrounding the nanoparticles was analyzed in TEM device. Neutron irradiation defects in the 3C-SiC nanoparticles and other effects investigated by TEM device. The effect of irradiation on the crystal structure of the nanomaterial was studied by selected area electron diffraction (SAED) and electron diffraction patterns (EDP) analysis.

  8. Characterization of uranium bioaccumulation on a fungal isolate Geotrichum sp. dwc-1 as investigated by FTIR, TEM and XPS

    International Nuclear Information System (INIS)

    Changsong Zhao; Congcong Ding; Jiali Liao; Jijun Yang; Yuanyou Yang; Jun Tang; Ning Liu; Qun Sun

    2016-01-01

    In this paper, TEM-EDX, FTIR, XPS, PIXE, and EPBS were employed to identify the uranium biosorption behavior and the potential mechanism on cells of Geotrichum sp. dwc-1, isolated from soils. These results displayed that the biosorption behavior was greatly dependent on pH and uranium was absorbed by bounding to amino, phosphate as well as carboxyl functional groups. Uranium biosorption behavior on Geotrichum sp. dwc-1 involves bioaccumulation, electrostatic interaction and ion exchange process. This work throws further light on potential fungal roles these mechanisms for elemental recovery and bioremediation. (author)

  9. Nuclear methods for 'in-situ' geophysical investigations. 2

    International Nuclear Information System (INIS)

    Russell, J.P.; Oliver, D.W.

    1985-01-01

    There has been considerable effort expended by governmental, institutional, and private agencies in the development of suitable materials and instruments for application of nuclear methods for exploration and evaluation of mineral, oil, and gas resources. As a consequence of the peculiar circumstances of in situ investigations, much of the apparatus is, of design and construction, specifically adapted to the environment of the borehole (limited lateral dimension, high temperature and pressure, deep boreholes, etc.) which differs considerably from laboratory conditions. Meeting the needs for reliability and stability under adverse conditions of operation has led to often unique and innovative instrumentation. Much of the development effort has been provided by commercial service organizations whose interests require many details be maintained as proprietary. In addition, the tailoring of services to meet varying environmental and informational constraints has led to a wide range of instrument designs. As a result, it is difficult to provide an exhaustive description of all apparatus available for in situ investigations, rather, in this instance, systems and subsystems will be generically discussed. Radiation sources, detectors, and borehole probe designs are covered. (Auth.)

  10. Spectral and raw quasi in-situ energy dispersive X-ray data captured via a TEM analysis of an ODS austenitic stainless steel sample under 1 MeV Kr2+ high temperature irradiation.

    Science.gov (United States)

    Brooks, Adam J; Yao, Zhongwen

    2017-10-01

    The data presented in this article is related to the research experiment, titled: ' Quasi in-situ energy dispersive X-ray spectroscopy observation of matrix and solute interactions on Y-Ti-O oxide particles in an austenitic stainless steel under 1 MeV Kr 2+ high temperature irradiation' (Brooks et al., 2017) [1]. Quasi in-situ analysis during 1 MeV Kr 2+ 520 °C irradiation allowed the same microstructural area to be observed using a transmission electron microscope (TEM), on an oxide dispersion strengthened (ODS) austenitic stainless steel sample. The data presented contains two sets of energy dispersive X-ray spectroscopy (EDX) data collected before and after irradiation to 1.5 displacements-per-atom (~1.25×10 -3  dpa/s with 7.5×10 14  ions cm -2 ). The vendor software used to process and output the data is the Bruker Esprit v1.9 suite. The data includes the spectral (counts vs. keV energy) of the quasi in-situ scanned region (512×512 pixels at 56k magnification), along with the EDX scanning parameters. The.raw files from the Bruker Esprit v1.9 output are additionally included along with the.rpl data information files. Furthermore included are the two quasi in-situ HAADF images for visual comparison of the regions before and after irradiation. This in-situ experiment is deemed ' quasi' due to the thin foil irradiation taking place at an external TEM facility. We present this data for critical and/or extended analysis from the scientific community, with applications applying to: experimental data correlation, confirmation of results, and as computer based modeling inputs.

  11. Investigation of properties of polyethylene/clay nanocomposites prepared by new in situ Ziegler-Natta catalyst

    International Nuclear Information System (INIS)

    Nikkhah, S. Javan; Ramazani, S.A.; Baniasadi, H.; Tavakolzadeh, F.

    2009-01-01

    This paper is devoted to investigation of morphological and physical-mechanical properties of polyethylene (PE)/clay nanocomposites prepared via in situ polymerization method using bi-supported Ziegler-Natta catalyst. Bentonite type clay and MgCl 2 (ethoxide type) were used as the support of TiCl 4 . Catalyst support and polymerization process have been done in slurry phase using Triisobutylaluminum as the co-catalyst. The microstructure of the nanocomposites was examined by X-ray diffraction (XRD) and transmission electron microscopy (TEM). XRD and TEM indicated that almost fully exfoliated PE/clay nanocomposites were produced successfully using this method. According to permeability measurements, it was found that oxygen permeability values of the nanocomposite samples prepared with in situ polymerization method were dropped more than 200% introducing only 1 wt% clay to polymeric matrix. Differential scanning calorimetry (DSC) results indicated that the crystallization temperatures of samples are significantly higher than that of virgin PE. Moderate thermal stability enhancement of in situ polymerized nanocomposites was confirmed using thermogravimetric analysis (TGA).The storage modulus, Young's modulus and tensile strength of prepared samples were increased where the toughness was declined slightly. It seems that good dispersion and exfoliation of clay during polymerization should be responsible to get more effective reinforcing properties for clay in this method comparing to melt blending method for preparation of polyethylene nanocomposites.

  12. Biomass Conversion in Ionic Liquids - in-situ Investigations

    DEFF Research Database (Denmark)

    Kunov-Kruse, Andreas Jonas

    Due to rising oil prices and global warming caused by CO2 emissions, there is an increased demand for new types of fuels and chemicals derived from biomass. This thesis investigates catalytic conversion of cellulose into sugars in ionic liquids and the important platform chemical 5-hydroxymethylf......Due to rising oil prices and global warming caused by CO2 emissions, there is an increased demand for new types of fuels and chemicals derived from biomass. This thesis investigates catalytic conversion of cellulose into sugars in ionic liquids and the important platform chemical 5......-hydroxymethylfurfural (HMF). The thesis focuses on kinetic and mechanistic investigations using new in-situ FTIR spectroscopic methods based on the ATR-principle. At first the kinetics of cellulose hydrolysis and the simultaneously HMF formation was investigated in the ionic liquid 1-butyl-2,3-dimethylimidazolium...... activation energies suggest that the ionic liquid acts co-catalytic by stabilizing the oxocarbenium transition state. The chromium catalyzed conversion of glucose to HMF in ionic liquid 1-butyl-3-methylimidazolium chloride with CrCl3⋅6H2O and CrCl2 as catalysts was investigated. The CrCl3⋅6H2O catalyst...

  13. 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

  14. Multi-Step Martensitic Transformations in Ni-rich NiTi Alloys - an In-situ TEM Investigation

    Czech Academy of Sciences Publication Activity Database

    Dlouhý, Antonín; Khalil Allafi, J.; Eggeler, G.

    2003-01-01

    Roč. 83, č. 3 (2003), s. 339-363 ISSN 1478-6435 R&D Projects: GA ČR GA106/99/1172 Grant - others:DFG(DE) SFB-459 Institutional research plan: CEZ:AV0Z2041904 Keywords : martensitic transformation * shape memory alloys * transmission electron microscopy Subject RIV: BM - Solid Matter Physics ; Magnetism

  15. Investigation of magnetization reversal process in pinned CoFeB thin film by in-situ Lorentz TEM

    Science.gov (United States)

    Pei, Ke; Xia, Wei-Xing; Wang, Bao-Min; Wen, Xing-Cheng; Sheng, Ping; Liu, Jia-Ping; Liu, Xin-Cai; Li, Run-Wei

    2018-04-01

    Not Available Project supported by the National Key Research and Development Program of China (Grant No. 2016YFA0201102), the National Natural Science Foundation of China (Grant No. 51571208), the Instrument Developing Project of Chinese Academy of Sciences (Grant No. YZ201536), the Program for Key Science and Technology Innovation Team of Zhejiang Province, China (Grant No. 2013TD08), the K C Wong Education Foundation (Grant No. rczx0800), and the K C Wong Magna Fund in Ningbo University.

  16. The effect of clustering on the mobility of dislocations during aging in Nb-microalloyed strip cast steels: In situ heating TEM observations

    International Nuclear Information System (INIS)

    Shrestha, Sachin L.; Xie, Kelvin Y.; Ringer, Simon P.; Carpenter, Kristin R.; Smith, David R.; Killmore, Chris R.; Cairney, Julie M.

    2013-01-01

    Cluster-strengthened Nb-microalloyed strip cast steels are of interest as clustering during aging leads to an enhancement in strength without compromising ductility, resulting in desirable mechanical properties. However, the precise strengthening mechanism is not well understood. Using in situ heating transmission electron microscopy, clustering was found to impede the movement of dislocations during aging. The attractive combination of ductility and strength was attributed to the effects of recovery and the restricted movement of dislocations through clustering

  17. Correlative Cryo-Tem Cryo-Stxm and Cryo-Shxm Investigation of Selenium Bioreduction in a Contaminated Aquifer

    Science.gov (United States)

    Fakra, S.; Luef, B.; Tyliszczak, T.; Castelle, C. J.; Mullin, S. W.; Hug, L. A.; Williams, K. H.; Marcus, M.; Banfield, J. F.

    2015-12-01

    Accurate mapping of the composition and ultrastructure of minerals and cells is key to understanding biogeochemical process in contaminated environments. Here we developed two apparatus that allow correlation of cryogenic transmission electron microscopy (TEM), synchrotron hard X-ray microprobe (SHXM) and scanning transmission X-ray microscopy (STXM) datasets. These cryogenic methods enabled precise determination of the distribution, valence state and structure of selenium in intact biofilms sampled during a biostimulation experiment in a contaminated aquifer near Rifle, CO, USA. Results were replicated in the laboratory via anaerobic selenate-reducing enrichment cultures. 16S rRNA analyses of field-derived biofilm indicated the dominance of Betaproteobacteria from the Comamonadaceae family, and uncultivated members of the Simplicispira genus. The major product in field and culture-derived biofilms consists of ~25-300 nm red amorphous Se0 aggregates of colloidal nanoparticles. Correlative analyses of the cultures provided direct evidence for microbial dissimilatory reduction of Se(VI) to Se(IV) to Se0. X-ray diffraction and Se K-edge extended X-ray absorption fine structure spectroscopy revealed red amorphous Se0 with a first shell Se-Se interatomic distance of 2.339 ± 0.003 Å. STXM showed that these aggregates are strongly associated with a protein-rich biofilm matrix containing acidic polysaccharides. From Rifle groundwater, we isolated a strain that shares 98.9% 16S rRNA gene sequence identity with Dechloromonas aromatica RCB and grows anaerobically by oxidizing acetate and reducing selenate. We refer to this isolate as Dechloromonas selenatis strain RGW99. 3D cryo-electron tomography showed that Se0 particles do not form inside the cytoplasm but rather originate in the cell membrane. The end product of selenate reduction by D. selenatis is 240 ± 66 nm diameter red amorphous Se0 colloidal aggregates. This product was found to be stable for months. Overall

  18. In situ vitrification program treatability investigation progress report

    International Nuclear Information System (INIS)

    Arrenholz, D.A.

    1991-02-01

    This document presents a summary of the efforts conducted under the in situ vitrification treatability study during the period from its initiation in FY-88 until FY-90. In situ vitrification is a thermal treatment process that uses electrical power to convert contaminated soils into a chemically inert and stable glass and crystalline product. Contaminants present in the soil are either incorporated into the product or are pyrolyzed during treatment. The treatability study being conducted at the Idaho National Engineering Laboratory by EG ampersand G Idaho is directed at examining the specific applicability of the in situ vitrification process to buried wastes contaminated with transuranic radionuclides and other contaminants found at the Subsurface Disposal Area of the Radioactive Waste Management Complex. This treatability study consists of a variety of tasks, including engineering tests, field tests, vitrified product evaluation, and analytical models of the in situ vitrification process. 6 refs., 4 figs., 3 tabs

  19. In situ TEM observations of the thermal degradation of the two way memory effect in a Cu-Al-Be alloy

    International Nuclear Information System (INIS)

    Flores-Zuniga, H.; Guenin, G.

    1995-01-01

    A Cu-Al-Be alloy with a martensitic transformation temperature (M S ) lower than room temperature, was trained to induce the two way memory effect (TWME) and the aging effects in austenitic phase were studied by in-situ observations in a Transmission Electron Microscope. The results show movements of dislocations at temperatures where the TWME deformation is well known to decrease after short aging times (about an hour). Since the Burgers vector of these dislocations does not change during aging, and precipitates have been not observed, we concluded that the TWME degrades as a result of modifications in the internal stresses field distribution associated with dislocation movements, that produces a more random orientation of martensitic plates on cooling. (orig.)

  20. Evolution of extended defects in polycrystalline Au-irradiated UO{sub 2} using in situ TEM: Temperature and fluence effects

    Energy Technology Data Exchange (ETDEWEB)

    Onofri, C., E-mail: claire.onofri@cea.fr [CEA, DEN, DEC, F-13108 Saint Paul Lez Durance Cedex (France); Sabathier, C. [CEA, DEN, DEC, F-13108 Saint Paul Lez Durance Cedex (France); Baumier, C.; Bachelet, C. [CSNSM/CNRS, PARIS-SUD University, F-91400 Orsay (France); Palancher, H. [CEA, DEN, DEC, F-13108 Saint Paul Lez Durance Cedex (France); Legros, M. [CEMES/CNRS, F-31055 Toulouse Cedex 4 (France)

    2016-12-15

    In situ Transmission Electron Microscopy irradiations were performed on polycrystalline UO{sub 2} thin foils with 4 MeV gold ions at three different temperatures: 600 °C, room and liquid nitrogen temperature. In order to study the dislocation evolution and to determine the growth mechanisms, the dislocation loop and line densities and the loop size repartition were monitored as a function of fluence, and irradiation temperature. We show that dislocation loops, with Burgers vectors along the <110> directions, evolve into dislocation lines with increasing fluence by a loop overlapping mechanism. Furthermore, a fluence offset is highlighted between the irradiations performed at high and low temperature due to an increase of the defect mobility. Indeed, a growth by Oswald ripening is probably activated at room temperature and 600 °C and changes the kinetic evolution of loops into lines. After this transformation, and for all the irradiation temperatures, a steady state equilibrium is reached where both extended defects (dislocation lines and small dislocations loops -around 5 nm in size-) are observed simultaneously. A continuous nucleation of small dislocation loops and of nanometer-sized cavities formed directly by irradiation is also highlighted.

  1. In-Situ Investigation of Local Boundary Migration During Recrystallization

    DEFF Research Database (Denmark)

    Zhang, Yubin; Godfrey, Andy; Juul Jensen, Dorte

    2014-01-01

    A combination of electron channeling contrast (ECC) and electron backscatter diffraction pattern (EBSP) techniques has been used to follow in situ the migration during annealing at 323 K (50 A degrees C) of a recrystallizing boundary through the deformed matrix of high-purity aluminum rolled to 8...

  2. In situ vitrification program treatability investigation progress report

    International Nuclear Information System (INIS)

    Arrenholz, D.A.

    1990-12-01

    This document presents a summary of the efforts conducted under the in situ vitrification treatability study during the period from its initiation in FY-88 until FY-90. In situ vitrification is a thermal treatment process that uses electrical power to convert contaminated soils into a chemically inert and stable glass and crystalline product. Contaminants present in the soil are either incorporated into the product or are pyrolyzed during treatment. The treatability study being conducted at the Idaho National Engineering Laboratory by EG ampersand G Idaho is directed at examining the specific applicability of the in situ vitrification process to buried wastes contaminated with transuranic radionuclides and other contaminants found at the Subsurface Disposal Area of the Radioactive Waste Management Complex. This treatability study consists of a variety of tasks, including engineering tests, field tests, vitrified product evaluation, and analytical models of the ISV process. The data collected in the course of these efforts will address the nine criteria set forth in the Comprehensive Environmental Response, Compensation, and Liability Act, which will be used to identify and select specific technologies to be used in the remediation of the buried wastes at the Subsurface Disposal Area. 6 refs., 4 figs., 3 tabs

  3. Investigation of InN layers grown by MOCVD using analytical and high resolution TEM: The structure, band gap, role of the buffer layers

    International Nuclear Information System (INIS)

    Ruterana, P.; Abouzaid, M.; Gloux, F.; Maciej, W.; Doualan, J.L.; Drago, M.; Schmidtling, T.; Pohl, U.W.; Richter, W.

    2006-01-01

    In this work we investigate the microstructure of InN layers grown by MOCVD on different buffer layers using TEM (InN, GaN). The large mismatch between the various lattices (InN, sapphire or GaN) leads to particular interface structures. Our local analysis allows to show that at atomic scale, the material has the InN lattice parameters and that no metallic In precipitates are present, meaning that the PL emission below 0.8 eV is a genuine property of the InN semiconductor. It is also shown that the N polar layers, which exhibit a 2D growth, have poorer PL emission than In polar layers. (copyright 2006 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  4. Tems Investigation -ohjelman päivittäminen versioon 10.0, mittaukset 3G-verkossa ja tulosten analysointi

    OpenAIRE

    Malakhina, Julia

    2010-01-01

    Insinöörityön tavoitteena oli päivittää Ascomin Tems Investigation-ohjelmaa versioon 10.0 Metropolialle ja selvittää samalla, minkälaisia uusia ominaisuuksia ja parannuksia ohjelma sisältää edellisempiin versioihin 9.1 ja 9.0 verrattuna. Tavoitteena oli myös näyttää, miten ohjelma toimii käytännössä eli suorittaa mittauksia 3G-verkossa käyttäen tätä ohjelmaa ja esittää mittauksista saadut tulokset. Työ aloitettiin perehtymällä 3G-perheeseen kuuluvaan UMTS-järjestelmään ja sen verkkoarkkitehtu...

  5. Investigation of the nanoscale two-component ZnS-ZnO heterostructures by means of HR-TEM and X-ray based analysis

    Science.gov (United States)

    Pankin, I. A.; Polozhentsev, O. E.; Soldatov, M. A.; Bugaev, A. L.; Tsaturyan, A.; Lomachenko, K. A.; Guda, A. A.; Budnyk, A. P.; Lamberti, C.; Soldatov, A. V.

    2018-06-01

    This article is devoted to the spectroscopic characterization of ZnS-ZnO nanoscale heterostructures synthesized by the microwave-assisted solvothermal method. The synthesized samples were investigated by means of X-ray powder diffraction (XRPD), high energy resolution fluorescence detected X-ray absorption near-edge-structure (HERFD-XANES) spectroscopy, valence-to-core X-ray emission spectroscopy (VtC-XES) and high resolution transmission electron microscopy (HR-TEM) as well as energy dispersive X-ray spectroscopy (EDX). The average crystallite size estimated by the broadening of XRPD peaks increases from 2.7 nm to 3.7 nm in the temperature range from 100 °C to 150 °C. HR-TEM images show that nanoparticles are arranged in aggregates with the 60-200 nm size. Theoretical estimation shows that the systems synthesized at higher temperatures more prone to the agglomeration. The full profile Reitveld analysis of XRPD data reveals the formation of hexagonal zinc sulfide structure, whereas electron diffraction data reveal also the formation of cubic zinc sulfide and claim the polymorphous character of the system. High energy resolution Zn K-edge XANES data unambiguously demonstrate the presence of a certain amount of the zinc oxide which is likely to have an amorphous structure and could not be detected by XRPD. Qualitative analysis of XANES data allows deriving ZnS/ZnO ratio as a function of synthesis temperature. EDX analysis depicts homogeneous distribution of ZnS and amorphous ZnO phases across the conglomerates. A complementary element-selective valence to core X-ray emission spectroscopy evidences formation of two-component system and confirms estimations of ZnS/ZnO fractions obtained by linear combination fit of XANES data.

  6. Simultaneous Investigation of Sediment Transport and Water Quality Parameters Using An In Situ Measurement Device

    Science.gov (United States)

    Prochnow, J. V.

    Though quality of surface waters has improved remarkably over the last twenty years, the contaminant load of soft cohesive sediments remained comparatively unimproved. That is why the new European water framework directive addresses contaminant loaded sediments and postulates criteria for assessing sediment quality. Surveys into contaminated sediment behaviour have revealed adsorption/desorption characteristics of individual toxins. Biomonitoring of pollutant pressure on specific benthic organ- isms on the other hand can be useful to elucidate potential dangers to aquatic ecosys- tems. However, it is yet unknown how a given contaminant loaded sediment will re- spond to different hypercritical flow conditions in terms of release rates and partition- ing of xenobiotica. On this account a small in situ measuring device (EROSIMESS) was constructed, that features simultaneous determination of suspended sediment con- centration (optical turbidity meter), dissolved oxygen levels, pH and temperature (membrane probes) under predefined hydraulic conditions. Samples of the suspen- sion can be withdrawn for subsequent chemical analysis. Bottom shear stresses up to 5N/m2 can be generated by means of a propeller that resides in cylindrical perspex tube (erosion chamber) two centimeters above the sediment bed. Baffles on the in- ner wall of the cylinder prevent a solid body rotation of the suspension by creating additional turbulence and a second propeller straight beneath the concentration me- ter inhibits the development of a concentration gradient within the chamber. A small CCD-camera is used to control positioning of the device. It can be used in water- depths up to 5m. The control unit consists of a trigger box and an ordinary laptop computer running LabView. EROSIMESS has been successfully used in various stud- ies on contaminant release, eutrophication, and SOD (sediment oxygen demand) in rivers (Spree: Germany; Maun: UK), reservoirs (Heimbach, Haus Ley: Germany), and

  7. In situ investigation of the tensile deformation of laser welded Ti{sub 2}AlNb joints

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Kezhao; Ni, Longchang; Lei, Zhenglong, E-mail: leizhenglong@hit.edu.cn; Chen, Yanbin; Hu, Xue

    2017-01-15

    The tensile deformation behavior of laser welded Ti{sub 2}AlNb joints was investigated using in situ analysis methods. The fracture mode of the single-B2-phase fusion zone was quasi-cleavage at room temperature and intergranular at 650 °C, while that of base metal was microvoid coalescence at both room temperature and 650 °C. Tensile deformation at room temperature was observed using in situ SEM tensile testing. In base metal, microcracks nucleated and propagated mainly within the O phase or along O/B2 phase boundaries. While both the cross- and multi-slips were found in the single-B2-phase fusion zone, a confocal laser scanning microscopy was used to observe the crack initiation and propagation process in situ at 650 °C. Cracks mainly formed along the B2/O phase boundaries in base metal, along the fragile grain boundaries of B2 phase in the fusion zone. The thermal simulation experiment and following TEM analysis indicated that the precipitation of continuous O-phase films along the B2 grain boundaries resulted in the high temperature brittleness of laser welded Ti{sub 2}AlNb joints. - Highlights: •Cracks formed within O phase or along B2/O boundaries in the base metal. •Cross- and multi-slips relieved stress in the fusion zone at room temperature. •Cracks mainly formed along the B2/O boundaries at 650 °C. •In the fusion zone, intergranular cracks were in situ observed at 650 °C. •O-phase films along B2 grain boundaries caused the high temperature brittleness.

  8. Accelerator-TEM interface facility and application

    International Nuclear Information System (INIS)

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

    2010-01-01

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

  9. In-situ investigation of the hydrogen release mechanism in bulk Mg2NiH4

    Science.gov (United States)

    Tran, Xuan Quy; McDonald, Stuart D.; Gu, Qinfen; Yamamoto, Tomokazu; Shigematsu, Koji; Aso, Kohei; Tanaka, Eishi; Matsumura, Syo; Nogita, Kazuhiro

    2017-02-01

    Hydrogen storage is an important aspect to enable the so-called hydrogen economy. Mg-Ni alloys are among the most promising candidates for solid-state hydrogen storage systems yet many questions remain unanswered regarding the hydriding/dehydriding mechanism of the alloys. Mg2NiH4 particularly has received much attention both for its potential as a hydrogen storage medium and also exhibits interesting properties relating to its different polymorphs. Here, the dehydriding mechanism in bulk Mg2NiH4 is investigated using in-situ ultra-high voltage transmission electron microscopy (TEM) combined with Synchrotron powder X-ray diffraction (XRPD) and differential scanning calorimetry (DSC). We find that the hydrogen release is based on a mechanism of nucleation and growth of Mg2NiHx (x∼0-0.3) solid solution grains and is greatly enhanced in the presence of crystal defects occurring as a result of the polymorphic phase transformation. Also importantly, with atomic resolution TEM imaging a high density of stacking faults is identified in the dehydrided Mg2NiHx (x∼0-0.3) lattices.

  10. Tomographic Heating Holder for In Situ TEM

    DEFF Research Database (Denmark)

    Gontard, Lionel C.; Dunin-Borkowski, Rafal E.; Fernández, Asunción

    2014-01-01

    distributions and changes in active surface area are quantified from tilt series of images acquired after subjecting the specimens to increasing temperatures. The porosity of the alumina support and the sintering mechanisms of the catalysts are shown to depend on distance from the heating filament....

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

    Science.gov (United States)

    Wagner, Andrew James

    photovoltaic performance. The annealing process, however, requires exceptionally high temperature (> 600 °C) and time (tens of hours), limiting throughput and costing energy. In an effort to fabricate polycrystalline solar cells at lower cost, large ( 30 nm) silicon nanocrystals were incorporated into hydrogenated amorphous silicon (a Si:H) thin films. When annealed, the embedded nanocrystals were expected to act as heterogeneous nucleation sites and crystallize the surrounding amorphous matrix. When observed in the TEM, an additional and unexpected event was observed. At the boundary between the nanocrystal and amorphous matrix, nanocavities were observed to form. Continued annealing resulted in movement of the cavities away from the nanocrystal while leaving behind a crystalline tail. The origins and fundamental mechanisms of this phenomenon were examined by in-situ heating TEM and ex-situ crystallographic TEM techniques. We demonstrate a mechanism of solid-phase crystallization (SPC) enabled by nanoscale cavities formed at the interface between an hydrogenated amorphous silicon film and embedded 30 nm to 40 nm Si nanocrystals. The nanocavities, 10 nm to 25 nm across, have the unique property of an internal surface that is part amorphous and part crystalline, enabling capillarity-driven diffusion from the amorphous to the crystalline domain. The nanocavities propagate rapidly through the amorphous phase, up to five times faster than the SPC growth rate, while "pulling behind" a crystalline tail. It is shown that twin boundaries exposed on the crystalline surface accelerate crystal growth and influence the direction of nanocavity propagation. The mechanical properties and mechanisms of plasticity in these same silicon nanocubes have also been investigated. The strain-dependent mechanical properties and the underlying mechanisms governing the elastic-plastic response are explored in detail. Elastic strains approaching 7% and flow stresses of 11 GPa were observed

  12. M23C6 carbides and Cr2N nitrides in aged duplex stainless steel: A SEM, TEM and FIB tomography investigation.

    Science.gov (United States)

    Maetz, J-Y; Douillard, T; Cazottes, S; Verdu, C; Kléber, X

    2016-05-01

    The precipitation evolution during ageing of a 2101 lean duplex stainless steel was investigated, revealing that the precipitate type and morphology depends on the nature of the grain boundary. Triangular M23C6 carbides precipitate only at γ/δ interfaces and rod-like Cr2N nitrides precipitate at both γ/δ and δ/δ interfaces. After 15min of ageing, the M23C6 size no longer evolves, whereas that of the Cr2N continues to evolve. For Cr2N, the morphology is maintained at γ/δ interfaces, whereas percolation occurs to form a continuous layer at δ/δ interfaces. By combining 2D and 3D characterisation at the nanoscale using transmission electron microscopy (TEM) and focused ion beam (FIB) tomography, a complete description of the precipitation evolution was obtained, including the composition, crystallographic structure, orientation relationship with the matrix phases, location, morphology, size and volume fraction. Copyright © 2016 Elsevier Ltd. All rights reserved.

  13. Accelerator-tem interface facility and application

    International Nuclear Information System (INIS)

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

    2010-01-01

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

  14. Is the TEM obsolescent?

    International Nuclear Information System (INIS)

    Williams, D.B.

    2002-01-01

    Full text: The TEM has undergone many revolutions since its invention 70 years ago, but is now a very mature instrument. The major functions of imaging, diffraction and analysis were invented decades ago. Much of the instrument development in the last 20 years has come in peripheral improvements such as ease of operation and computer control which, nevertheless, have made no substantial differences to basic operational methods. The TEM remains a predominantly manual instrument, still providing analog viewing and recording, well into the digital age. Indeed any operator of a Siemens Elmiskop 1 TEM from the 1950s would be more than skilled enough to operate a modern FEG TEM, with little more than a few minutes of training. It is arguable that no other cutting-edge scientific instrument is so basically unchanged in its method of operation over the last five decades, as the TEM. This state of affairs is a recipe for obsolescence. Students today are not interested in mastering the complexities of balancing potentiometers (which are still necessary for good centered dark-field operation) or manipulating sets of tilt controls to move from to , while fighting to maintain eucentricity and a recognizable image on the screen at 200 kX. Students are already masters of the mouse, keyboard or joystick and expect information to be generated, stored, processed and analyzed rapidly and efficiently under full computer control. We need to provide today's students with an instrument to challenge their skills, not those of their parents. There is nothing preventing the creation of a TEM that is under full computer control, except perhaps the notion that the TEM is an instrument worthy of mastery per se, rather than being simply a tool for the characterization of materials. In contrast, the SEM has never been seen as a 'real' electron microscope and consequently has found its way into many more research, education and commercial operations than the TEM. The SEM has also evolved

  15. Anthropogenic wetlands due to over-irrigation of desert areas: a challenging hydrogeological investigation with extensive geophysical input from TEM and MRS measurements

    Science.gov (United States)

    Behroozmand, Ahmad Ali; Teatini, Pietro; Bjergsted Pedersen, Jesper; Auken, Esben; Tosatto, Omar; Vest Christiansen, Anders

    2017-03-01

    During the last century, many large irrigation projects were carried out in arid lands worldwide. Despite a tremendous increase in food production, a common problem when characterizing these zones is land degradation in the form of waterlogging. A clear example of this phenomenon is in the Nubariya depression in the Western Desert of Egypt. Following the reclamation of desert lands for agricultural production, an artificial brackish and contaminated pond started to develop in the late 1990s, which at present extends for about 2.5 km2. The available data provide evidence of a simultaneous general deterioration of the groundwater system. An extensive hydrogeophysical investigation was carried out in this challenging environment using magnetic resonance sounding (MRS) and ground-based time-domain electromagnetic (TEM) techniques with the following main objectives: (1) understanding the hydrological evolution of the area; (2) characterizing the hydrogeological setting; and (3) developing scenarios for artificial aquifer remediation and recharge. The integrated interpretation of the geophysical surveys provided a hydrogeological picture of the upper 100 m sedimentary setting in terms of both lithological distribution and groundwater quality. The information is then used to set up (1) a regional groundwater flow and (2) a local density-dependent flow and transport numerical model to reproduce the evolution of the aquifer system and develop a few scenarios for artificial aquifer recharge using the treated water provided by a nearby wastewater treatment plant. The research outcomes point to the hydrological challenges that emerge for the effective management of water resources in reclaimed desert areas, and they highlight the effectiveness of using advanced geophysical and modeling methodologies.

  16. Experimental in situ investigations of turbulence under high pressure.

    Science.gov (United States)

    Song, Kwonyul; Al-Salaymeh, Ahmed; Jovanovic, Jovan; Rauh, Cornelia; Delgado, Antonio

    2010-02-01

    In tube injection systems applied in high-pressure processing of packed biomaterials and foods, the pressure-transmitting medium is injected into the vessel to increase the pressure up to 1000 MPa, generating a submerged liquid-free jet. The presence of a turbulent-free jet during the pressurization phase and its positive influence on the homogeneity of the product treatment has already been examined by computational fluid dynamics investigations. However, no experimental data have supported the existence and properties of turbulent flow under high-pressure (HP) conditions up to 400 MPa. This contribution presents the development of two experimental setups: HP-laser Doppler anemometry and HP-hot wire anemometry. For the first time the time-averaged velocity profiles of a free jet during pressurization up to 300 MPa at different Reynolds numbers (Re) have been obtained. In this article, the dependence of the velocity profiles on the Re is discussed in detail. Moreover, the relaminarization phenomenon of the turbulent pipe flow most likely caused by the compressibility effects and viscosity changes of the pressure-transmitting medium is examined.

  17. Characterization of TEM1/endosialin in human and murine brain tumors

    International Nuclear Information System (INIS)

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

    2009-01-01

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

  18. Experimental Investigation and High Resolution Simulation of In-Situ Combustion Processes

    Energy Technology Data Exchange (ETDEWEB)

    Margot Gerritsen; Tony Kovscek

    2008-04-30

    This final technical report describes work performed for the project 'Experimental Investigation and High Resolution Numerical Simulator of In-Situ Combustion Processes', DE-FC26-03NT15405. In summary, this work improved our understanding of in-situ combustion (ISC) process physics and oil recovery. This understanding was translated into improved conceptual models and a suite of software algorithms that extended predictive capabilities. We pursued experimental, theoretical, and numerical tasks during the performance period. The specific project objectives were (i) identification, experimentally, of chemical additives/injectants that improve combustion performance and delineation of the physics of improved performance, (ii) establishment of a benchmark one-dimensional, experimental data set for verification of in-situ combustion dynamics computed by simulators, (iii) develop improved numerical methods that can be used to describe in-situ combustion more accurately, and (iv) to lay the underpinnings of a highly efficient, 3D, in-situ combustion simulator using adaptive mesh refinement techniques and parallelization. We believe that project goals were met and exceeded as discussed.

  19. Electronic excitation induced defect dynamics in HfO2 based MOS devices investigated by in-situ electrical measurements

    Science.gov (United States)

    Manikanthababu, N.; Vajandar, S.; Arun, N.; Pathak, A. P.; Asokan, K.; Osipowicz, T.; Basu, T.; Nageswara Rao, S. V. S.

    2018-03-01

    In-situ I-V and C-V characterization studies were carried out to determine the device quality of atomic layer deposited HfO2 (2.7 nm)/SiO2 (0.6 nm)/Si-based metal oxide semiconductor devices during 120 MeV Ag ion irradiation. The influence of various tunneling mechanisms has been investigated by analyzing the I-V characteristics as a function of ion fluence. The nature of the defects created is tentatively identified by the determination of the significant tunneling processes. While the ion induced annealing of defects is observed at lower fluences, ion induced intermixing and radiation damage is found to be significant at higher fluences. The C-V characteristics also reveal significant changes at the interface and oxide trap densities: an increase in the oxide layer thickness occurs through the formation of an HfSiO interlayer. The interlayer is due to the swift heavy ion induced intermixing, which has been confirmed by X-TEM and X-ray photoelectron spectroscopy measurements.

  20. ''In situ'' investigations of the radioactive fissionable element infiltration and retention in different soils

    International Nuclear Information System (INIS)

    Oncescu, M.; Danis, A.; Sahagia, M.; Negrescu, C.; Bobe, M.; Balanescu, P.; Burcescu, M.; Tautu, N.

    1980-01-01

    ''In situ'' investigations of the natural and forced infiltration and retention of the fissionable elements from a liquid residue in several natural compacted soils and compacted clays are presented. The velocities and flow rates for different stages of the residue infiltration are determined. The retention of the fissionable elements by variation of the fissionable element concentration with the distance from the place of the residue depot is investigated. (author)

  1. 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.

  2. In-situ investigation of the icosahedral Al-Cu-Fe phase formation in thin films

    Energy Technology Data Exchange (ETDEWEB)

    Haidara, F., E-mail: fanta.haidara@im2np.fr [IM2NP, UMR 6242 CNRS - Universite Aix-Marseille, Av. Escadrille Normandie-Niemen, Case 142, 13397 Marseille Cedex 20 (France); Duployer, B. [Universite Paul Sabatier CIRIMAT-LCMIE 2R1, 118, Route de Narbonne, 31062 Toulouse Cedex 09 (France); Mangelinck, D.; Record, M.-C. [IM2NP, UMR 6242 CNRS - Universite Aix-Marseille, Av. Escadrille Normandie-Niemen, Case 142, 13397 Marseille Cedex 20 (France)

    2012-09-05

    Highlights: Black-Right-Pointing-Pointer We investigated the phase formation of i-Al{sub 62.5}Cu{sub 25}Fe{sub 12.5} in thin films. Black-Right-Pointing-Pointer We characterized the samples by DSC and in-situ XRD and resistance measurements. Black-Right-Pointing-Pointer The resistivity value for i-Al{sub 62.5}Cu{sub 25}Fe{sub 12.5} was determined. - Abstract: This work is an investigation of the formation by reactive diffusion at high temperatures of the icosahedral phase, i-Al{sub 62.5}Cu{sub 25}Fe{sub 12.5}, in thin films. The samples were prepared by sputtering at room temperature. The elements Al, Cu and Fe were sequentially deposited onto oxidized silicon substrates. The two following stacking sequences, Al/Cu/Fe and Al/Fe/Cu, were investigated. The phase formation was studied using in situ resistivity, in situ X-ray Diffraction and Differential Scanning Calorimetry measurements. Whatever the stacking sequence, the sequences of phase formation evidenced during the heating treatment are similar. However the temperatures of formation for the first phases that are formed are different; they are higher in the case of the Al/Fe/Cu stacking sequence.

  3. Stereoscopic methods in TEM

    International Nuclear Information System (INIS)

    Thomas, L.E.

    1975-07-01

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

  4. In-situ investigation of laser surface modifications of WC-Co hard metals inside a scanning electron microscope

    Science.gov (United States)

    Mueller, H.; Wetzig, K.; Schultrich, B.; Pompe, Wolfgang; Chapliev, N. I.; Konov, Vitaly I.; Pimenov, S. M.; Prokhorov, Alexander M.

    1989-05-01

    The investigation of laser interaction with solid surfaces and of the resulting mechanism of surface modification are of technical interest to optimize technological processes, and they are also of fundamental scientific importance. Most instructive indormation is available with the ail of the in-situ techniques. For instance, measuring of the photon emission of the irradiated surface ane the plasma torch (if it is produced) simultaneously to laser action, makes it possible to gain a global characterization of the laser-solid interaction. In order to obtain additional information about surface and structure modifications in microscopic detail , a laser and scanning electron microscope were combined in to a tandem equipment (LASEM). Inside this eqiipment the microscopic observation is carried out directly at the laser irradiated area without any displacement of the sample. In this way, the stepwise development of surface modification during multipulse irradiation is visible in microscopic details and much more reliable information about the surface modification process is obtainable in comparison to an external laser irradiation. Such kind of equipments were realized simultaneously and independently in the Institut of General Physics (Moscow) and the Central Institute of Solid State Physics and Material Research (Dresden) using a CO2 and a LTd-glass-laser, respectively. In the following the advantages and possibilities of a LASEM shall be demonstrated by some selected investigations of WC-CO hardmeta. The results were obtained in collaboration by both groups with the aid of the pulsed CO2-laser. The TEA CO2 laser was transmitted through a ZnSe-window into the sample chamber of the SEM and focused ofAo tfte sample surface. It was operated in TEM - oo mode with a repetition rate of about 1 pulse per second. A peak power density of about 160 MW/cm2 was achieved in front of the sample surface.

  5. Structural Investigation of Sodium Layered Oxides Via in Situ Synchrotron X-Ray Diffraction

    DEFF Research Database (Denmark)

    Jung, Young Hwa; Christiansen, Ane Sælland; Johnsen, Rune

    2015-01-01

    electrochemical reaction is generally considered to be a pivotal feature for understanding the relationship between layered structures and electrochemical properties. Here the structure, phase stability, and electrochemical properties of two kinds of layered oxides, P2 and O3, are investigated through in......-situ synchrotron XRD experiments. A capillary Na-based cell is designed to minimize interference in other substances such as a separator or external battery parts. This approach could give us to obtain clear diffraction patterns with high intensity during electrochemical reaction in a short period of time without...... further relaxation step. We carefully scrutinized reversible structural phase transformations during electrochemical reaction of P2 and O3-layered compounds based on in situ analysis, and detailed results will be discussed....

  6. In situ tests for investigating thermal and mechanical rock behaviors at an underground research tunnel

    International Nuclear Information System (INIS)

    Kwon, Sangki; Cho, Won-Jin

    2013-01-01

    The understanding of the thermal and mechanical behaviors expected to be happened around an underground high-level radioactive waste (HLW) repository is important for a successful site selection, construction, operation, and closure of the repository. In this study, the thermal and mechanical behaviors of rock and rock mass were investigated from in situ borehole heater test and the studies for characterizing an excavation damaged zone (EDZ), which had been carried out at an underground research tunnel, KURT, constructed in granite for the validation of a HLW disposal concept. Thermal, mechanical, and hydraulic properties in EDZ could be predicted from various in situ and laboratory tests as well as numerical simulations. The complex thermo-mechanical coupling behavior of rock could be modeled using the rock properties. (author)

  7. XPS, TEM and SAD investigations of nanosized Co{sub x}B{sub y}H{sub z} particles obtained by two different borohydride methods

    Energy Technology Data Exchange (ETDEWEB)

    Krastev, V. [Bulgarian Acad. of Sci., Sofia (Bulgaria). Inst. of General and Inorg. Chem.; Stoycheva, M. [Central Laboratory of Electrochemical Power Sources, Bulgarian Academy of Sciences, Sofia 1113 (Bulgaria); Lefterova, E. [Central Laboratory of Electrochemical Power Sources, Bulgarian Academy of Sciences, Sofia 1113 (Bulgaria); Dragieva, I. [Central Laboratory of Electrochemical Power Sources, Bulgarian Academy of Sciences, Sofia 1113 (Bulgaria); Stoynov, Z. [Central Laboratory of Electrochemical Power Sources, Bulgarian Academy of Sciences, Sofia 1113 (Bulgaria)

    1996-07-01

    The nanosized Co{sub x}B{sub y}H{sub z} particles synthesised by the ``tea`` and ``antigravity`` methods using a borohydride reduction process have been subjected to structure and composition studies by X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM) and selected area diffraction (SAD). The amounts of the elements Co, B, O{sub 2}, H{sub 2} and C as mean volume values, and surface values for the as-prepared particles, as well as after Ar{sup +} etching to a depth of about 15 nm and 30 nm from the initial particle surface, are determined. About 1.5 atoms of cobalt per atom of boron correspond to samples obtained by the ``antigravity`` method. The binding energy (BE) of 1s electrons of boron atoms has only one value. These particles are angular and are in the typical nanocrystalline state. In the case of samples prepared by the ``tea`` method, two atoms of cobalt per atom of boron are found. The presence of two kinds of BE (B{sup I} and B{sup II}) of 1s electrons of boron atoms in the particles obtained by the ``tea`` method is observed and almost equal amounts of these two states are established in the spectrum. The particles` shape and structure are typical of the amorphous state. The fact that there is one peak when the ``antigravity`` method is applied, in contrast to the two peaks with the ``tea`` method indicates the presence of a metal amorphous state in the latter case. (orig.)

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

    International Nuclear Information System (INIS)

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

    2004-01-01

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

  9. Investigation on the Vibration Effect of Shock Wave in Rock Burst by In Situ Microseismic Monitoring

    Directory of Open Access Journals (Sweden)

    Mingshi Gao

    2018-01-01

    Full Text Available Rock burst is a physical explosion associated with enormous damage at a short time. Due to the complicity of mechanics of rock burst in coal mine roadway, the direct use of traditional investigation method applied in tunnel is inappropriate since the components of surrounding rock are much more complex in underground than that of tunnel. In addition, the reliability of the results obtained through these methods (i.e., physical simulation, theoretical analysis, and monitoring in filed application is still not certain with complex geological conditions. Against this background, present experimental study was first ever conducted at initial site to evaluate the effect of shock wave during the rock burst. TDS-6 microseismic monitoring system was set up in situ to evaluate the propagation of shock wave resulting in microexplosions of roadway surrounding rock. Various parameters including the distance of epicentre and the characteristic of response have been investigated. Detailed test results revealed that (1 the shock wave attenuated exponentially with the increase of the distance to seismic source according to the equation of E=E0e-ηl; particularly, the amplitude decreased significantly after being 20 m apart from explosive resource and then became very weak after being 30 m apart from the seismic source; (2 the response mechanics are characteristic with large scatter based on the real location of surrounding rock despite being at the same section. That is, the surrounding rock of floor experienced serious damage, followed by ribs, the roof, and the humeral angles. This in situ experimental study also demonstrated that microseismic monitoring system can be effectively used in rock burst through careful setup and data investigation. The proposed in situ monitoring method has provided a new way to predict rock burst due to its simple instalment procedure associated with direct and reasonable experimental results.

  10. In Situ Techniques for the Investigation of the Kinetics of Austenitization of Supermartensitic Stainless Steel

    DEFF Research Database (Denmark)

    Nießen, Frank; Villa, Matteo; Apel, Daniel

    2016-01-01

    The austenitization and inter-critical annealing of X4CrNiMo16-5-1 (1.4418) supermartensitic stainless steel were investigated in-situ with synchrotron X-ray diffraction (XRD), dilatometry and differential scanning calorimetry (DSC) under isochronal heating conditions. Austenitization occurred...... of surface martensite formation on the XRD measurement. The applicable temperature range for DSC as well as the close proximity of the Ac1- and the Curietemperature limited the usage of the technique in the present case....

  11. Multiphoton microscopy for the in-situ investigation of cellular processes and integrity in cryopreservation.

    Science.gov (United States)

    Doerr, Daniel; Stark, Martin; Ehrhart, Friederike; Zimmermann, Heiko; Stracke, Frank

    2009-08-01

    In this study we demonstrate a new noninvasive imaging method to monitor freezing processes in biological samples and to investigate life in the frozen state. It combines a laser scanning microscope with a computer-controlled cryostage. Nearinfrared (NIR) femtosecond laser pulses evoke the fluorescence of endogenous fluorophores and fluorescent labels due to multiphoton absorption.The inherent optical nonlinearity of multiphoton absorption allows 3D fluorescence imaging for optical tomography of frozen biological material in-situ. As an example for functional imaging we use fluorescence lifetime imaging (FLIM) to create images with chemical and physical contrast.

  12. Prion structure investigated in situ, ex vivo, and in vitro by FTIR spectroscopy

    Science.gov (United States)

    Kneipp, Janina; Miller, Lisa M.; Spassov, Sashko; Sokolowski, Fabian; Lasch, Peter; Beekes, Michael; Naumann, Dieter

    2004-07-01

    Syrian hamster nervous tissue was investigated by FTIR microspectroscopy with conventional and synchrotron infrared light sources. Various tissue structures from the cerebellum and medulla oblongata of scrapie-infected and control hamsters were investigated at a spatial resolution of 50 μm. Single neurons in dorsal root ganglia of scrapie-infected hamsters were analyzed by raster scan mapping at 6 μm spatial resolution. These measurements enabled us to (i) scrutinize structural differences between infected and non-infected tissue and (ii) analyze for the first time the distribution of different protein structures in situ within single nerve cells. Single nerve cells exhibited areas of increased β-sheet content, which co-localized consistently with accumulations of the pathological prion protein (PrPSc). Spectral data were also obtained from purified, partly proteinase K digested PrPSc isolated from scrapie-infected nervous tissue of hamsters to elucidate similarities/dissimilarities between prion structure in situ and ex vivo. A further comparison is drawn to the recombinant Syrian hamster prion protein SHaPrP90-232, whose in vitro transition from the predominantly a-helical isoform to β-sheet rich oligomeric structures was also investigated by FTIR spectroscopy.

  13. 3-D Magnetotelluric Investigations for geothermal exploration in Martinique (Lesser Antilles). Characteristic Deep Resistivity Structures, and Shallow Resistivity Distribution Matching Heliborne TEM Results

    OpenAIRE

    Coppo , Nicolas; Baltassat , Jean-Michel; Girard , Jean-François; Wawrzyniak , Pierre; Hautot , Sophie; Tarits , Pascal; Jacob , Thomas; Martelet , Guillaume; Mathieu , Francis; Gadalia , Alain; Bouchot , Vincent; Traineau , Hervé

    2015-01-01

    International audience; Within the framework of a global French program oriented towards the development of renewable energies, Martinique Island (Lesser Antilles, France) has been extensively investigated (from 2012 to 2013) through an integrated multi-methods approach, with the aim to define precisely the potential geothermal ressources, previously highlighted (Sanjuan et al., 2003). Amongst the common investigation methods deployed, we carried out three magnetotelluric (MT) surveys located...

  14. Plans for Selection and In-Situ Investigation of Return Samples by the Supercam Instrument Onboard the Mars 2020 Rover

    Science.gov (United States)

    Wiens, R. C.; Maurice, S.; Mangold, N.; Anderson, R.; Beyssac, O.; Bonal, L.; Clegg, S.; Cousin, A.; DeFlores, L.; Dromart, G.; Fisher, W.; Forni, O.; Fouchet, T.; Gasnault, O.; Grotzinger, J.; Johnson, J.; Martinez-Frias, J.; McLennan, S.; Meslin, P.-Y.; Montmessin, F.; Poulet, F.; Rull, F.; Sharma, S.

    2018-04-01

    The SuperCam instrument onboard Rover 2020 still provides a complementary set of analyses with IR reflectance and Raman spectroscopy for mineralogy, LIBS for chemistry, and a color imager in order to investigate in-situ samples to return.

  15. MetNet - In situ observational Network and Orbital platform to investigate the Martian environment

    Science.gov (United States)

    Harri, Ari-Matti; Leinonen, Jussi; Merikallio, Sini; Paton, Mark; Haukka, Harri; Polkko, Jouni

    2007-09-01

    MetNet Mars Mission is an in situ observational network and orbital platform mission to investigate the Martian environment and it has been proposed to European Space Agency in response to Call for proposals for the first planning cycle of Cosmic Vision 2015-2025 D/SCI/DJS/SV/val/21851. The MetNet Mars Mission is to be implemented in collaboration with ESA, FMI, LA, IKI and the payload providing science teams. The scope of the MetNet Mission is to deploy 16 MetNet Landers (MNLs) on the Martian surface by using inflatable descent system structures accompanied by an atmospheric sounder and data relay onboard the MetNet Orbiter (MNO), which is based on ESA Mars Express satellite platform. The MNLs are attached on the three sides of the satellite and most of the MNLs are deployed to Mars separately a few weeks prior to the arrival to Mars. The MetNet Orbiter will perform continuous atmospheric soundings thus complementing the accurate in situ observations at the Martian ground produced by the MetNet observation network, as well as the orbiter will serve as the primary data relay between the MetNet Landers and the Earth. The MNLs are equipped with a versatile science payload focused on the atmospheric science of Mars. Detailed characterisation of the Martian atmospheric circulation patterns, boundary layer phenomena, and climatological cycles, as well as interior investigations, require simultaneous in situ meteorological, seismic and magnetic measurements from networks of stations on the Martian surface. MetNet Mars Mission will also provide a crucial support for the safety of large landing missions in general and manned Mars missions in particular. Accurate knowledge of atmospheric conditions and weather data is essential to guarantee safe landings of the forthcoming Mars mission elements.

  16. In-situ investigation of hydrogen evolution behavior in vanadium redox flow batteries

    International Nuclear Information System (INIS)

    Wei, L.; Zhao, T.S.; Xu, Q.; Zhou, X.L.; Zhang, Z.H.

    2017-01-01

    Highlights: • An in-situ method to investigate hydrogen evolution in VRFBs is developed. • The rate of hydrogen evolution during battery operation is quantified. • The gas evolution behaviors in the charge process of VRFBs are observed. - Abstract: In this work, we conceived and fabricated a three-electrode electrochemical cell and transparent vanadium redox flow battery to in-situ investigate the hydrogen evolution reaction during battery operation. Experimental results show that operating temperature has a strong influence on the HER rate. In particular, compared with V"3"+ reduction reaction, HER is more sensitive to temperature variation. It is also found that, contrary to the conventional wisdom that side reactions occur at the late stage of the charge process, H_2 evolves at a relatively low SOC. About 0.26 and 1.94 mL H_2 were collected at an early (SOC lower than 20%) and end of the charge process, respectively, suggesting that attention to the hydrogen formation at the negative electrode in the early charge process should also be paid to during long-term battery operations. Moreover, the produced hydrogen gas at the negative side prefers to form macroscopically observable bubbles onto the electrode surface, covering the active sites for vanadium redox reactions, while oxygen evolution (including CO_2 production) at the positive side corrodes electrode surface and introduces certain oxygen-containing functional groups.

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

    International Nuclear Information System (INIS)

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

    2015-01-01

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

  18. 2D BiOCl/Bi12O17Cl2 nanojunction: Enhanced visible light photocatalytic NO removal and in situ DRIFTS investigation

    Science.gov (United States)

    Zhang, Wendong; Dong, Xin'an; Jia, Bin; Zhong, Junbo; Sun, Yanjuan; Dong, Fan

    2018-02-01

    Novel two-dimensional (2D) BiOCl/Bi12O17Cl2 nanojunctions were fabricated by a facile one-pot in situ method at room temperature. The as-prepared samples were analyzed by XRD, SEM, TEM, HRTEM, UV-vis DRS, PL, ESR and BET-BJH measurement in detail. The photocatalytic performance of the samples was evaluated by removal of NO at ppb level under visible-light illumination. The result reveals that the BiOCl/Bi12O17Cl2 nanojunctions manifests conspicuously enhanced photocatalytic efficiency for NO removal. The facilitated performance can be ascribed to the well-matched band structure and relatively high specific surface area. In addition, the in situ diffuse reflectance infrared Fourier transform spectroscopy was applied to investigate the adsorption and photocatalytic NO oxidation processes. The reaction mechanism of photocatalytic NO oxidation was proposed based on the observed intermediates. The present work could pave a way to synthesize novel visible light photocatalysts at room temperature for environmental application.

  19. In-situ investigation of protein and DNA structure using UVRRS

    Science.gov (United States)

    Greek, L. Shane; Schulze, H. Georg; Blades, Michael W.; Haynes, Charles A.; Turner, Robin F. B.

    1997-05-01

    Ultraviolet resonance Raman spectroscopy (UVRRS) has the potential to become a sensitive, specific, versatile bioanalytical and biophysical technique for routine investigations of proteins, DNA, and their monomeric components, as well as a variety smaller, physiologically important aromatic molecules. The transition of UVRRS from a complex, specialized spectroscopic method to a common laboratory assay depends upon several developments, including a robust sample introduction method permitting routine, in situ analysis in standard laboratory environments. To this end, we recently reported the first fiber-optic probes suitable for deep-UV pulsed laser UVRRS. In this paper, we extend this work by demonstrating the applicability of such probes to studies of biochemical relevance, including investigations of the resonance enhancement of phosphotyrosine, thermal denaturation of RNase T1, and specific and non-specific protein binding. The advantages and disadvantages of the probes are discussed with reference to sample conditions and probe design considerations.

  20. The ultrasonic technique for in situ investigations on stones: suggestions for uses

    Science.gov (United States)

    Bellopede, R.; Marini, P.

    2012-04-01

    The Ultrasound Pulse Velocity (UPV) is one of the main non destructive techniques to detect both in laboratory and in situ the stone decay and many international papers of the recent years deal with its application. This technique is often executed in laboratory, where the possibility to keep constant the environmental and test conditions are a guarantee of the reliability of the results. It is known in fact the UPV are mainly conditioned by the following factors: - the characteristics of the stone tested (not only petrographic properties such as texture and structure, but even specimen dimension and water content); - the transducers features such as frequency, divergence angle , near field and wavelength; - external climate factors such as environmental temperature, humidity. In spite of the many factors affecting the measurements, UPV performed in laboratory is well correlated with mechanical strength of the stone , with its porosity and, as consequence, it is a reliable technique to detect the durability of a stone. On the other side, for in situ UPV test it is important to take into account that the measurement uncertainty is affected by the unknown water content in the stone. From tests performed on different rocks (marble, limestones, travertines, granites, gneiss, schists , sandstones) , the ratios between UPV tested in dry and saturated conditions can be > 1 or stone in order to choose the suitable measurement frequency; the correct choice of transducers frequencies; the use of a reference slab, with a known UPV in dry conditions, to be exposed in the investigated site some days before the in situ tests, in order to appreciate the UPV variation due to climate factors.

  1. Investigation of Ion-Solvent Interactions in Nonaqueous Electrolytes Using in Situ Liquid SIMS

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Yanyan; Su, Mao; Yu, Xiaofei; Zhou, Yufan; Wang, Jungang; Cao, Ruiguo; Xu, Wu; Wang, Chongmin; Baer, Donald R.; Borodin, Oleg; Xu, Kang; Wang, Yanting; Wang, Xue-Lin; Xu, Zhijie; Wang, Fuyi; Zhu, Zihua

    2018-02-06

    Ion-solvent interactions in non-aqueous electrolytes are of fundamental interest and practical importance, yet debates regarding ion preferential solvation and coordination numbers persist. In this work, in situ liquid SIMS was used to examine ion-solvent interactions in three representative electrolytes, i.e., lithium hexafluorophosphate (LiPF6) at 1.0 M in ethylene carbonate (EC)-dimethyl carbonate (DMC), and lithium bis(fluorosulfonyl)imide (LiFSI) at both low (1.0 M) and high (4.0 M) concentrations in 1,2-dimethoxyethane (DME). In the positive ion mode, solid molecular evidence strongly supports the preferential solvation of Li+ by EC. Besides, from the negative spectra, we also found that PF6- forms association with EC, which has been neglected by previous studies due to the relatively weak interaction. While in both LiFSI in DME electrolytes, no evidence shows that FSI- is associated with DME. Furthermore, strong salt ion cluster signals were observed in the 1.0 M LiPF6 in EC-DMC electrolyte, suggesting that a significant amount of Li+ ions stay in vicinity of anions. In sharp comparison, weak ion cluster signals were detected in dilute LiFSI in DME electrolyte, suggesting most ions are well separated, in agreement with our molecular dynamics (MD) simulation results. These findings indicate that with virtues of little bias on detecting positive and negative ions and the capability of directly analyzing concentrated electrolytes, in situ liquid SIMS is a powerful tool that can provide key evidence for improved understanding on the ion-solvent interactions in non-aqueous electrolytes. Therefore, we anticipate wide applications of in situ liquid SIMS on investigations of various ion-solvent interactions in the near future.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2017-02-15

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

  3. Solar System Exploration Augmented by In-Situ Resource Utilization: Mercury and Saturn Propulsion Investigations

    Science.gov (United States)

    Palaszewski, Bryan

    2016-01-01

    Human and robotic missions to Mercury and Saturn are presented and analyzed with a range of propulsion options. Historical studies of space exploration, in-situ resource utilization (ISRU), and industrialization all point to the vastness of natural resources in the solar system. Advanced propulsion benefitted from these resources in many ways. While advanced propulsion systems were proposed in these historical studies, further investigation of nuclear options using high power nuclear thermal and nuclear pulse propulsion as well as advanced chemical propulsion can significantly enhance these scenarios. Updated analyses based on these historical visions will be presented. Nuclear thermal propulsion and ISRU enhanced chemical propulsion landers are assessed for Mercury missions. At Saturn, nuclear pulse propulsion with alternate propellant feed systems and Titan exploration with chemical propulsion options are discussed. In-situ resource utilization was found to be critical in making Mercury missions more amenable for human visits. At Saturn, refueling using local atmospheric mining was found to be difficult to impractical, while refueling the Saturn missions from Uranus was more practical and less complex.

  4. An in situ FTIR step-scan photoacoustic investigation of kerogen and minerals in oil shale.

    Science.gov (United States)

    Alstadt, Kristin N; Katti, Dinesh R; Katti, Kalpana S

    2012-04-01

    Step-scan photoacoustic infrared spectroscopy experiments were performed on Green River oil shale samples obtained from the Piceance Basin located in Colorado, USA. We have investigated the molecular nature of light and dark colored areas of the oil shale core using FTIR photoacoustic step-scan spectroscopy. This technique provided us with the means to analyze the oil shale in its original in situ form with the kerogen-mineral interactions intact. All vibrational bands characteristic of kerogen were found in the dark and light colored oil shale samples confirming that kerogen is present throughout the depth of the core. Depth profiling experiments indicated that there are changes between layers in the oil shale molecular structure at a length scale of micron. Comparisons of spectra from the light and dark colored oil shale core samples suggest that the light colored regions have high kerogen content, with spectra similar to that from isolated kerogen, whereas, the dark colored areas contain more mineral components which include clay minerals, dolomite, calcite, and pyrite. The mineral components of the oil shale are important in understanding how the kerogen is "trapped" in the oil shale. Comparing in situ kerogen spectra with spectra from isolated kerogen indicate significant band shifts suggesting important nonbonded molecular interactions between the kerogen and minerals. Copyright © 2011 Elsevier B.V. All rights reserved.

  5. Mechanical Conversion for High-Throughput TEM Sample Preparation

    International Nuclear Information System (INIS)

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

    2006-01-01

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

  6. Investigation on microstructural characterization of in situ TiB/Al metal matrix composite by laser cladding

    International Nuclear Information System (INIS)

    Xu Jiang; Li Zhengyang; Zhu Wenhui; Liu Zili; Liu Wenjin

    2007-01-01

    The aluminum matrix composite (AMC) coating reinforced with TiB was prepared utilizing in situ synthesized technique by laser cladding. Microstructural characterization and dry sliding wear behavior of in situ TiB/Al metal matrix composite were studied by SEM, XRD, TEM and Pin-on-disc friction and wear tester. The phase structure of the composite coating consists of α-Al, TiB, Al 3 Ti and Al 3 Fe. It has been found that the shape of in situ synthesized TiB is mainly taken on micro-magnitude lump and nano-magnitude whisker. Owing to B27 structure of TiB, the TiB has an anisotropy axis of growth, which results in the TiB strip and whisker preferring grown along [0 1 0] direction. It is worth to notice that the novel microstructure inside of TiB is particle and strip Al 5 Fe 2 phase and definite crystallographic relationship between the Al 5 Fe 2 phase and TiB has been determined by selected area diffraction pattern. The wear tests results show that the composite coatings can only improve wear resistance at the lower applied load (below 26.7 N), but at higher applied load (26.7-35.6 N) the wear resistance behavior of the coating is worsened due to the fracture and pullout of reinforcement phase

  7. Investigation on microstructural characterization of in situ TiB/Al metal matrix composite by laser cladding

    Energy Technology Data Exchange (ETDEWEB)

    Xu Jiang [Department of Material Science and Engineering, Nanjing University of Aeronautics and Astronautics, 29 Yudao Street, Nanjing 210016 (China)]. E-mail: xujiang73@nuaa.edu.cn; Li Zhengyang [Key Laboratory for Advanced Materials Manufacturing Processing, Mechanical Engineering Department, Tsinghua University, Beijing 10084 (China); Zhu Wenhui [Department of Material Science and Engineering, Nanjing University of Aeronautics and Astronautics, 29 Yudao Street, Nanjing 210016 (China); Liu Zili [Department of Material Science and Engineering, Nanjing University of Aeronautics and Astronautics, 29 Yudao Street, Nanjing 210016 (China); Liu Wenjin [Key Laboratory for Advanced Materials Manufacturing Processing, Mechanical Engineering Department, Tsinghua University, Beijing 10084 (China)

    2007-02-25

    The aluminum matrix composite (AMC) coating reinforced with TiB was prepared utilizing in situ synthesized technique by laser cladding. Microstructural characterization and dry sliding wear behavior of in situ TiB/Al metal matrix composite were studied by SEM, XRD, TEM and Pin-on-disc friction and wear tester. The phase structure of the composite coating consists of {alpha}-Al, TiB, Al{sub 3}Ti and Al{sub 3}Fe. It has been found that the shape of in situ synthesized TiB is mainly taken on micro-magnitude lump and nano-magnitude whisker. Owing to B27 structure of TiB, the TiB has an anisotropy axis of growth, which results in the TiB strip and whisker preferring grown along [0 1 0] direction. It is worth to notice that the novel microstructure inside of TiB is particle and strip Al{sub 5}Fe{sub 2} phase and definite crystallographic relationship between the Al{sub 5}Fe{sub 2} phase and TiB has been determined by selected area diffraction pattern. The wear tests results show that the composite coatings can only improve wear resistance at the lower applied load (below 26.7 N), but at higher applied load (26.7-35.6 N) the wear resistance behavior of the coating is worsened due to the fracture and pullout of reinforcement phase.

  8. Novel sample preparation for operando TEM of catalysts

    International Nuclear Information System (INIS)

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

    2015-01-01

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

  9. Fabrication and in-situ STM investigation of growth dynamics of semiconductor nanostructures grown by MBE

    International Nuclear Information System (INIS)

    Borisova, Svetlana

    2012-01-01

    Modern development of information technologies requires an introduction of new fundamental concepts, in order to create more efficient devices and to decrease their size. One of the most promising ways is to increase the functionality of silicon by integrating novel materials into Si-based production. This PhD thesis reports on the fabrication and investigation of the growth of semiconductor nanostructures on Si substrates by molecular beam epitaxy (MBE). In-situ scanning tunneling microscopy (STM) is a powerful technique in order to study morphological and electronic properties of the grown structures directly under ultra high vacuum (UHV) conditions. It is shown that the combination of MBE and in-situ STM enables the study of nucleation and growth dynamics at the atomic scale. It provides us with numerous information concerning the nucleation mechanism, the growth mode of the structures, adatom kinetics, influence of the lattice mismatch between the substrate and the grown structure as well as formation and morphology of crystal defects. The first part of the thesis focuses on the experimental realization based upon an existing setup. The construction of an in-situ UHV STM compatible with the MBE cluster and the technical improvement of the STM setup are described. Subsequently, test measurements are performed on the technologically most important surfaces, Ge (100) and Si (111). The second part of the thesis is dedicated to ordered small-period arrays of self-assembled Ge quantum dots (QDs) grown on pre-patterned Si (100) substrates. Small-period Ge QD crystals are highly interesting since band structure calculations indicate coupled electronic states of the QDs in the case of the small lateral period of approximately 30 nm. Small-period hole patterns with a period of 56 nm are fabricated by e-beam lithography on Si substrates. The evolution of the hole morphology during the in-situ pre-growth annealing and the Si buffer layer growth are studied. Deposition of 5

  10. Fabrication and in-situ STM investigation of growth dynamics of semiconductor nanostructures grown by MBE

    Energy Technology Data Exchange (ETDEWEB)

    Borisova, Svetlana

    2012-05-23

    Modern development of information technologies requires an introduction of new fundamental concepts, in order to create more efficient devices and to decrease their size. One of the most promising ways is to increase the functionality of silicon by integrating novel materials into Si-based production. This PhD thesis reports on the fabrication and investigation of the growth of semiconductor nanostructures on Si substrates by molecular beam epitaxy (MBE). In-situ scanning tunneling microscopy (STM) is a powerful technique in order to study morphological and electronic properties of the grown structures directly under ultra high vacuum (UHV) conditions. It is shown that the combination of MBE and in-situ STM enables the study of nucleation and growth dynamics at the atomic scale. It provides us with numerous information concerning the nucleation mechanism, the growth mode of the structures, adatom kinetics, influence of the lattice mismatch between the substrate and the grown structure as well as formation and morphology of crystal defects. The first part of the thesis focuses on the experimental realization based upon an existing setup. The construction of an in-situ UHV STM compatible with the MBE cluster and the technical improvement of the STM setup are described. Subsequently, test measurements are performed on the technologically most important surfaces, Ge (100) and Si (111). The second part of the thesis is dedicated to ordered small-period arrays of self-assembled Ge quantum dots (QDs) grown on pre-patterned Si (100) substrates. Small-period Ge QD crystals are highly interesting since band structure calculations indicate coupled electronic states of the QDs in the case of the small lateral period of approximately 30 nm. Small-period hole patterns with a period of 56 nm are fabricated by e-beam lithography on Si substrates. The evolution of the hole morphology during the in-situ pre-growth annealing and the Si buffer layer growth are studied. Deposition of 5

  11. Identification of the silver state in the framework of Ag-containing zeolite by XRD, FTIR, photoluminescence, 109Ag NMR, EPR, DR UV-vis, TEM and XPS investigations.

    Science.gov (United States)

    Popovych, Nataliia; Kyriienko, Pavlo; Soloviev, Sergiy; Baran, Rafal; Millot, Yannick; Dzwigaj, Stanislaw

    2016-10-26

    Silver has been identified in the framework of Ag x SiBEA zeolites (where x = 3-6 Ag wt%) by the combined use of XRD, 109 Ag MAS NMR, FTIR, diffuse reflectance UV-visible, EPR and XPS spectroscopy. The incorporation of Ag ions into the framework of SiBEA zeolite has been evidenced by XRD. The consumption of OH groups as a result of their reaction with the silver precursor has been monitored by FTIR and photoluminescence spectroscopy. The changes in the silver state as a function of Ag content and thermal and hydrogen treatment at 573 K have been identified by 109 Ag MAS NMR, EPR, DR UV-visible, TEM and XPS investigations. The acidity of AgSiBEA has been investigated by FTIR spectroscopy of adsorbed CO and pyridine used as probe molecules.

  12. In-situ investigation of the microstructure evolution in nanocrystalline copper electrodeposits at room temperature

    DEFF Research Database (Denmark)

    Pantleon, Karen; Somers, Marcel A. J.

    2006-01-01

    The microstructure evolution in copper electrodeposits at room temperature (self-annealing) was investigated by means of x-ray diffraction analysis and simultaneous measurements of the electrical resistivity as a function of time. In situ studies were started immediately after deposition...... growth, crystallographic texture changes by multiple twinning, and a decrease of the electrical resistivity occurred as a function of time at room temperature. The kinetics of self-annealing is strongly affected by the layer thickness: the thinner the layer, the slower the microstructure evolution is......, and self-annealing is suppressed completely for a thin layer with 0.4 µm. The preferred crystallographic orientation of the as-deposited crystallites is suggested to cause the observed thickness dependence of the self-annealing kinetics. ©2006 American Institute of Physics...

  13. Development of In situ Geological Investigation and Test Equipment in KURT

    Energy Technology Data Exchange (ETDEWEB)

    Koh, Yong Kweon; Kim, Kyung Su; Park, Kyung Woo; Koh, Yong Kweon; Choi, Jong Won [KAERI, Daejeon (Korea, Republic of)

    2010-12-15

    For establishment of the advanced infrastructures of KURT, geological investigation and in situ test equipment were installed. The optical sensor technique could be applicable to monitoring system for the safe operation of various kinds of facilities having static and/or dynamic characteristics, such as chemical plant, pipeline, rail, huge building, long and slim structures, bridge, subway and marine vessel. etc. The micro-seismic monitoring system is able to predict the location and timing of fracturing of rock mass and rock fall around an underground openings as well as analysis on safety of various kinds of engineering structures such as nuclear facilities and other structures. The straddle packer system for hydro-testing in a deep borehole will lead to not only improve current technical level in the field of hydraulic testing but also provide important information to radioactive waste disposal technology development and site characterization project

  14. In-situ investigations of surface modifications by swift heavy ions

    International Nuclear Information System (INIS)

    Bolse, W.; Sankarakumar, A.; Ferhati, R.; Garmatter, D.; Haag, M.; Dautel, K.; Asdi, M.; Srivastava, N.; Widmann, B.; Bauer, M.

    2014-01-01

    We are running a High Resolution Scanning Electron Microscope in the beam line of the UNILAC ion accelerator at the GSI Helmholtz Centre for Heavy Ion Research in Danustadt, Germany, which has recently been extended also with an EDX-system and two micro-manipulators. This instrument allows us to in-situ investigate the structural and compositional development of individual objects and structures in the μm- and nm-range under swift heavy ion bombardment, from the very first ion impact up to high fluences of the order of several 10 15 /cm 2 . The sample under investigation is irradiated in small fluence steps and in between SEM-images (and EDX-scans) of one and the same surface area are taken. The irradiation can be carried out at any incidence angle between 0° and 90° and also under stepwise or continuous azimuthal rotation of the sample. The micro-manipulator system allows us to perform additional analysis like electrical and mechanical characterization as well as substrate-free EDX at sub-μm objects. We are now also able to irradiate almost free standing sub-μm structures (pasted on a nanoscale tip or held in micro-tweezers). In this report an overview over this unique instrument and its capabilities and advantages will be given, illustrated by the results of our recent in-situ studies on ion induced modification of thin films (dewetting and self-organisation) and on shaping of sub-μm objects with swift heavy ions (by taking advantage of ion sputtering, ion hammering and ion induced visco-elastic flow). (author)

  15. 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

  16. 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.

  17. 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.

  18. In situ investigation of SnAgCu solder alloy microstructure

    International Nuclear Information System (INIS)

    Pietrikova, Alena; Bednarcik, Jozef; Durisin, Juraj

    2011-01-01

    Research highlights: → In situ X-ray diffraction investigation enabled detailed analysis of the melting and solidification process of the SAC305 alloy. → It was found that the SAC305 solder melts at 230 deg. C. When cooling from 240 deg. C the SAC305 alloy solidifies at the temperature of 214 deg. C. During solidification β-Sn and Cu 6 Sn 5 is also formed. Formation of Ag 3 Sn occurs at 206 deg. C and the remaining amount of alloy crystallizes approximately at 160 deg. C. → Furthermore, observation of the thermal expansion behaviour of the β-Sn tetragonal unit cell revealed linear dependence of the unit cell volume on temperature. The unit cell parameters a and c also increase linearly with the temperature. Despite the fact that the c parameter is substantially smaller than parameter a, it exhibits a significantly higher linear thermal expansion coefficient. Comparison between data obtained during heating and cooling indicates that the thermal expansion coefficient is slightly greater in the case of cooling. - Abstract: In situ X-ray diffraction experiments, using synchrotron radiation, were employed to analyze microstructure evolution of the 96.5Sn3Ag0.5Cu (wt.%)-SAC305 lead-free solder alloy during heating (30-240 deg. C), isothermal dwell (240 deg. C) and cooling (240-30 deg. C). The special emphasis was placed on the study of the melting and solidification processes, explaining formation, distribution and the order of crystallization of the crystal phases (β-Sn, intermetallic compounds) in the solder alloy. Furthermore, thermal expansion behaviour of the main constituent phase β-Sn was analyzed prior to melting and after the consequent solidification.

  19. In Situ Investigation of the Iron Carbide Precipitation Process in a Fe-C-Mn-Si Q&P Steel

    Directory of Open Access Journals (Sweden)

    Sébastien Y. P. Allain

    2018-06-01

    Full Text Available Quenching and Partitioning (Q&P steels are promising candidates for automotive applications because of their lightweight potential. Their properties depend on carbon enrichment in austenite which, in turn, is strongly influenced by carbide precipitation in martensite during quenching and partitioning treatment. In this paper, by coupling in situ High Energy X-Ray Diffraction (HEXRD experiments and Transmission Electron Microscopy (TEM, we give some clarification regarding the precipitation process of iron carbides in martensite throughout the Q&P process. For the first time, precipitation kinetics was followed in real time. It was shown that precipitation starts during the reheating sequence for the steel studied. Surprisingly, the precipitated fraction remains stable all along the partitioning step at 400 °C. Furthermore, the analyses enable the conclusion that the iron carbides are most probably eta carbides. The presence of cementite was ruled out, while the presence of several epsilon carbides cannot be strictly excluded.

  20. New insights into the toxicity of mineral fibres: A combined in situ synchrotron μ-XRD and HR-TEM study of chrysotile, crocidolite, and erionite fibres found in the tissues of Sprague-Dawley rats.

    Science.gov (United States)

    Gualtieri, Alessandro F; Bursi Gandolfi, Nicola; Pollastri, Simone; Burghammer, Manfred; Tibaldi, Eva; Belpoggi, Fiorella; Pollok, Kilian; Langenhorst, Falko; Vigliaturo, Ruggero; Dražić, Goran

    2017-05-15

    Along the line of the recent research topic aimed at understanding the in vivo activity of mineral fibres and their mechanisms of toxicity, this work describes the morpho-chemical characteristics of the mineral fibres found in the tissues of Sprague-Dawley rats subjected to intraperitoneal/intrapleural injection of UICC chrysotile, UICC crocidolite and erionite-Na from Nevada (USA). The fibres are studied with in situ synchrotron powder diffraction and high resolution transmission electron microscopy to improve our understanding of the mechanisms of toxicity of these mineral fibres. In contact with the tissues of the rats, chrysotile fibres are prone to dissolve, with leaching of Mg and production of a silica rich relict. On the other hand, crocidolite and erionite-Na fibres are stable even for very long contact times within the tissues of the rats, showing just a thin dissolution amorphous halo. These findings support the model of a lower biopersistence of chrysotile with respect to crocidolite and erionite-Na but the formation of a silica-rich fibrous residue after the pseudo-amorphization of chrysotile may justify a higher cytotoxic potential and intense inflammatory activity of chrysotile in the short term in contact with the lung tissues. Copyright © 2017 Elsevier B.V. All rights reserved.

  1. New approaches investigating production rates of in-situ produced terrestrial cosmogenic nuclides

    Energy Technology Data Exchange (ETDEWEB)

    Merchel, Silke [CEREGE, CNRS-IRD-Universite Aix-Marseille, Aix-en-Provence (France); FZD, Dresden (Germany); Braucher, Regis; Benedetti, Lucilla; Bourles, Didier [CEREGE, CNRS-IRD-Universite Aix-Marseille, Aix-en-Provence (France)

    2010-07-01

    In-situ produced cosmogenic nuclides have proved to be valuable tools for environmental and Earth sciences. However, accurate application of this method is only possible, if terrestrial production rates in a certain environment over a certain time period and their depth-dependence within the exposed material are exactly known. Unfortunately, the existing data and models differ up to several tens of percent. Thus, one of the European project CRONUS-EU goals is the high quality calibration of the {sup 36}Cl production rate by spallation at independently dated surfaces. As part of fulfilling this task we have investigated calcite-rich samples from four medieval landslide areas in the Alps: Mont Granier, Le Claps, Dobratsch, and Veliki Vrh (330-1620 m, 1248-1442 AD). For investigating the depth-dependence of the different nuclear reactions, especially, the muon- and thermal neutron-induced contributions, we have analysed mixtures of carbonates and siliceous conglomerate samples - for {sup 10}Be, {sup 26}Al, and {sup 36}Cl - exposed at different shielding depths and taken from a core drilled in 2005 at La Ciotat, France (from surface to 11 m shielding). AMS of {sup 36}Cl was performed at LLNL and ETH, {sup 10}Be and {sup 26}Al at ASTER.

  2. In-situ structural investigations of ferroelasticity in soft and hard rhombohedral and tetragonal PZT

    Energy Technology Data Exchange (ETDEWEB)

    Morozov, Maxim I., E-mail: maximm@alumni.ntnu.no; Einarsrud, Mari-Ann; Tolchard, Julian R.; Grande, Tor [Department of Materials Science and Engineering, Norwegian University of Science and Technology, NO-7491 Trondheim (Norway); Geiger, Philipp T.; Webber, Kyle G. [Department of Materials Science, Friedrich-Alexander-Universität Erlangen-Nürnberg, 91058 Erlangen (Germany); Damjanovic, Dragan [Ceramics Laboratory, Swiss Federal Institute of Technology in Lausanne-EPFL, 1015 Lausanne (Switzerland)

    2015-10-28

    Despite the technological importance of hard and soft PZT, Pb(Zr,Ti)O{sub 3}, ceramics, the mechanisms of ferroelectric hardening and softening remain widely discussed in the literature. The hardening and softening phenomena have traditionally been investigated in relation with dielectric manifestations such as aging of the dielectric susceptibility and constriction of the polarization-electric field hysteresis loop. Here, we present a systematic investigation of the ferroelectric and ferroelastic properties of soft and hard PZT in both the tetragonal and rhombohedral phases. A particular focus has been devoted to ferroelastic domain switching by characterizing the macroscopic mechanical constitutive behavior and in-situ synchrotron X-ray diffraction during compression. It is demonstrated that variation of the ordering state of point defects in PZT ceramics affects the switching behavior of both ferroelectric and ferroelastic domains under mechanical or electrical fields. Softening of the mechanical and electrical properties of originally hard PZT ceramics was conferred by quenching the materials from above the Curie temperature. The present findings are discussed with respect to the current understanding of hardening-softening transitions in ferroelectric materials.

  3. Custom AFM for X-ray beamlines: in situ biological investigations under physiological conditions

    Energy Technology Data Exchange (ETDEWEB)

    Gumí-Audenis, B. [ESRF, The European Synchrotron, Grenoble (France); Institute for Bioengineering of Catalonia (IBEC), Barcelona (Spain); Physical Chemistry Department, Universitat de Barcelona, Barcelona (Spain); Networking Biomedical Research Center on Bioengineering, Biomaterials and Nanomedicine (CIBER-BBN), Madrid (Spain); Carlà, F. [ESRF, The European Synchrotron, Grenoble (France); Vitorino, M. V. [University of Lisboa, Falculty of Science, Biosystems and Integrative Sciences Institute - BIOISI, Lisbon (Portugal); Panzarella, A. [ESRF, The European Synchrotron, Grenoble (France); Porcar, L. [Institut Laue-Langevin, Grenoble (France); Boilot, M. [ORTEC, Marseille (France); Guerber, S. [CEA, LETI Grenoble (France); Bernard, P. [ESRF, The European Synchrotron, Grenoble (France); Rodrigues, M. S. [University of Lisboa, Falculty of Science, Biosystems and Integrative Sciences Institute - BIOISI, Lisbon (Portugal); Sanz, F.; Giannotti, M. I. [Institute for Bioengineering of Catalonia (IBEC), Barcelona (Spain); Physical Chemistry Department, Universitat de Barcelona, Barcelona (Spain); Networking Biomedical Research Center on Bioengineering, Biomaterials and Nanomedicine (CIBER-BBN), Madrid (Spain); Costa, L., E-mail: luca.costa@esrf.fr [ESRF, The European Synchrotron, Grenoble (France)

    2015-09-30

    The performance of a custom atomic force microscope for grazing-incidence X-ray experiments on hydrated soft and biological samples is presented. A fast atomic force microscope (AFM) has been developed that can be installed as a sample holder for grazing-incidence X-ray experiments at solid/gas or solid/liquid interfaces. It allows a wide range of possible investigations, including soft and biological samples under physiological conditions (hydrated specimens). The structural information obtained using the X-rays is combined with the data gathered with the AFM (morphology and mechanical properties), providing a unique characterization of the specimen and its dynamics in situ during an experiment. In this work, lipid monolayers and bilayers in air or liquid environment have been investigated by means of AFM, both with imaging and force spectroscopy, and X-ray reflectivity. In addition, this combination allows the radiation damage induced by the beam on the sample to be studied, as has been observed on DOPC and DPPC supported lipid bilayers under physiological conditions.

  4. Tem holder for sample transfer under reaction conditions

    DEFF Research Database (Denmark)

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

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

  5. 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

  6. Next generation in-situ optical Raman sensor for seawater investigations

    Science.gov (United States)

    Kolomijeca, A.; Kwon, Y.-H.; Ahmad, H.; Kronfeldt, H.-D.

    2012-04-01

    We introduce the next generation of optical sensors based on a combination of surfaced enhanced Raman scattering (SERS) and shifted excitation Raman difference spectroscopy (SERDS) suited for investigations of tiny concentrations of pollutions in the seawater. First field measurements were carried out in the Arctic area which is of global interest since it is more affected by global warming caused climatic changes than any other areas of our planet and it is a recipient for many toxic organic pollutants. A significant long-range atmospheric transport of pollutants to Svalbard is mainly originated from industrialized countries in Europe and North America during the last decades. Therefore, the main interest is to investigate the Arctic water column and also the sediments. Standard chemical methods for water/sediment analysis are extremely accurate but complex and time-consuming. The primary objective of our study was to develop a fast response in-situ optical sensor for easy to use and quick analysis. The system comprises several components: a handheld measurement head containing a 671 nm microsystem diode laser and the Raman optical bench, a laser driver electronics board, a custom-designed miniature spectrometer with an optical resolution of 8 cm-1 and a netbook to control the spectrometer as well as for data evaluation. We introduced for the first time the portable Raman sensor system on an Artic sea-trial during a three week cruise on board of the James Clark Ross research vessel in August 2011. Numerous Raman and SERS measurements followed by SERDS evaluations were taken around locations 78° N and 9° E. Different SERS substrates developed for SERS measurements in sea-water were tested for their capability to detect different substances (PAHs) in the water down to very small (nmol/l) concentrations. Stability tests of the substrates were carried out also for the applicability of our system e.g. on a mooring. Details of the in-situ Raman sensor were presented

  7. TEM turbulence optimisation in stellarators

    Science.gov (United States)

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

    2016-01-01

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

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

    Science.gov (United States)

    Kobler, A; Kübel, C

    2017-02-01

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

  9. An investigation of the potential for in situ bioremediation of oil sands tailings

    International Nuclear Information System (INIS)

    Herman, D.C.; Costerton, J.W.; Fedorak, P.M.; Mackinnon, M.D.

    1993-01-01

    Oil sand tailings water has been shown to be acutely toxic to aquatic organisms. Naphthenic acids have been shown to be the primary source of this toxicity within oil sand tailings waste. The potential for in-situ bioremediation of oil sand tailings was investigated by determining the ability of indigenous bacteria to biodegrade naphthenic acids. A mixed bacterial culture enriched from oil sand tailings was found to be capable of growth on a commercially available naphthenic acid mixture. When sodium naphthenates (30 mg/l) were added to a minimal salts medium and inoculated with the mixed bacterial culture, gas chromatography revealed that many components of the naphthenic acid mixture were biodegraded within eight days of incubation. The same culture was also tested against the naphthenic acid fraction extracted directly from oil sand tailings. The tailings extract was diluted into the minimal salts medium in sealed flasks and inoculated with the enrichment culture. The production of CO 2 indicated microbial mineralization of components within the oil sands extract. Microtox analysis determined that microbial activity resulted in a reduction in the acute toxicity of the tailings extract. 5 refs., 3 figs

  10. In situ neutron diffraction investigation on the phase transformation sequence of kaolinite and halloysite to mullite

    Energy Technology Data Exchange (ETDEWEB)

    Tezuka, Nobuo [Department of Applied Physics, Curtin University of Technology, GPO Box U1987, Perth, WA 6845 (Australia); Low, It-Meng [Department of Applied Physics, Curtin University of Technology, GPO Box U1987, Perth, WA 6845 (Australia)]. E-mail: J.Low@curtin.edu.au; Davies, Ian J. [Department of Mechanical Engineering, Curtin University of Technology, GPO Box U1987, Perth, WA 6845 (Australia); Prior, Michael [Bragg Institute, ANSTO, PMB 1, Menai, NSW 2234 (Australia); Studer, Andrew [Bragg Institute, ANSTO, PMB 1, Menai, NSW 2234 (Australia)

    2006-11-15

    'Kaolin' is a major raw material for the fabrication of conventional ceramics. In this work the authors have investigated the thermal phase transformation of mullite from two different types of kaolin (kaolinite and halloysite), with or without alumina matrix constraint, during heating up to 1500 deg. C and then cooling using in situ neutron diffraction. Mullitization was initiated upon heating to 1200 deg. C for all specimens and followed spinel formation at 1100 deg. C. Above this temperature, however, evolution of the main phases, i.e., mullite, cristobalite and corundum, was influenced by the presence of impurities, initial type of silica, and alumina constraint. The relative amount of mullite was largest for the pure kaolinite specimen, particularly during heating, and this was attributed to the presence of a glassy phase. However, kaolinite with alumina suppressed the crystallization of cristobalite from the glassy phase upon cooling due to a reaction between alumina and amorphous silica, consequently resulting in an amount of mullite as for the pure kaolinite specimen (approximately 65 wt%). Halloysite was less active in terms of mullitization due to the lower level of initial impurities and greater amount of cristobalite, particularly for the alumina-constrained specimen. However, the final amount of mullite derived from the pure halloysite specimen was similar to that as from the kaolinite specimen.

  11. In situ neutron diffraction investigation on the phase transformation sequence of kaolinite and halloysite to mullite

    International Nuclear Information System (INIS)

    Tezuka, Nobuo; Low, It-Meng; Davies, Ian J.; Prior, Michael; Studer, Andrew

    2006-01-01

    'Kaolin' is a major raw material for the fabrication of conventional ceramics. In this work the authors have investigated the thermal phase transformation of mullite from two different types of kaolin (kaolinite and halloysite), with or without alumina matrix constraint, during heating up to 1500 deg. C and then cooling using in situ neutron diffraction. Mullitization was initiated upon heating to 1200 deg. C for all specimens and followed spinel formation at 1100 deg. C. Above this temperature, however, evolution of the main phases, i.e., mullite, cristobalite and corundum, was influenced by the presence of impurities, initial type of silica, and alumina constraint. The relative amount of mullite was largest for the pure kaolinite specimen, particularly during heating, and this was attributed to the presence of a glassy phase. However, kaolinite with alumina suppressed the crystallization of cristobalite from the glassy phase upon cooling due to a reaction between alumina and amorphous silica, consequently resulting in an amount of mullite as for the pure kaolinite specimen (approximately 65 wt%). Halloysite was less active in terms of mullitization due to the lower level of initial impurities and greater amount of cristobalite, particularly for the alumina-constrained specimen. However, the final amount of mullite derived from the pure halloysite specimen was similar to that as from the kaolinite specimen

  12. A New Platform for Investigating In-Situ NIR Reflectance in Snow

    Science.gov (United States)

    Johnson, M.; Taubenheim, J. R. L.; Stevenson, R.; Eldred, D.

    2017-12-01

    In-situ near infrared (NIR) reflectance measurements of the snowpack have been shown to have correlations to valuable snowpack properties. To-date many studies take these measurements by digging a pit and setting up a NIR camera to take images of the wall. This setup is cumbersome, making it challenging to investigate things like spatial variability. Over the course of 3 winters, a new device has been developed capable of mitigating some of the downfalls of NIR open pit photography. This new instrument is a NIR profiler capable of taking NIR reflectance measurements without digging a pit, with most measurements taking less than 30 seconds to retrieve data. The latest prototype is built into a ski pole and automatically transfers data wirelessly to the users smartphone. During 2016-2017 winter, the device was used by 37 different users resulting in over 4000 measurements in the Western United States, demonstrating a dramatic reduction in time to data when compared to other methods. Presented here are some initial findings from a full winter of using the ski pole version of this device.

  13. Investigation on the determining factor in the performance of in situ fabricated lithium polymer secondary battery

    International Nuclear Information System (INIS)

    Kong Lingbo; Zhan Hui; Li Yajuan; Zhou Yunhong

    2008-01-01

    In our preliminary research, an in situ fabrication of the lithium polymer cell starting from Li/1 M LiTFSI in DOL + DME (2:1 by weight)/LiCoO 2 cell is successfully achieved owing to the electro-polymerization of DOL solvent. Basing on previous work, a comprehensive investigation on the new technology is conducted and some significant result is presented in this paper. The influence of three leading factors such as: current rate, upper limit voltage and temperature are laid a heavy emphasis. It is found that upper limit voltage is a prerequisite to the initiation of DOL polymerization as long as the operating temperature is kept far below the temperature limit for the occurrence of thermal-initiated polymerization. Once this requirement is satisfied, the current rate exerts a positive influence on DOL's electro-polymerization and helps to the formation of a conductive polymer electrolyte, but as another two factors are concerned, the case is just the reverse. And besides, benefiting from the 'regulation' effect of current rate, the lack of capacity retentivity that is encountered during the high-temperature or high-voltage cycling can be compensated by an electrochemical pretreatment. And finally, it is indicated that all the influential mechanism tightly related to the variation in the cell internal resistance

  14. Investigation of the Interaction between Perovskite Films with Moisture via in Situ Electrical Resistance Measurement.

    Science.gov (United States)

    Hu, Long; Shao, Gang; Jiang, Tao; Li, Dengbing; Lv, Xinlin; Wang, Hongya; Liu, Xinsheng; Song, Haisheng; Tang, Jiang; Liu, Huan

    2015-11-18

    Organometal halide perovskites have recently emerged as outstanding semiconductors for solid-state optoelectronic devices. Their sensitivity to moisture is one of the biggest barriers to commercialization. In order to identify the effect of moisture in the degradation process, here we combined the in situ electrical resistance measurement with time-resolved X-ray diffraction analysis to investigate the interaction of CH3NH3PbI(3-x)Cl(x) perovskite films with moisture. Upon short-time exposure, the resistance of the perovskite films decreased and it could be fully recovered, which were ascribed to a mere chemisorption of water molecules, followed by the reversible hydration into CH3NH3PbI(3-x)Cl(x)·H2O. Upon long-time exposure, however, the resistance became irreversible due to the decomposition into PbI2. The results demonstrated the formation of monohydrated intermediate phase when the perovskites interacted with moisture. The role of moisture in accelerating the thermal degradation at 85 °C was also demonstrated. Furthermore, our study suggested that the perovskite films with fewer defects may be more inherently resistant to moisture.

  15. Stability investigations of zinc and cobalt precipitates immobilized by in situ bioprecipitation (ISBP) process

    KAUST Repository

    Satyawali, Yamini; Schols, Edo; Van Roy, Sandra; Dejonghe, Winnie; Diels, Ludo; Vanbroekhoven, Karolien

    2010-01-01

    In situ bioprecipitation (ISBP), which involves immobilizing the metals as precipitates (mainly sulphides) in the solid phase, is an effective method of metal removal from contaminated groundwater. This study investigated the stability of metal precipitates formed after ISBP in two different solid-liquid matrices (artificial and natural). The artificial matrix consisted of sand, Zn (200mgL-1), artificial groundwater and a carbon source (electron donor). Here the stability of the Zn precipitates was evaluated by manipulation of redox and pH. The natural system matrices included aquifer material and groundwater samples collected from three different metal (Zn and Co) contaminated sites and different carbon sources were provided as electron donors. In the natural matrices, metal precipitates stability was assessed by changing aquifer redox conditions, sequential extraction, and BIOMET® assay. The results indicated that, in the artificial matrix, redox manipulation did not impact the Zn precipitates. However the sequential pH change proved detrimental, releasing 58% of the precipitated Zn back into liquid phase. In natural matrices, the applied carbon source largely affected the stability of metal precipitates. Elemental analysis performed on the precipitates formed in natural matrix showed that the main elements of the precipitates were sulphur with Zn and Co. © 2010 Elsevier B.V.

  16. Novel in situ resistance measurement for the investigation of CIGS growth in a selenization process

    International Nuclear Information System (INIS)

    Liu Wei; He Qing; Li Fengyan; Li Changjian; Sun Yun; Tian Jianguo; Li Zubin

    2009-01-01

    During the selenization process of CIGS thin films, the relation between the element loss rate and the precursor depositions are analyzed. The growth of the CIGS thin films during the selenization process is investigated by the novel in situ resistance measurement, by which the formation of compound semiconductors can be observed directly and simultaneously. Their structures, phase evolutions and element losses are analyzed by XRD and XRF. Based on the experimental results, it can be concluded that the phase transforms have nothing to do with the deposition sequences of precursors, while the element loss rates are related to the deposition sequences in this process. In addition, element loss mechanisms of CIGS thin films prepared by the selenization process are analyzed by the phase evolutions and chemical combined path in the In, Ga–Se reaction processes. Moreover it is verified that the element losses are depressed by increasing the ramping-up rate finally. The results provide effective methods to fabricate high-quality CIGS thin films with low element losses

  17. Novel in situ resistance measurement for the investigation of CIGS growth in a selenization process

    Science.gov (United States)

    Liu, Wei; Tian, Jian-Guo; Li, Zu-Bin; He, Qing; Li, Feng-Yan; Li, Chang-Jian; Sun, Yun

    2009-03-01

    During the selenization process of CIGS thin films, the relation between the element loss rate and the precursor depositions are analyzed. The growth of the CIGS thin films during the selenization process is investigated by the novel in situ resistance measurement, by which the formation of compound semiconductors can be observed directly and simultaneously. Their structures, phase evolutions and element losses are analyzed by XRD and XRF. Based on the experimental results, it can be concluded that the phase transforms have nothing to do with the deposition sequences of precursors, while the element loss rates are related to the deposition sequences in this process. In addition, element loss mechanisms of CIGS thin films prepared by the selenization process are analyzed by the phase evolutions and chemical combined path in the In, Ga-Se reaction processes. Moreover it is verified that the element losses are depressed by increasing the ramping-up rate finally. The results provide effective methods to fabricate high-quality CIGS thin films with low element losses.

  18. Stability investigations of zinc and cobalt precipitates immobilized by in situ bioprecipitation (ISBP) process

    KAUST Repository

    Satyawali, Yamini

    2010-09-01

    In situ bioprecipitation (ISBP), which involves immobilizing the metals as precipitates (mainly sulphides) in the solid phase, is an effective method of metal removal from contaminated groundwater. This study investigated the stability of metal precipitates formed after ISBP in two different solid-liquid matrices (artificial and natural). The artificial matrix consisted of sand, Zn (200mgL-1), artificial groundwater and a carbon source (electron donor). Here the stability of the Zn precipitates was evaluated by manipulation of redox and pH. The natural system matrices included aquifer material and groundwater samples collected from three different metal (Zn and Co) contaminated sites and different carbon sources were provided as electron donors. In the natural matrices, metal precipitates stability was assessed by changing aquifer redox conditions, sequential extraction, and BIOMET® assay. The results indicated that, in the artificial matrix, redox manipulation did not impact the Zn precipitates. However the sequential pH change proved detrimental, releasing 58% of the precipitated Zn back into liquid phase. In natural matrices, the applied carbon source largely affected the stability of metal precipitates. Elemental analysis performed on the precipitates formed in natural matrix showed that the main elements of the precipitates were sulphur with Zn and Co. © 2010 Elsevier B.V.

  19. Charge transfer in carbon nanotube actuators investigated using in situ Raman spectroscopy

    International Nuclear Information System (INIS)

    Gupta, S.; Hughes, M.; Windle, A.H.; Robertson, J.

    2004-01-01

    Charge transfer dynamics on the surface of single-wall carbon nanotube sheets is investigated using in situ Raman spectroscopy in order to understand the actuation mechanism of an electrochemical actuator and to determine associated parameters. We built an actuator from single-wall carbon nanotube mat and studied its actuation in several alkali metal (Li, Na, and K) and alkaline earth (Ca) halide and sulfate solutions in order to clarify the role of counterion as mobile ions in the film. The variation of bonding with applied potential was monitored using in situ Raman spectroscopy. This is because Raman can detect changes in C-C bond length: the radial breathing mode at ∼190 cm-1 varies inversely with the nanotube diameter, and the G band at ∼1590 cm-1 varies with the axial bond length. In addition, the intensities of both the modes vary with the emptying/depleting or filling of the bonding and antibonding states due to electrochemical charge injection. We discussed the variation of peak height and wave numbers of these modes providing valuable information concerning electrochemical charge injection on the carbon nanotube mat surface. We found in-plane microscopic compressive strain (∼-0.25%) and the equivalent charge transfer per carbon atom (f c ∼-0.005) as an upper bound for the actuators studied hereby. It is demonstrated that though the present analysis does comply with the proposition for the actuation principle made earlier, the quantitative estimates are significantly lower if compared with those of reported values. Furthermore, the extent of variation, i.e., coupled electro-chemo-mechanical response of single-wall carbon nanotubes (SWNT) mat depended upon the type of counterion used (Group I versus Group II). The cyclic voltammetry and ac electrochemical impedance spectroscopy results were described briefly, which help to demonstrate well-developed capacitive behavior of SWNT mat and to estimate the specific capacitances as well. Summarizing, the

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

    DEFF Research Database (Denmark)

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

    2011-01-01

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

  1. In-situ Investigation of Lead-free Solder Alloy Formation Using a Hot-plate Microscope

    DEFF Research Database (Denmark)

    Bergmann, René; Tang, Peter Torben; Hansen, Hans Nørgaard

    2007-01-01

    This work presents the advantages of using a hot-plate microscope for investigation of new (high-temperature) lead- free solders as in-situ analysis tool and preparation equipment. A description of the equipment and the preparation method is given and some examples are outlined. The formation...

  2. 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)

  3. Investigation of Lobular Carcinoma In Situ, Using Molecular Genetic Techniques, for the Involvement of Novel Genes

    National Research Council Canada - National Science Library

    Mastracci, Teresa

    2003-01-01

    Atypical lobular hyperplasia (ALH) and lobular carcinoma in situ (LCIS), i.e. lobular neoplasia, are lesions of significance in terms of implication of risk to the patient in the development of invasive carcinorna...

  4. Solution-Processing of Organic Solar Cells: From In Situ Investigation to Scalable Manufacturing

    KAUST Repository

    Abdelsamie, Maged

    2016-12-05

    implementation of organic solar cells with high efficiency and manufacturability. In this dissertation, we investigate the mechanism of the BHJ layer formation during solution processing from common lab-based processes, such as spin-coating, with the aim of understanding the roles of materials, formulations and processing conditions and subsequently using this insight to enable the scalable manufacturing of high efficiency organic solar cells by such methods as wire-bar coating and blade-coating. To do so, we have developed state-of-the-art in situ diagnostics techniques to provide us with insight into the thin film formation process. As a first step, we have developed a modified spin-coater which allows us to perform in situ UV-visible absorption measurements during spin coating and provides key insight into the formation and evolution of polymer aggregates in solution and during the transformation to the solid state. Using this method, we have investigated the formation of organic BHJs made of a blend of poly (3-hexylthiophene) (P3HT) and fullerene, reference materials in the organic solar cell field. We show that process kinetics directly influence the microstructure and morphology of the bulk heterojunction, highlighting the value of in situ measurements. We have investigated the influence of crystallization dynamics of a wide-range of small-molecule donors and their solidification pathways on the processing routes needed for attaining high-performance solar cells. The study revealed the reason behind the need of empirically-adopted processing strategies such as solvent additives or alternatively thermal or solvent vapor annealing for achieving optimal performance. The study has provided a new perspective to materials design linking the need for solvent additives or annealing to the ease of crystallization of small-molecule donors and the presence or absence of transient phases before crystallization. From there, we have extended our investigation to small-molecule (p

  5. Investigating the biogeochemical interactions involved in simultaneous TCE and Arsenic in situ bioremediation

    Science.gov (United States)

    Cook, E.; Troyer, E.; Keren, R.; Liu, T.; Alvarez-Cohen, L.

    2016-12-01

    The in situ bioremediation of contaminated sediment and groundwater is often focused on one toxin, even though many of these sites contain multiple contaminants. This reductionist approach neglects how other toxins may affect the biological and chemical conditions, or vice versa. Therefore, it is of high value to investigate the concurrent bioremediation of multiple contaminants while studying the microbial activities affected by biogeochemical factors. A prevalent example is the bioremediation of arsenic at sites co-contaminated with trichloroethene (TCE). The conditions used to promote a microbial community to dechlorinate TCE often has the adverse effect of inducing the release of previously sequestered arsenic. The overarching goal of our study is to simultaneously evaluate the bioremediation of arsenic and TCE. Although TCE bioremediation is a well-understood process, there is still a lack of thorough understanding of the conditions necessary for effective and stable arsenic bioremediation in the presence of TCE. The objective of this study is to promote bacterial activity that stimulates the precipitation of stable arsenic-bearing minerals while providing anaerobic, non-extreme conditions necessary for TCE dechlorination. To that end, endemic microbial communities were examined under various conditions to attempt successful sequestration of arsenic in addition to complete TCE dechlorination. Tested conditions included variations of substrates, carbon source, arsenate and sulfate concentrations, and the presence or absence of TCE. Initial arsenic-reducing enrichments were unable to achieve TCE dechlorination, probably due to low abundance of dechlorinating bacteria in the culture. However, favorable conditions for arsenic precipitation in the presence of TCE were eventually discovered. This study will contribute to the understanding of the key species in arsenic cycling, how they are affected by various concentrations of TCE, and how they interact with the key

  6. Investigation of digestion Kinetics in commercial starches using in-situ small-angle neutron scattering

    International Nuclear Information System (INIS)

    Blazek, Jaroslav; Gilbert, Elliot Paul

    2009-01-01

    Full text: The digestion of starch has been the subject of many investigations, mostly involving in vitro measurement of the susceptibility of starches to attack by different enzymes, rather than measuring actual digestibility in vivo. The rate and extent of amylolytic hydrolysis of granular starches is known to vary according to botanical origin. Granule characteristics considered to influence susceptibility to attack by alpha-amylase include crystallinity, granule size and available specific surface, amylose content, porosity, structural inhomogeneities and degree of integrity. Most in-vitro studies of granular starch digestion have been limited to samples for which aliquots have been removed from the reaction mixture at various time intervals and freeze-dried to be subsequently characterized using a range of techniques. It remains unclear whether sample preparation creates artefacts in the samples. In this study, we have studied the kinetics of starch digestion of several commercial granular starches by time-resolved small-angle neutron scattering using an in-situ digestion chamber allowing, for the first time, to follow structural changes of starch in the course of digestion directly in the digestion mixture. Additionally, samples before and after digestion were studied by x-ray diffraction, small-angle x-ray scattering, differential scanning calorimetry and microscopy. Microscopy revealed that studied starches, which varied in their amylose content and digestion kinetics, followed different modes of attack The multidisciplinary approach allowed the nanostructural changes detected by small-angle scattering in the course of enzymic breakdown to be correlated with changes in crystallinity and functional properties.

  7. Investigation of CaO-CO₂ reaction kinetics by in-situ XRD using synchrotron radiation

    Energy Technology Data Exchange (ETDEWEB)

    Biasin, A.; Segre, C. U.; Salviulo, G.; Zorzi, F.; Strumendo, M. [Padova; (IIT)

    2015-02-05

    In this work, in-situ synchrotron radiation x-ray powder diffraction (SR-XRPD), performed at the Advanced Photon Source (APS) facilities of the Argonne National Laboratory, was applied to investigate the CaO–CO2 reaction. A set of CO2 absorption experiments were conducted in a high temperature reaction capillary with a controlled atmosphere (CO2 partial pressure of 1 bar), in the temperature range between 450 °C and 750 °C using CaO based sorbents obtained by calcination of commercial calcium carbonate. The evolution of the crystalline phases during CO2 uptake by the CaO solid sorbents was monitored for a carbonation time of 20 min as a function of the carbonation temperature and of the calcination conditions. The Rietveld refinement method was applied to estimate the calcium oxide conversion during the reaction progress and the average size of the initial (at the beginning of carbonation) calcium oxide crystallites. The measured average initial carbonation rate (in terms of conversion time derivative) of 0.280 s-1 (±13.2% standard deviation) is significantly higher than the values obtained by thermo-gravimetric analysis and reported thus far in the literature. Additionally, a dependence of the conversion versus time curves on the initial calcium oxide crystallite size was observed and a linear relationship between the initial CaO crystallite size and the calcium oxide final conversion was identified.

  8. Investigation of the Geokinetics horizontal in situ oil-shale-retorting process. Fourth annual report, 1980

    Energy Technology Data Exchange (ETDEWEB)

    Hutchinson, D.L. (ed.)

    1981-03-01

    The Geokinetics in situ shale oil project is a cooperative venture between Geokinetics Inc. and the US Department of Energy. The objective is to develop a true in situ process for recovering shale oil using a fire front moving in a horizontal direction. The project is being conducted at a field site, Kamp Kerogen, located 70 miles south of Vernal, Utah. This Fourth Annual Report covers work completed during the calendar year 1980. During 1980 one full-size retort was blasted. Two retorts, blasted the previous year, were burned. A total of 4891 barrels of oil was produced during the year.

  9. Taoshan uranium ore fields in situ blasting heap leaching rate influence factors to investigate

    International Nuclear Information System (INIS)

    Xie Wangnan; Dong Chunming

    2014-01-01

    Taoshan ore field ore in situ blasting heap leaching out build industrial test and production process, stope leaching rate and leaching cycle is large than that, after analysis, blasting method and cloth liquid way is to affect leaching rate and leaching cycle of the main factors. This paper holds that as far as possible using stratified deep hole blasting of squeezing up ways to reduce the building pile of in-situ leaching ore block rate; Adopting effective cloth tube way, increase the leaching agent and ore contact comprehensive; Introduction of bacterial leaching, and other means to improve leaching rate, shorten production cycle, etc to solve it. (authors)

  10. In-situ Liquid Electron Microscopy Setups for Investigation of Nanoscale Electrochemistry

    DEFF Research Database (Denmark)

    Jensen, Eric; Møller-Nilsen, Rolf Erling Robberstad; Canepa, Silvia

    2014-01-01

    -situ electrochemistry and has achieved ~10 nm resolution. Such systems are important tools for developing sustainable technology and for understanding nanoscale phenomena. However, both systems suffer from interacting with theelectron beam, which is a high-voltage radiation source, and therefore initial experiments...

  11. Laboratory investigations of Titan haze formation: In situ measurement of gas and particle composition

    Science.gov (United States)

    Hörst, Sarah M.; Yoon, Y. Heidi; Ugelow, Melissa S.; Parker, Alex H.; Li, Rui; de Gouw, Joost A.; Tolbert, Margaret A.

    2018-02-01

    Prior to the arrival of the Cassini-Huygens spacecraft, aerosol production in Titan's atmosphere was believed to begin in the stratosphere where chemical processes are predominantly initiated by far ultraviolet (FUV) radiation. However, measurements taken by the Cassini Ultraviolet Imaging Spectrograph (UVIS) and Cassini Plasma Spectrometer (CAPS) indicate that haze formation initiates in the thermosphere where there is a greater flux of extreme ultraviolet (EUV) photons and energetic particles available to initiate chemical reactions, including the destruction of N2. The discovery of previously unpredicted nitrogen species in measurements of Titan's atmosphere by the Cassini Ion and Neutral Mass Spectrometer (INMS) indicates that nitrogen participates in the chemistry to a much greater extent than was appreciated before Cassini. The degree of nitrogen incorporation in the haze particles is important for understanding the diversity of molecules that may be present in Titan's atmosphere and on its surface. We have conducted a series of Titan atmosphere simulation experiments using either spark discharge (Tesla coil) or FUV photons (deuterium lamp) to initiate chemistry in CH4/N2 gas mixtures ranging from 0.01% CH4/99.99% N2 to 10% CH4/90% N2. We obtained in situ real-time measurements using a high-resolution time-of-flight aerosol mass spectrometer (HR-ToF-AMS) to measure the particle composition as a function of particle size and a proton-transfer ion-trap mass spectrometer (PIT-MS) to measure the composition of gas phase products. These two techniques allow us to investigate the effect of energy source and initial CH4 concentration on the degree of nitrogen incorporation in both the gas and solid phase products. The results presented here confirm that FUV photons produce not only solid phase nitrogen bearing products but also gas phase nitrogen species. We find that in both the gas and solid phase, nitrogen is found in nitriles rather than amines and that both the

  12. Experimental and in situ investigations on americium, curium and plutonium behaviour in marine benthic species: transfer from water or sediments

    International Nuclear Information System (INIS)

    Miramand, P.

    1984-06-01

    The tranfer of transuranic elements -americium, curium and plutonium- from the sediments containing them to some marine benthic species (endofauna and epifauna) was studied with a twofold approach - laboratory and in-situ investigation. The experimental investigations, divided into three parts, made it possible to specify concentration factors (F.C.), transfer factors (F.T.) and to understand the process involved for 5 benthic species. The result were refined by an in-situ study that brought new data on the marine distribution of the transuranic elements released by the La Hague plant. Finally, the localization of americium and plutonium in the tissues and cells of these species was determined by autoradiography [fr

  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. 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...

  15. Thermodynamic modelling and in-situ neutron diffraction investigation of the (Ce + Mg + Zn) system

    International Nuclear Information System (INIS)

    Zhu, Zhijun; Gharghouri, Michael A.; Medraj, Mamoun; Lee, Soo Yeol; Pelton, Arthur D.

    2016-01-01

    Highlights: • All phase diagram and thermodynamic data critically assessed for the (Ce + Mg + Zn) system. • All phases described by optimized thermodynamic models. • In-situ neutron diffraction performed to identify phases and transition temperatures. • Assessments of other (RE + Mg + Zn) systems have been carried out simultaneously. • The final product is a thermodynamic database for multicomponent (Mg + RE + Zn) systems. - Abstract: All available phase diagram data for the (Ce + Mg + Zn) system were critically assessed. In-situ neutron diffraction (ND) experiments were performed on selected samples to identify phases and transition temperatures. A critical thermodynamic evaluation and optimization of the (Ce + Mg + Zn) system were carried out and model parameters for the thermodynamic properties of all phases were obtained. The phase transformation behaviour of selected samples was well resolved from the ND experiments and experimental data were used to refine the thermodynamic model parameters.

  16. In-situ investigation of the calcination process of mixed oxide xerogels with Raman spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Panitz, J C [Paul Scherrer Inst. (PSI), Villigen (Switzerland)

    1997-06-01

    The controlled calcination of materials derived by sol-gel reactions is important for the evolution of the final structure. Raman spectroscopy is an ideal tool for the identification of surface species under in-situ conditions, as demonstrated in the following for the example of a molybdenum oxide-silica xerogel. Raman spectra of this particular sample were recorded at temperatures as high as 1173 K, and compared with those of a reference material.(author) 3 figs., 4 refs.

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

    Science.gov (United States)

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

    2004-03-01

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

  18. Investigation into the Use of the Concept Laser QM System as an In-Situ Research and Evaluation Tool

    Science.gov (United States)

    Bagg, Stacey

    2014-01-01

    The NASA Marshall Space Flight Center (MSFC) is using a Concept Laser Fusing (Cusing) M2 powder bed additive manufacturing system for the build of space flight prototypes and hardware. NASA MSFC is collecting and analyzing data from the M2 QM Meltpool and QM Coating systems for builds. This data is intended to aide in understanding of the powder-bed additive manufacturing process, and in the development of a thermal model for the process. The QM systems are marketed by Concept Laser GmbH as in-situ quality management modules. The QM Meltpool system uses both a high-speed near-IR camera and a photodiode to monitor the melt pool generated by the laser. The software determines from the camera images the size of the melt pool. The camera also measures the integrated intensity of the IR radiation, and the photodiode gives an intensity value based on the brightness of the melt pool. The QM coating system uses a high resolution optical camera to image the surface after each layer has been formed. The objective of this investigation was to determine the adequacy of the QM Meltpool system as a research instrument for in-situ measurement of melt pool size and temperature and its applicability to NASA's objectives in (1) Developing a process thermal model and (2) Quantifying feedback measurements with the intent of meeting quality requirements or specifications. Note that Concept Laser markets the system only as capable of giving an indication of changes between builds, not as an in-situ research and evaluation tool. A secondary objective of the investigation is to determine the adequacy of the QM Coating system as an in-situ layer-wise geometry and layer quality evaluation tool.

  19. TEM sample preparation by femtosecond laser machining and ion milling for high-rate TEM straining experiments

    Energy Technology Data Exchange (ETDEWEB)

    Voisin, Thomas; Grapes, Michael D. [Dept. of Materials Science and Engineering, Johns Hopkins University, Baltimore, MD 21218 (United States); Zhang, Yong [Dept. of Mechanical Engineering, Johns Hopkins University, Baltimore, MD 21218 (United States); Lorenzo, Nicholas; Ligda, Jonathan; Schuster, Brian [US Army Research Laboratory, Aberdeen Proving Ground, Aberdeen, MD 21005 (United States); Weihs, Timothy P. [Dept. of Materials Science and Engineering, Johns Hopkins University, Baltimore, MD 21218 (United States)

    2017-04-15

    To model mechanical properties of metals at high strain rates, it is important to visualize and understand their deformation at the nanoscale. Unlike post mortem Transmission Electron Microscopy (TEM), which allows one to analyze defects within samples before or after deformation, in situ TEM is a powerful tool that enables imaging and recording of deformation and the associated defect motion during mechanical loading. Unfortunately, all current in situ TEM mechanical testing techniques are limited to quasi-static strain rates. In this context, we are developing a new test technique that utilizes a rapid straining stage and the Dynamic TEM (DTEM) at the Lawrence Livermore National Laboratory (LLNL). The new straining stage can load samples in tension at strain rates as high as 4×10{sup 3}/s using two piezoelectric actuators operating in bending while the DTEM at LLNL can image in movie mode with a time resolution as short as 70 ns. Given the piezoelectric actuators are limited in force, speed, and displacement, we have developed a method for fabricating TEM samples with small cross-sectional areas to increase the applied stresses and short gage lengths to raise the applied strain rates and to limit the areas of deformation. In this paper, we present our effort to fabricate such samples from bulk materials. The new sample preparation procedure combines femtosecond laser machining and ion milling to obtain 300 µm wide samples with control of both the size and location of the electron transparent area, as well as the gage cross-section and length. - Highlights: • Tensile straining TEM specimens made by femtosecond laser machining and ion milling. • Accurate positioning of the electron transparent area within a controlled gauge region. • Optimization of femtosecond laser and ion milling parameters. • Fast production of numerous samples with a highly repeatable geometry.

  20. Experimental Investigation of In Situ Cleanable or Regenerative Filters for High Level Radioactive Waste Tanks

    International Nuclear Information System (INIS)

    Adamson, D.J.

    2000-01-01

    The Westinghouse Savannah River Company, located at the Savannah River Site (SRS) in Aiken, South Carolina, is currently testing two types of filter media for application as in situ regenerable/cleanable filters on high-level radioactive liquid waste tanks. Each of the 1.3 million-gallon tanks is equipped with an exhaust ventilation system to provide tank ventilation and to maintain the tank contents at approximately 1-in. water gauge vacuum to prevent the release of radioactive material to the environment. These systems are equipped with conventional, disposable, glass-fiber, High Efficiency Particulate Air (HEPA) filters that require frequent removal, replacement, and disposal. The need for routine replacements is often caused by accelerated filter loading due to the moist operating environment, which structurally weakens the filter media. This is not only costly, but subjects site personnel to radiation exposure and possible contamination. The types of filter media tested, as part of a National Energy Technology Laboratory procurement, were sintered metal and monolith ceramic. The media were subjected to a hostile environment to simulate conditions that challenge the tank ventilation systems. The environment promoted rapid filter plugging to maximize the number of filter loading/cleaning cycles that would occur in a specified period of time. The filters were challenged using non-radioactive, simulated high level waste materials and atmospheric dust, as these materials are most responsible for filter pluggage in the field. The filters were cleaned/regenerated in situ using an aqueous solution of dilute (10% volume) nitric acid. The study found that both filter media were insensitive to high humidity or moisture conditions and were easily cleaned in situ. The filters regenerated to approximately clean filter status even after numerous plugging and cleaning cycles. The filters were leak tested using poly alpha olefin aerosol at the beginning, middle, and end of the

  1. In-situ Investigation of the Fracture Behaviors of 2195-T8 Aluminum-Lithium alloy

    Directory of Open Access Journals (Sweden)

    Wang Liang

    2016-01-01

    Full Text Available In this paper, the tensile crack initiation and propagation behavior of 2195-T8 Aluminum-Lithium alloy was studied by in situ scanning electron microscope observation at room temperature. It was found that cracks initiated at second phases which propagated along the grain boundaries only as T1 phases could retard crack growth inside grains. With further increase of strain, within the grain a large number of slip bands were produced, resulting in the deflection of the grains, which leaded to transgranular fracture at last. SEM examination show both intergranular and transgranular fracture surface morphology indicating that the 2195-T8 alloy revealed a mix mechanism for the fracture.

  2. In Situ Investigations of Li-MoS2 with Planar Batteries

    Energy Technology Data Exchange (ETDEWEB)

    Wan, Jiayu [Univ. of Maryland, College Park, MD (United States). Dept. of Materials Science and Engineering; Bao, Wenzhong [Univ. of Maryland, College Park, MD (United States). Dept. of Materials Science and Engineering and Dept. of Physics; Liu, Yang [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States). Center for Integrated Nanotechnologies (CINT); Dai, Jiaqi [Univ. of Maryland, College Park, MD (United States). Dept. of Materials Science and Engineering; Shen, Fei [Univ. of Maryland, College Park, MD (United States). Dept. of Materials Science and Engineering; Zhou, Lihui [Univ. of Maryland, College Park, MD (United States). Dept. of Materials Science and Engineering; Cai, Xinghan [Univ. of Maryland, College Park, MD (United States). Dept. of Physics; Urban, Daniel [Univ. of Maryland, College Park, MD (United States). Dept. of Materials Science and Engineering; Li, Yuanyuan [Univ. of Maryland, College Park, MD (United States). Dept. of Materials Science and Engineering; Jungjohann, Katherine [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States). Center for Integrated Nanotechnologies (CINT); Fuhrer, Michael S. [Univ. of Maryland, College Park, MD (United States). Dept. of Physics; Monash Univ., Melbourne, VIC (Australia). School of Physics; Hu, Liangbing [Univ. of Maryland, College Park, MD (United States). Dept. of Materials Science and Engineering

    2014-11-25

    For this study, a planar microbattery that enables various in situ measurements of lithiation of 2D materials on the individual-flake scale is developed. A large conductivity increase of thick MoS2 crystallite lithiation due to the formation of a percolative Mo nanoparticle network embedded in a Li2S matrix is observed. The nanoscale study leads to the development of a novel charging strategy for batteries that largely improves the capacity and cycling performance confirmed in bulk MoS2/Li coin cells.

  3. In situ AFM investigation of electrochemically induced surface-initiated atom-transfer radical polymerization.

    Science.gov (United States)

    Li, Bin; Yu, Bo; Zhou, Feng

    2013-02-12

    Electrochemically induced surface-initiated atom-transfer radical polymerization is traced by in situ AFM technology for the first time, which allows visualization of the polymer growth process. It affords a fundamental insight into the surface morphology and growth mechanism simultaneously. Using this technique, the polymerization kinetics of two model monomers were studied, namely the anionic 3-sulfopropyl methacrylate potassium salt (SPMA) and the cationic 2-(metharyloyloxy)ethyltrimethylammonium chloride (METAC). The growth of METAC is significantly improved by screening the ammonium cations by the addition of ionic liquid electrolyte in aqueous solution. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. In-situ investigations of structural changes during cyclic loading by high resolution reciprocal space mapping

    DEFF Research Database (Denmark)

    Diederichs, Annika M.; Thiel, Felix; Lienert, Ulrich

    2017-01-01

    dislocation structures can be identified using advanced electron microscopy and synchrotron techniques. A detailed characterization of the microstructure during cyclic loading by in-situ monitoring the internal structure within individual grains with high energy x-rays can help to understand and predict...... the materials behavior during cyclic deformation and to improve the material design. While monitoring macroscopic stress and strain during cyclic loading, reciprocal space maps of diffraction peaks from single grains are obtained with high resolution. High Resolution Reciprocal Space Mapping was applied...

  5. Novel sample preparation for operando TEM of catalysts.

    Science.gov (United States)

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

    2015-09-01

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

  6. In situ electron backscatter diffraction investigation of recrystallization in a copper wire.

    Science.gov (United States)

    Brisset, François; Helbert, Anne-Laure; Baudin, Thierry

    2013-08-01

    The microstructural evolution of a cold drawn copper wire (reduction area of 38%) during primary recrystallization and grain growth was observed in situ by electron backscatter diffraction. Two thermal treatments were performed, and successive scans were acquired on samples undergoing heating from ambient temperature to a steady state of 200°C or 215°C. During a third in situ annealing, the temperature was continuously increased up to 600°C. Nuclei were observed to grow at the expense of the deformed microstructure. This growth was enhanced by the high stored energy difference between the nuclei and their neighbors (driving energy in recrystallization) and by the presence of high-angle grain boundaries of high mobility. In the early stages of growth, the nuclei twin and the newly created orientations continue to grow to the detriment of the strained copper. At high temperatures, the disappearance of some twins was evidenced by the migration of the incoherent twin boundaries. Thermal grooving of grain boundaries is observed at these high temperatures and affects the high mobile boundaries but tends to preserve the twin boundaries of lower energy. Thus, grooving may contribute to the twin vanishing.

  7. In situ reflectivity investigations of solid/liquid interface during laser backside etching

    International Nuclear Information System (INIS)

    Boehme, R.; Otto, T.; Zimmer, K.

    2006-01-01

    In situ reflectivity measurements of the solid/liquid interface with a pump-probe setup were performed during laser-induced backside wet etching (LIBWE) of fused silica with KrF excimer laser using toluene as absorbing liquid. The intensity, the temporal shape, and the duration of the reflected light measured in dependence on the laser fluence are discussed referring to the surface modification and the bubble formation. The vaporisation of the superheated liquid at the solid interface causes a considerable increase of the reflectivity and gives information about the bubble lifetime. The alterations of the reflectivity after bubbles collapse can be explained with the changed optical properties due to surface modifications of the solid surface. Comparative studies of the reflectivity at different times and the etch rate behaviour in dependence on the laser fluence show that the in situ measured surface modification begins just at the etch threshold fluence and correlates further with etch rate behaviour and the etched surface appearance. The already observed surface modification at LIBWE due to a carbon deposition and structural changes of the near surface region are approved by the changes of the interface reflectivity and emphasizes the importance of the modified surface region in the laser-induced backside wet etching process

  8. In-situ experiments to investigate rock matrix retention properties in ONKALO, Olkiluoto, Finland

    Energy Technology Data Exchange (ETDEWEB)

    Voutilainen, Mikko; Helariutta, Kerttuli [Helsinki Univ. (Finland). Dept. of Chemistry; Poteri, Antti [Technical Research Centre of Finland VTT (Finland); and others

    2015-07-01

    Spent nuclear fuel from nuclear power plants, owned by TVO (Teollisuuden Voima Oy) and Fortum, is planned to be disposed to a repository at a depth of more than 400 meters in the bedrock of Olkiluoto (Eurajoki, Finland). The repository system of multiple release barriers consists of both manmade and natural barriers. The surrounding rock acts as the last barrier if other barriers fail during passage of the millennia. Therefore, safe disposal of spent nuclear fuel requires information on the radionuclide transport and retention properties within the porous and water-containing rock matrix along the water conducting flow paths. To this end, various types of experiments are being performed and planned within ONKALO, the underground rock characterization facility in Olkiluoto, as part of the project @''rock matrix REtention PROperties'' (REPRO). The research site is located at a depth of 420 meters close to the repository site. The aim is to study the diffusion and sorption properties of nuclear compounds in the rock matrix under real in-situ conditions. The first in-situ experiment was performed during 2012 using HTO, Na-22, Cl-36 and I-125 as tracer nuclides. Breakthrough curves show retention and asymptotic behavior that are in-line with those caused by matrix diffusion and sorption were observed in their breakthrough curves. Weak sorption was also observed in the breakthrough curves of Na-22 and I-125.

  9. Electrochemical activation of Li2MnO3 at elevated temperature investigated by in situ Raman microscopy

    International Nuclear Information System (INIS)

    Lanz, Patrick; Villevieille, Claire; Novák, Petr

    2013-01-01

    Layered-layered oxides of the type xLi 2 MnO 3 ·(1 − x)LiMO 2 (M = Mn, Ni, Co) have been postulated to contain Li 2 MnO 3 domains which, upon electrochemical activation, give rise to a characteristic potential plateau at 4.5 V vs. Li + /Li. To improve our understanding of the complex reaction mechanisms at play, we applied in situ Raman microscopy to investigate the constituent Li 2 MnO 3 . Li 2 MnO 3 synthesised via a two-step solid-state reaction was characterised by scanning electron microscopy and X-ray diffraction. Preliminary electrochemical tests and ex situ Raman microscopy showed the need for elevated temperatures to achieve activation. For the first time, in situ Raman microscopy (at 50 °C) confirmed the activation of Li 2 MnO 3 . The main signal at 615 cm −1 shifted to higher wavenumbers upon charging. After reaching 4.4 V vs. Li + /Li, this shift grew significantly, which is in good agreement with the onset of the potential plateau in both Li 2 MnO 3 and xLi 2 MnO 3 ·(1 − x)LiMO 2 , and is assigned to the partial formation of a spinel-like phase

  10. In situ QCM and TM-AFM investigations of the early stages of degradation of silver and copper surfaces

    International Nuclear Information System (INIS)

    Kleber, Ch.; Hilfrich, U.; Schreiner, M.

    2007-01-01

    The early stages of atmospheric corrosion of pure copper and pure silver specimens were investigated performing in situ tapping mode atomic force microscopy (TM-AFM), in situ quartz crystal microbalance (QCM) and X-ray photoelectron spectroscopy (XPS). The information obtained by TM-AFM is the change of the topography of the sample surfaces with emphasis on the shape and lateral distribution of the corrosion products grown within the first hours of weathering. The simultaneously performed in situ QCM measurements are indicating the mass changes due to possibly occurring corrosive processes on the surface during weathering and are therefore a valuable tool for the determination of corrosion rates. Investigations were carried out in synthetic air at different levels of relative humidity (RH) with and without addition of 250 ppb SO 2 as acidifying agent. On a polished copper surface the growth of corrosion products could be observed by TM-AFM analysis at 60% RH without any addition of acidifying gases [M. Wadsak, M. Schreiner, T. Aastrup, C. Leygraf, Surf. Sci. 454-456 (2000) 246-250]. On a weathered copper surface the addition of SO 2 to the moist air stream leads to the formation of additional features as already described in the literature [M. Wadsak, M. Schreiner, T. Aastrup, C. Leygraf, Surf. Sci. 454-456 (2000) 246-250; Ch. Kleber, J. Weissenrieder, M. Schreiner, C. Leygraf, Appl. Surf. Sci. 193 (2002) 245-253]. Exposing a silver specimen to humidity leads to the degradation of the surface structure as well as to a formation of corrosion products, which could be detected by in situ QCM measurements. After addition of 250 ppb SO 2 to the moist gas stream an increase of the formed feature's volume on the silver surface could be observed by TM-AFM measurements. The results obtained additionally from the in situ QCM measurements confirm the influence of SO 2 due to a further increase of the mass of the formed corrosion layer (and therefore an increase of the

  11. Application of TEM to highly reactive metals

    International Nuclear Information System (INIS)

    Sherry, W.M.; Prinz, F.

    1982-01-01

    In the following a method for the preparation and observation of sodium TEM specimens and the first TEM micrograph ever to be published on the dislocation microstructure of sodium are reported. (orig./IHOE) [de

  12. Ex situ investigation of the step bunching on crystal surfaces by atomic force microscopy

    Science.gov (United States)

    Krasinski, Mariusz J.

    1997-07-01

    We are describing ex situ observation of step bunching on the surfaces of solution grown potassium dihydrogen phosphate (KDP) and sodium chlorate monocrystals. The measurements have been done with the use of atomic force microscope. The use of this equipment allowed us to see directly the structure of macrosteps. Observation confirmed the existence of step pinning which is one of the proposed mechanisms of step bunching. Despite the very high resolution of AFM it was not possible to determine the nature of pinning point. The monatomic steps on KDP and sodium chlorate crystal surfaces are mainly one unit cell high what seems to be the result of the steps pairing. The origin of observed step pattern is discussed in frames of existing theories.

  13. In Situ FTIR and NMR Spectroscopic Investigations on Ruthenium-Based Catalysts for Alkene Hydroformylation.

    Science.gov (United States)

    Kubis, Christoph; Profir, Irina; Fleischer, Ivana; Baumann, Wolfgang; Selent, Detlef; Fischer, Christine; Spannenberg, Anke; Ludwig, Ralf; Hess, Dieter; Franke, Robert; Börner, Armin

    2016-02-18

    Homogeneous ruthenium complexes modified by imidazole-substituted monophosphines as catalysts for various highly efficient hydroformylation reactions were characterized by in situ IR spectroscopy under reaction conditions and NMR spectroscopy. A proper protocol for the preformation reaction from [Ru3 (CO)12] is decisive to prevent the formation of inactive ligand-modified polynuclear complexes. During catalysis, ligand-modified mononuclear ruthenium(0) carbonyls were detected as resting states. Changes in the ligand structure have a crucial impact on the coordination behavior of the ligand and consequently on the catalytic performance. The substitution of CO by a nitrogen atom of the imidazolyl moiety in the ligand is not a general feature, but it takes place when structural prerequisites of the ligand are fulfilled. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Investigation and in situ removal of spatter generated during laser ablation of aluminium composites

    International Nuclear Information System (INIS)

    Popescu, A.C.; Delval, C.; Shadman, S.; Leparoux, M.

    2016-01-01

    Highlights: • Study of spatter generated during laser irradiation of an aluminium nanocomposite. • Number of droplets was 1.5–3 times higher for laser in depth vs surface focused beams. • High speed imaging revealed particles exploding in flight similar to a fireworks effect. • Three methods were selected for droplets removal in situ and the results are analyzed. - Abstract: Spatter generated during laser irradiation of an aluminium alloy nanocomposite (AlMg5 reinforced with Al_2O_3 nanoparticles) was monitored by high speed imaging. Droplets trajectory and speed were assessed by computerized image analysis. The effects of laser peak power and laser focusing on the plume expansion and expulsed droplet speeds were studied in air or under argon flow. It was found that the velocity of visible droplets expulsed laterally or at the end of the plume emission from the metal surface was not dependent on the plasma plume speed. The neighbouring area of irradiation sites was studied by optical and scanning electron microscopy. Droplets deposited on the surface were classified according to their size and counted using a digital image processing software. It was observed that the number of droplets on surface was 1.5–3 times higher when the laser beam was focused in depth as compared to focused beams, even though the populations average diameter were comparable. Three methods were selected for removing droplets in situ, during plume expansion: an argon gas jet crossing the plasma plume, a fused silica plate collector transparent to the laser wavelength placed parallel to the irradiated surface and a mask placed onto the aluminium composite surface. The argon gas jet was efficient only for low power irradiation conditions, the fused silica plate failed in all tested conditions and the mask was successful for all irradiation regimes.

  15. In Situ Investigation of Electrochemically Mediated Surface-Initiated Atom Transfer Radical Polymerization by Electrochemical Surface Plasmon Resonance.

    Science.gov (United States)

    Chen, Daqun; Hu, Weihua

    2017-04-18

    Electrochemically mediated atom transfer radical polymerization (eATRP) initiates/controls the controlled/living ATRP chain propagation process by electrochemically generating (regenerating) the activator (lower-oxidation-state metal complex) from deactivator (higher-oxidation-state metal complex). Despite successful demonstrations in both of the homogeneous polymerization and heterogeneous systems (namely, surface-initiated ATRP, SI-ATRP), the eATRP process itself has never been in situ investigated, and important information regarding this process remains unrevealed. In this work, we report the first investigation of the electrochemically mediated SI-ATRP (eSI-ATRP) by rationally combining the electrochemical technique with real-time surface plasmon resonance (SPR). In the experiment, the potential of a SPR gold chip modified by the self-assembled monolayer of the ATRP initiator was controlled to electrochemically reduce the deactivator to activator to initiate the SI-ATRP, and the whole process was simultaneously monitored by SPR with a high time resolution of 0.1 s. It is found that it is feasible to electrochemically trigger/control the SI-ATRP and the polymerization rate is correlated to the potential applied to the gold chip. This work reveals important kinetic information for eSI-ATRP and offers a powerful platform for in situ investigation of such complicated processes.

  16. 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

  17. In-situ investigations of corrosion processes on glass and metal surfaces by scanning probe microscopy (SPM)

    International Nuclear Information System (INIS)

    Nicolussi-Leck, G.

    1996-09-01

    The corrosion of potash-lime-silica glass was observed in-situ by AFM (atomic force microscopy) for the first time. The topographic changes with time due to the interaction of a replica glass with the ambient atmosphere were studied. A comparison of dynamic mode AFM and static mode AFM has demonstrated their potential for the investigation of soft, sensitive specimens. A combination of both methods yielded a correlation between structural changes during the corrosion process and different corrosion products on glass. The activation of surface reactions by the tip touching the surface could be observed with dynamic mode AFM. In-situ sample preparation and introduction of a defined atmosphere consisting of nitrogen with adjustable amounts of relative humidity and varying contents of SO 2 and NO 2 allowed model studies of the atmospheric corrosion. A replica glass with medieval composition was used in order to investigate the impact of the above described conditions. Besides the influence of the relative humidity the effects of SO 2 and NO 2 as well as their, synergistic effects could be studied. The evaluation of the phase signal in dynamic mode AFM in addition to the topographic information allowed the identification of humid domains in and on corrosion products, respectively. The observed contrast and thus the adhesion forces, are mainly related to the different water coverage of the surface regions or the hydroscopic properties, respectively. Furthermore, the topographic changes of copper-nickel, and palladium surfaces exposed to humidified nitrogen with SO 2 have been observed in-situ. Contrary to the assumption of the metal surfaces being covered by a homogeneous layer of corrosion products, distinct clusters of products could be observed. In case of different kinds of products these clusters were arranged adjacent to each other rather than in different stacked layers. (author)

  18. VICI (Venus In Situ Composition Investigations): The Next Step in Understanding Venus Climate Evolution

    Science.gov (United States)

    Glaze, L. S.; Garvin, J. B.

    2017-12-01

    Venus provides a natural laboratory to explore an example of terrestrial planet evolution that may be cosmically ubiquitous. By better understanding the composition of the Venus atmosphere and surface, we can better constrain the efficiency of the Venusian greenhouse. VICI is a proposed NASA New Frontiers mission that delivers two landers to Venus on two separate Venus fly-bys. Following six orbital remote sensing missions to Venus (since 1978), VICI would be the first mission to land on the Venus surface since 1985, and the first U.S. mission to enter the Venus atmosphere in 49 years. The four major VICI science objectives are: Atmospheric origin and evolution: Understand the origin of the Venus atmosphere, how it has evolved, including how recently Venus lost its oceans, and how and why it is different from the atmospheres of Earth and Mars, through in situ measurements of key noble gases, nitrogen, and hydrogen. Atmospheric composition and structure: Reveal the unknown chemical processes and structure in Venus' deepest atmosphere that dominate the current climate through two comprehensive, in situ vertical profiles. Surface properties and geologic evolution: For the first time ever, explore the tessera from the surface, specifically to test hypotheses of ancient content-building cycles, erosion, and links to past climates using multi-point mineralogy, elemental chemistry, imaging and topography. Surface-atmosphere interactions: Characterize Venus' surface weathering environment and provide insight into the sulfur cycle at the surface-atmosphere interface by integrating rich atmospheric composition and structure datasets with imaging, surface mineralogy, and elemental rock composition. VICI is designed to study Venus' climate history through detailed atmospheric composition measurements not possible on earlier missions. In addition, VICI images the tessera surface during descent enabling detailed topography to be generated. Finally, VICI makes multiple elemental

  19. Time-Dependent Damage Investigation of Rock Mass in an In Situ Experimental Tunnel

    Science.gov (United States)

    Jiang, Quan; Cui, Jie; Chen, Jing

    2012-01-01

    In underground tunnels or caverns, time-dependent deformation or failure of rock mass, such as extending cracks, gradual rock falls, etc., are a costly irritant and a major safety concern if the time-dependent damage of surrounding rock is serious. To understand the damage evolution of rock mass in underground engineering, an in situ experimental testing was carried out in a large belowground tunnel with a scale of 28.5 m in width, 21 m in height and 352 m in length. The time-dependent damage of rock mass was detected in succession by an ultrasonic wave test after excavation. The testing results showed that the time-dependent damage of rock mass could last a long time, i.e., nearly 30 days. Regression analysis of damage factors defined by wave velocity, resulted in the time-dependent evolutional damage equation of rock mass, which corresponded with logarithmic format. A damage viscoelastic-plastic model was developed to describe the exposed time-dependent deterioration of rock mass by field test, such as convergence of time-dependent damage, deterioration of elastic modules and logarithmic format of damage factor. Furthermore, the remedial measures for damaged surrounding rock were discussed based on the measured results and the conception of damage compensation, which provides new clues for underground engineering design.

  20. In situ ellipsometric investigation of stainless steel corrosion behavior in buffered solutions with amino acids

    International Nuclear Information System (INIS)

    Vinnichenko, M.V.; Pham, M.T.; Chevolleau, T.; Poperenko, L.V.; Maitz, M.F.

    2003-01-01

    The corrosion of metals is associated both with a release of ions and changes in optical surface properties. In this study, these two effects were correlated by a potentiodynamic corrosion test and in situ probing of the surface by ellipsometry. The studies were carried out with stainless steel (SS) AISI 304 and 316 in phosphate buffered saline (PBS) and in Dulbecco's modified minimal essential medium (DMEM) at pH 7.4. In both media, 304 steel is more susceptible to corrosion than 316 grade. The 316 steel shows a higher corrosion potential and higher corrosion current density in PBS than in DMEM, for 304 steel this behavior is vice versa. Ellipsometry demonstrated a higher sensitivity than potentiodynamics to surface modification in the cathodic area. In DMEM the removal of a surface layer at negative potential and a further repassivation with increasing potential was characteristic. In PBS a surface layer started to grow immediately. X-ray photoelectron spectra of this layer formed in PBS are consistent with iron phosphate. Its formation is inhibited in DMEM; the presence of amino acids is discussed as the reason

  1. Investigating the Trimethylaluminium/Water ALD Process on Mesoporous Silica by In Situ Gravimetric Monitoring

    Directory of Open Access Journals (Sweden)

    Verena E. Strempel

    2018-05-01

    Full Text Available A low amount of AlOx was successfully deposited on an unordered, mesoporous SiO2 powder using 1–3 ALD (Atomic Layer Deposition cycles of trimethylaluminium and water. The process was realized in a self-built ALD setup featuring a microbalanceand a fixed particle bed. The reactor temperature was varied between 75, 120, and 200 °C. The self-limiting nature of the deposition was verified by in situ gravimetric monitoring for all temperatures. The coated material was further analyzed by nitrogen sorption, inductively coupled plasma-optical emission spectroscopy, powder X-ray diffraction, high-resolution transmission electron microscopy, attenuated total reflection Fourier transformed infrared spectroscopy, and elemental analysis. The obtained mass gains correspond to average growth between 0.81–1.10 Å/cycle depending on substrate temperature. In addition, the different mass gains during the half-cycles in combination with the analyzed aluminum content after one, two, and three cycles indicate a change in the preferred surface reaction of the trimethylaluminium molecule from a predominately two-ligand exchange with hydroxyl groups to more single-ligand exchange with increasing cycle number. Nitrogen sorption isotherms demonstrate (1 homogeneously coated mesopores, (2 a decrease in surface area, and (3 a reduction of the pore size. The experiment is successfully repeated in a scale-up using a ten times higher substrate batch size.

  2. Regulation of ETG turbulence by TEM driven zonal flows

    Science.gov (United States)

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

    2013-10-01

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

  3. In-situ investigation of thermal instabilities and solid state dewetting in polycrystalline platinum thin films via confocal laser microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Jahangir, S.; Cheng, Xuan; Huang, H. H.; Nagarajan, V. [School of Materials Science and Engineering, University of New South Wales, Sydney 2052 (Australia); Ihlefeld, J. [Electronic, Optical, and Nanomaterials Department, Sandia National Laboratories, Albuquerque, New Mexico 87185 (United States)

    2014-10-28

    Solid state dewetting and the subsequent morphological changes for platinum thin films grown on zinc oxide (ZnO) buffered (001) silicon substrates (Pt/ZnO/SiO{sub 2}/(001)Si system) is investigated under vacuum conditions via a custom-designed confocal laser microscope coupled with a laser heating system. Live imaging of thin film dewetting under a range of heating and quenching vacuum ambients reveals events including hillock formation, hole formation, and hole growth that lead to formation of a network of Pt ligaments, break up of Pt ligaments to individual islands and subsequent Pt islands shape reformation, in chronological fashion. These findings are corroborated by ex-situ materials characterization and quantitative electron microscopy analysis. A secondary hole formation via blistering before film rupture is revealed to be the critical stage, after which a rapid dewetting catastrophe occurs. This process is instantaneous and cannot be captured by ex-situ methods. Finally, an intermetallic phase forms at 900 °C and alters the morphology of Pt islands, suggesting a practical limit to the thermal environments that may be used for these platinized silicon wafers in vacuum conditions.

  4. In-situ investigation of thermal instabilities and solid state dewetting in polycrystalline platinum thin films via confocal laser microscopy

    International Nuclear Information System (INIS)

    Jahangir, S.; Cheng, Xuan; Huang, H. H.; Nagarajan, V.; Ihlefeld, J.

    2014-01-01

    Solid state dewetting and the subsequent morphological changes for platinum thin films grown on zinc oxide (ZnO) buffered (001) silicon substrates (Pt/ZnO/SiO 2 /(001)Si system) is investigated under vacuum conditions via a custom-designed confocal laser microscope coupled with a laser heating system. Live imaging of thin film dewetting under a range of heating and quenching vacuum ambients reveals events including hillock formation, hole formation, and hole growth that lead to formation of a network of Pt ligaments, break up of Pt ligaments to individual islands and subsequent Pt islands shape reformation, in chronological fashion. These findings are corroborated by ex-situ materials characterization and quantitative electron microscopy analysis. A secondary hole formation via blistering before film rupture is revealed to be the critical stage, after which a rapid dewetting catastrophe occurs. This process is instantaneous and cannot be captured by ex-situ methods. Finally, an intermetallic phase forms at 900 °C and alters the morphology of Pt islands, suggesting a practical limit to the thermal environments that may be used for these platinized silicon wafers in vacuum conditions.

  5. Interface Energy Alignment of Atomic-Layer-Deposited VOx on Pentacene: an in Situ Photoelectron Spectroscopy Investigation.

    Science.gov (United States)

    Zhao, Ran; Gao, Yuanhong; Guo, Zheng; Su, Yantao; Wang, Xinwei

    2017-01-18

    Ultrathin atomic-layer-deposited (ALD) vanadium oxide (VO x ) interlayer has recently been demonstrated for remarkably reducing the contact resistance in organic electronic devices (Adv. Funct. Mater. 2016, 26, 4456). Herein, we present an in situ photoelectron spectroscopy investigation (including X-ray and ultraviolet photoelectron spectroscopies) of ALD VO x grown on pentacene to understand the role of the ALD VO x interlayer for the improved contact resistance. The in situ photoelectron spectroscopy characterizations allow us to monitor the ALD growth process of VO x and trace the evolutions of the work function, pentacene HOMO level, and VO x defect states during the growth. The initial VO x growth is found to be partially delayed on pentacene in the first ∼20 ALD cycles. The underneath pentacene layer is largely intact after ALD. The ALD VO x is found to contain a high density of defect states starting from 0.67 eV below the Fermi level, and the energy level of these defect states is in excellent alignment with the HOMO level of pentacene, which therefore allows these VO x defect states to provide an efficient hole-injection pathway at the contact interface.

  6. Hydrogen Absorption in Metal Thin Films and Heterostructures Investigated in Situ with Neutron and X-ray Scattering

    Directory of Open Access Journals (Sweden)

    Sara J. Callori

    2016-05-01

    Full Text Available Due to hydrogen possessing a relatively large neutron scattering length, hydrogen absorption and desorption behaviors in metal thin films can straightforwardly be investigated by neutron reflectometry. However, to further elucidate the chemical structure of the hydrogen absorbing materials, complementary techniques such as high resolution X-ray reflectometry and diffraction remain important too. Examples of work on such systems include Nb- and Pd-based multilayers, where Nb and Pd both have strong affinity to hydrogen. W/Nb and Fe/Nb multilayers were measured in situ with unpolarized and polarized neutron reflectometry under hydrogen gas charging conditions. The gas-pressure/hydrogen-concentration dependence, the hydrogen-induced macroscopic film swelling as well as the increase in crystal lattice plane distances of the films were determined. Ferromagnetic-Co/Pd multilayers were studied with polarized neutron reflectometry and in situ ferromagnetic resonance measurements to understand the effect of hydrogen absorption on the magnetic properties of the system. This electronic effect enables a novel approach for hydrogen sensing using a magnetic readout scheme.

  7. Investigating phase behavior and structural changes in NiO/Ni-YSZ composite with monochromatic in-situ 2D and static 3D neutron imaging

    DEFF Research Database (Denmark)

    Makowska, Malgorzata G.; Strobl, Markus; Kardjilov, Nikolay

    2017-01-01

    oxide fuel cells, and for cathodes in solid oxide electrolysis cells). Results of in-situ 2D and ex-situ 3D measurements are presented. In-situ observation of phase transition between NiO and Ni were performed at the test Beamline for neutron Optics and other Applications (BOA) at the continuous neutron...... and post mortem tomography provides complementary information about the reduction/oxidation degree and e.g. crack evolution in the investigated system and it is therefore possible to acquire information about the rate of chemical reactions and spatial evolution of phases and morphological features....

  8. Environmental TEM for Materials Research

    DEFF Research Database (Denmark)

    Hansen, Thomas Willum

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

  9. Environmental TEM in Materials Research

    DEFF Research Database (Denmark)

    Hansen, Thomas Willum; Wagner, Jakob Birkedal

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

  10. In-situ X-ray diffraction : a useful tool to investigate hydride-formation reactions

    NARCIS (Netherlands)

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

    1994-01-01

    A high-pressure X-ray diffraction (XRD) cell has been designed which allowed us to study simultaneously hydrogen absorption/desorption isotherms and XRD powder diffraction patterns on (de)hydrided intermetallic compounds. The hydride formation reaction was investigated in the case of LaNi5 under

  11. Non-invasive in-situ investigations versus micro-sampling: a comparative study on a Renoirs painting

    International Nuclear Information System (INIS)

    Miliani, C.; Sgamellotti, A.; Universita degli Studi di Perugia . Centro di Eccellenza SMAArt; Scientific Methodologies applied to Archaeology and Art)

    2007-01-01

    In this paper, a multi-technique in-situ non-invasive approach has been followed for the study of the materials used for a painting by Pierre-Auguste Renoir, ''A woman at her toilette''. The study was carried out using five portable spectroscopic techniques, namely X-ray fluorescence, mid-infrared reflectance spectroscopy, near infrared reflectance spectroscopy, and UV-Vis spectroscopy in absorption and emission. The painting was selected as a case study because it was examined in advance of the current investigation using conventional micro-sampling techniques. This provided the opportunity to evaluate potential and limitations of the non-invasive approach to the complex case of the modern painting. (orig.)

  12. In situ grazing incidence small-angle X-ray scattering investigation of polystyrene nanoparticle spray deposition onto silicon.

    Science.gov (United States)

    Herzog, Gerd; Benecke, Gunthard; Buffet, Adeline; Heidmann, Berit; Perlich, Jan; Risch, Johannes F H; Santoro, Gonzalo; Schwartzkopf, Matthias; Yu, Shun; Wurth, Wilfried; Roth, Stephan V

    2013-09-10

    We investigated the spray deposition and subsequent self-assembly during drying of a polystyrene nanoparticle dispersion with in situ grazing incidence small-angle X-ray scattering at high time resolution. During the fast deposition of the dispersion and the subsequent evaporation of the solvent, different transient stages of nanoparticle assembly can be identified. In the first stage, the solvent starts to evaporate without ordering of the nanoparticles. During the second stage, large-scale structures imposed by the breakup of the liquid film are observable. In this stage, the solvent evaporates further and nanoparticle ordering starts. In the late third drying stage, the nanoparticles self-assemble into the final layer structure.

  13. 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

  14. 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.

  15. 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.

  16. Investigating Forest Harvest Effects on DOC Concentration and Quality: An In Situ, High Resolution Approach to Quantifying DOC Export Dynamics

    Science.gov (United States)

    Jollymore, A. J.; Johnson, M. S.; Hawthorne, I.

    2013-12-01

    Justification: Forest harvest effects on water quality can signal alterations in hydrologic and ecologic processes incurred as a result of forest harvest activities. Organic matter (OM), specifically dissolved organic carbon (DOC), plays a number of important roles mediating UV-light penetration, redox reactivity and microbial activity within aquatic ecosystems. Quantification of DOC is typically pursued via grab sampling followed by chemical or spectrophotometric analysis, limiting the temporal resolution obtained as well as the accuracy of export calculations. The advent of field-deployable sensors capable of measuring DOC concentration and certain quality characteristics in situ provides the ability to observe dynamics at temporal scales necessary for accurate calculation of DOC flux, as well as the observation of dynamic changes in DOC quality on timescales impossible to observe through grab sampling. Methods: This study utilizes a field deployable UV-Vis spectrophotometer (spectro::lyzer, s::can, Austria) to investigate how forest harvest affects DOC export. The sensor was installed at an existing hydrologic monitoring site at the outlet of a headwater stream draining a small (91 hectare) second growth Douglasfir-dominated catchment near Campbell River on Vancouver Island, British Columbia. Measurement began late in 2009, prior to forest harvest and associated activities such as road building (which commenced in October 2010 and ended in early 2011), and continues to present. During this time - encompassing the pre, during and post-harvest conditions - the absorbance spectrum of stream water from 200 to 750 nm was measured. DOC concentration and spectroscopic indices related to DOC quality (including SUVA, which relates to the concentration of aromatic carbon, and spectral slope) were subsequently calculated for each spectra obtained at 30-minute intervals. Results and conclusions: High frequency measurements of DOC show that overall export of OM increased in

  17. In situ investigation of wet chemical processes for chalcopyrite solar cells by L-edge XAS under ambient conditions

    Energy Technology Data Exchange (ETDEWEB)

    Greil, Stefanie M. [Helmholtz-Zentrum Berlin fuer Materialien und Energie, Albert-Einstein-Strasse 15, 12489 Berlin (Germany); Lauermann, Iver, E-mail: Iver.lauermann@helmholtz-berlin.d [Helmholtz-Zentrum Berlin fuer Materialien und Energie, Albert-Einstein-Strasse 15, 12489 Berlin (Germany); Ennaoui, Ahmed; Kropp, Timo; Lange, Kathrin M.; Weber, Matthieu [Helmholtz-Zentrum Berlin fuer Materialien und Energie, Albert-Einstein-Strasse 15, 12489 Berlin (Germany); Aziz, Emad F., E-mail: Emad.Aziz@helmholtz-berlin.d [Helmholtz-Zentrum Berlin fuer Materialien und Energie, Albert-Einstein-Strasse 15, 12489 Berlin (Germany)

    2010-02-15

    Two instrumental setups for in situ soft X-ray absorption spectroscopy in liquid systems are demonstrated in this work. One for investigating chemical reactions in solutions and a new one for the solid component of a liquid / (as in both / absorber) solid interface. We used these setups for investigating two production processes for chalcopyrite solar cells under ambient conditions, probing the L-edge of Zn and Cu. The first one is a flow cell with a silicon nitride membrane to study the chemical bath deposition process for Cd-free buffer layers. Examining the electronic structure of involved Zn complexes allows to determine the exact reaction mechanism taking place during this process. The second setup is a rotating disk for investigating the bath/absorber interface upon the etching process of superficial binary copper compounds of the absorber as a function of time. The time resolution of the chemical reaction demonstrated in this study ranges from the second to minute time scale.

  18. In situ investigation of wet chemical processes for chalcopyrite solar cells by L-edge XAS under ambient conditions

    International Nuclear Information System (INIS)

    Greil, Stefanie M.; Lauermann, Iver; Ennaoui, Ahmed; Kropp, Timo; Lange, Kathrin M.; Weber, Matthieu; Aziz, Emad F.

    2010-01-01

    Two instrumental setups for in situ soft X-ray absorption spectroscopy in liquid systems are demonstrated in this work. One for investigating chemical reactions in solutions and a new one for the solid component of a liquid / (as in both / absorber) solid interface. We used these setups for investigating two production processes for chalcopyrite solar cells under ambient conditions, probing the L-edge of Zn and Cu. The first one is a flow cell with a silicon nitride membrane to study the chemical bath deposition process for Cd-free buffer layers. Examining the electronic structure of involved Zn complexes allows to determine the exact reaction mechanism taking place during this process. The second setup is a rotating disk for investigating the bath/absorber interface upon the etching process of superficial binary copper compounds of the absorber as a function of time. The time resolution of the chemical reaction demonstrated in this study ranges from the second to minute time scale.

  19. In situ investigation of wet chemical processes for chalcopyrite solar cells by L-edge XAS under ambient conditions

    Science.gov (United States)

    Greil, Stefanie M.; Lauermann, Iver; Ennaoui, Ahmed; Kropp, Timo; Lange, Kathrin M.; Weber, Matthieu; Aziz, Emad F.

    2010-02-01

    Two instrumental setups for in situ soft X-ray absorption spectroscopy in liquid systems are demonstrated in this work. One for investigating chemical reactions in solutions and a new one for the solid component of a liquid / (as in both / absorber) solid interface. We used these setups for investigating two production processes for chalcopyrite solar cells under ambient conditions, probing the L-edge of Zn and Cu. The first one is a flow cell with a silicon nitride membrane to study the chemical bath deposition process for Cd-free buffer layers. Examining the electronic structure of involved Zn complexes allows to determine the exact reaction mechanism taking place during this process. The second setup is a rotating disk for investigating the bath/absorber interface upon the etching process of superficial binary copper compounds of the absorber as a function of time. The time resolution of the chemical reaction demonstrated in this study ranges from the second to minute time scale.

  20. In situ high-frequency UV-Vis spectrometer probes for investigating runoff processes and end member stability.

    Science.gov (United States)

    Schwab, Michael; Weiler, Markus; Pfister, Laurent; Klaus, Julian

    2014-05-01

    In recent years, several limitations as to the application of end member mixing analysis with isotope and geochemical tracers have been revealed: unstable end member solutions, inputs varying in space and time, and unrealistic mixing assumptions. In addition, the necessary high-frequency sampling using conventional methods is time and resources consuming, and hence most sampling rates are not suitable for capturing the response times of the majority of observed headwater catchments. However, high-frequency observations are considered fundamental for gaining new insights into hydrological systems. In our study, we have used two portable, in situ, high-frequency UV-Vis spectrometers (spectro::lyser; scan Messtechnik GmbH) to investigate the variability of several signatures in streamflow and end member stability. The spectro::lyser measures TOC, DOC, nitrate and the light absorption spectrum from 220 to 720 nm with 2.5 nm increment. The Weierbach catchment (0.45 km2) in the Attert basin (297 km2) in Luxemburg is a small headwater research catchment (operated by the CRP Gabriel Lippmann), which is completely forested and underlain by schist bedrock. The catchment is equipped with a dense network of hydrological instruments and for this study, the outlet of the Weierbach catchment was equipped with one spectro::lyser, permanently sensing stream water at a 15 minutes time step over several months. Hydrometric and meteorologic data was compared with the high-frequency spectro::lyser time series of TOC, DOC, nitrate and the light absorption spectrum, to get a first insight into the behaviour of the catchment under different environmental conditions. As a preliminary step for a successful end member mixing analysis, the stability of rainfall, soil water, and groundwater was tested with one spectro::lyser, both temporally and spatially. Thereby, we focused on the investigation of changes and patterns of the light absorption spectrum of the different end members and the

  1. Electrochemical and spectroscopic in situ techniques for the investigation of the phosphating of zinc coated steel

    International Nuclear Information System (INIS)

    Tomandl, A.

    2003-05-01

    In this work spectroscopic and electrochemical techniques were developed for the investigation of surface treatments used in steel industry. ICP-atomic emission spectroscopy (ICP-AES), Raman spectroscopy and the Quartz crystal microbalance (QCM) were applied to the investigation of the kinetics of phosphating as well as the properties of phosphate layers. Phosphating of zinc coated steel leads to the formation of a crystalline layer consisting of zinc phosphate and is employed to enhance paint adhesion and corrosion protection. For the high reaction rates necessary in industrial production lines, oxidation agents are added to the phosphating bathes to accelerate the reaction. The oxidation agents provide an additional reduction reaction beside the hydrogen formation and therefore decrease the number of gas bubbles, which would block the zinc surface and reduce the rate of phosphating. With addition of H2O2 or nitrates the rate of layer formation is distinctly increased. In a combined experiment of ICP-AES with QCM and potential transients, it was shown that the presence of these accelerators in the phosphating bath increases the rate of zinc dissolution and hence leads to a faster formation of the phosphate layer. In under paint corrosion of painted, zinc coated steel phosphate layers are exposed to a highly alkaline environment. The stability of a phosphate layer against alkaline attack is therefore essential for its performance in corrosion protection. To enhance the alkaline stability Mn and Ni are added to modern phosphating bathes. The incorporation of these elements reduces the dissolution rate in 0.1 M NaOH proportional to their concentration in the phosphate layer. The dissolution of Zn, P, Mn and Ni was determined quantitatively with ICP-AES. Raman spectroscopy showed the formation of a Mn-hydroxide layer during alkaline attack, which protects the phosphate layer and reduces further dissolution. On basis of these results the reaction of phosphate layers

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

    International Nuclear Information System (INIS)

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

    2002-01-01

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

  3. 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.

  4. In Situ Strategy of the 2011 Mars Science Laboratory to Investigate the Habitability of Ancient Mars

    Science.gov (United States)

    Mahaffy, Paul R.

    2011-01-01

    The ten science investigations of the 2011 Mars Science Laboratory (MSL) Rover named "Curiosity" seek to provide a quantitative assessment of habitability through chemical and geological measurements from a highly capable robotic' platform. This mission seeks to understand if the conditions for life on ancient Mars are preserved in the near-surface geochemical record. These substantial payload resources enabled by MSL's new entry descent and landing (EDL) system have allowed the inclusion of instrument types nevv to the Mars surface including those that can accept delivered sample from rocks and soils and perform a wide range of chemical, isotopic, and mineralogical analyses. The Chemistry and Mineralogy (CheMin) experiment that is located in the interior of the rover is a powder x-ray Diffraction (XRD) and X-ray Fluorescence (XRF) instrument that provides elemental and mineralogical information. The Sample Analysis at Mars (SAM) suite of instruments complements this experiment by analyzing the volatile component of identically processed samples and by analyzing atmospheric composition. Other MSL payload tools such as the Mast Camera (Mastcam) and the Chemistry & Camera (ChemCam) instruments are utilized to identify targets for interrogation first by the arm tools and subsequent ingestion into SAM and CheMin using the Sample Acquisition, Processing, and Handling (SA/SPaH) subsystem. The arm tools include the Mars Hand Lens Imager (MAHLI) and the Chemistry and Alpha Particle X-ray Spectrometer (APXX). The Dynamic Albedo of Neutrons (DAN) instrument provides subsurface identification of hydrogen such as that contained in hydrated minerals

  5. Areas and limits of employment of portable EDXRF equipment for in situ investigations

    International Nuclear Information System (INIS)

    Gigante, G.E.; Ricciardi, P.; Ridolfi, St.

    2005-01-01

    The use of mobile spectrometers in the archaeo-metric study of ancient artefacts has become a very common practice over the past few years. It does open methodological questions on the employment of such techniques in a non-destructive manner, i.e. avoiding the damage of the artifact. Some additional methodological questions come by (i) the use of such instrumentation for diagnostic scopes (in which a different approach to the measurement is required) and (ii) the use of the spectrometers in systematic analysis on big number of artefacts, stored in several museums (during experimental campaigns). This paper's aim is to discuss some of this questions, on the basis of the experience in the use of mobile (or Field Portable) systems for Energy Dispersive X-ray Fluorescence (EDXRF) spectroscopy that we have harvested in the last years. Our conclusions mainly regard the precision of measures, which is related both to the positioning of the spectrometer and to the instrument's instability. Also we deal with the more complex problem of the object's matrix not being homogeneous and of how this can affect the response of the measuring system. Moreover, it is discussed the more general question of the use of portable spectrometers and, consequently, of the meaning one can give to the results so obtained. As a matter of fact the use of such systems, which have an intrinsic analytic potential, in a non-destructive manner, frequently creates ambiguities that have not been, sometimes, taken into account with attention by the investigators. Finally some ideas are traced on the development of methodologies which favor a better use of such spectroscopic systems for the analysis of ancient artefacts. (authors)

  6. Interdiffusion in nanometer-scale multilayers investigated by in situ low-angle x-ray diffraction

    Science.gov (United States)

    Wang, Wei-Hua; Bai, Hai Yang; Zhang, Ming; Zhao, J. H.; Zhang, X. Y.; Wang, W. K.

    1999-04-01

    An in situ low-angle x-ray diffraction technique is used to investigate interdiffusion phenomena in various metal-metal and metal-amorphous Si nanometer-scale compositionally modulated multilayers (ML's). The temperature-dependent interdiffusivities are obtained by accurately monitoring the decay of the first-order modulation peak as a function of annealing time. Activation enthalpies and preexponential factors for the interdiffusion in the Fe-Ti, Ag-Bi, Fe-Mo, Mo-Si, Ni-Si, Nb-Si, and Ag-Si ML's are determined. Activation enthalpies and preexponential factors for the interdiffusion in the ML's are very small compared with that in amorphous alloys and crystalline solids. The relation between the atomic-size difference and interdiffusion in the ML's are investigated. The observed interdiffusion characteristics are compared with that in amorphous alloys and crystalline α-Zr, α-Ti, and Si. The experimental results suggest that a collective atomic-jumping mechanism govern the interdiffusion in the ML's, the collective proposal involving 8-15 atoms moving between extended nonequilibrium defects by thermal activation. The role of the interdiffusion in the solid-state reaction in the ML's is also discussed.

  7. Investigation of potential for occurrence of molten soil displacement events during in situ vitrification of combustible wastes

    International Nuclear Information System (INIS)

    Roberts, J.S.; Strachan, C.W.; Luey, J.

    1993-02-01

    Computer simulations are used to investigate the application of in situ vitrification (ISV) for processing contaminated soil containing high loadings of solid, compressible waste material, typical of landfills and solid waste trenches. Specifically, these simulations predict whether significant displacement of molten soil, due to large, 1 to 2 m diameter, gas bubbles rising up through the ISV melt, are likely to occur during processing of combustible waste-loaded sites. These bubbles are believed to originate from high-pressure regions below the melt caused by vaporization of water and gases generated by the combustion, volatilization, or pyrolyzation of combustible materials in the waste. Simulations were run using the TOUGH2 computer code to predict pressures underneath the ISV melt TOUGH2 is an unsaturated groundwater modeling code capable of treating non-isothermal problems. These simulations include moving melt front and simple pyrolysis models and investigate how the gas pressure in the soil below the melt is affected by melt progression rate, soil permeability, combustible and impermeable material loading. The following, conclusions have been drawn based on the TOUGH2 simulations

  8. Global gyrokinetic simulations of TEM microturbulence

    Science.gov (United States)

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

    2013-07-01

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

  9. TEMS: results of a specialist centre.

    Science.gov (United States)

    Flexer, S M; Durham-Hall, A C; Steward, M A; Robinson, J M

    2014-06-01

    Transanal endoscopic microsurgery (TEMS) is becoming more widespread due to the increasing body of evidence to support its role. Previous published data has reported recurrence rates in excess of 10% for benign polyps after TEMS. Bradford Royal Infirmary is a tertiary referral centre for TEMS and early rectal cancer in the UK. Data for all TEMS operations were entered into a prospective database over a 7-year period. Demographic data, complications and recurrence rates were recorded. Both benign adenomas and malignant lesions were included. A total of 164 patients (65% male), with a mean age of 68 years were included; 114 (70%) of the lesions resected were benign adenomas, and 50 (30%) were malignant lesions. Median polyp size was 4 (range 0.6-14.5) cm. Mean length of operation was 55 (range 10-120) min. There were no recurrences in any patients with a benign adenoma resected; two patients with malignant lesions developed recurrences. Three intra-operative complications were recorded, two rectal perforations (repaired primarily, one requiring defunctioning stoma), and a further patient suffered a blood loss of >300 ml requiring transfusion. Six patients developed strictures requiring dilation either endoscopically or under anaesthetic in the post-operative period. We have demonstrated that TEMS procedures performed in a specialist centre provide low rates of both recurrence and complication. Within a specialist centre, TEMS surgery should be offered to all patients for rectal lesions, both benign and malignant, that are amenable to TEMS.

  10. Developments in TEM Nanotomography of Calcium Silicate Hydrate

    KAUST Repository

    Taylor, Rae; Sakdinawat, Anne E.; Chae, Sejung R.; Wenk, Haz Rudolf; Levitz, Pierre E.; Sougrat, Rachid; Monteiro, Paulo José Meleragno

    2015-01-01

    This investigation was designed to explore the possibility of using transmission electron microscope (TEM) tomography on cement-based systems gain a greater understanding of their nanostructure and pore network. The preliminary results show a clearly a well-defined pore network at the nanoscale, with pore size approximately 1.7-2.4 nm in diameter and spaced around 5-8 nm apart. A comparison of small angle X-ray scattering data with 2-D TEM images analyzed with the Fourier slice theorem documents an excellent structural correlation. © 2015 The American Ceramic Society.

  11. Developments in TEM Nanotomography of Calcium Silicate Hydrate

    KAUST Repository

    Taylor, Rae

    2015-04-01

    This investigation was designed to explore the possibility of using transmission electron microscope (TEM) tomography on cement-based systems gain a greater understanding of their nanostructure and pore network. The preliminary results show a clearly a well-defined pore network at the nanoscale, with pore size approximately 1.7-2.4 nm in diameter and spaced around 5-8 nm apart. A comparison of small angle X-ray scattering data with 2-D TEM images analyzed with the Fourier slice theorem documents an excellent structural correlation. © 2015 The American Ceramic Society.

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

    International Nuclear Information System (INIS)

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

    1979-05-01

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

  13. SIMS and TEM study on oxide characteristics of Zircaloy

    International Nuclear Information System (INIS)

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

    1998-01-01

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

  14. Suspended DNA structural characterization by TEM diffraction

    KAUST Repository

    Marini, Monica

    2017-12-01

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

  15. Suspended DNA structural characterization by TEM diffraction

    KAUST Repository

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

    2017-01-01

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

  16. In situ investigation of the long-term sealing system as component of dam construction (Dam project)

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    1996-12-31

    The project ``In situ investigation of the long term sealing system as a component of a Dam Construction`` started on April 1991. The main objectives of the research to be developed by DIT-UPC group is to model and validate the effects of multiphase flow through the components of the long-term seal and at the interface between the seal and the host rock. These include the following main tasks: -Task 1: State of the art-review -Task 2: Laboratory work -Task 3: Modelling -Task 4: Code verification -Task 5: Validation From these tasks, the main research directions that have been followed are: Constitutive modelling of the mechanical behaviour of porous salt aggregates. Development of a theoretical framework for the study and charaterization of the coupled hydro-thermo-mechanical behaviour of a porous/non-porous saline system. This includes both, establishing the governing equations and the adoption of constitutive laws. The final objective is the development of a numerical simulator able to handle problems in saline environments.

  17. In situ electrochemical-mass spectroscopic investigation of solid electrolyte interphase formation on the surface of a carbon electrode

    International Nuclear Information System (INIS)

    Gourdin, Gerald; Zheng, Dong; Smith, Patricia H.; Qu, Deyang

    2013-01-01

    The energy density of an electrochemical capacitor can be significantly improved by utilizing a lithiated negative electrode and a high surface area positive electrode. During lithiation of the negative carbon electrode, the electrolyte reacts with the electrode surface and undergoes decomposition to form a solid electrolyte interphase (SEI) layer that passivates the surface of the carbon electrode from further reactions between Li and the electrolyte. The reduction reactions that the solvent undergoes also form insoluble and gaseous by-products. In this work, those gaseous by-products generated by reductive decomposition of a carbonate-based electrolyte, 1.2 M LiPF 6 in EC/PC/DEC (3:1:4), were analyzed at different stages during the lithiation process of an amorphous carbon electrode. The stages in the generation of gaseous by-products were determined to come as a result of two, 1-electron reduction steps of the cyclic carbonate components of the electrolyte. Electrochemical impedance spectroscopy was also used to investigate the two distinct electrochemical processes and the development of the two phases of the SEI structure. This is the first time that the state of an electrochemical cell during the formation of the SEI layer has been systematically correlated with theoretical reaction mechanisms through the use of in situ electrochemical-MS and impedance spectroscopy analyses

  18. In situ investigation of the long-term sealing system as component of dam construction (Dam project)

    International Nuclear Information System (INIS)

    1995-01-01

    The project ''In situ investigation of the long term sealing system as a component of a Dam Construction'' started on April 1991. The main objectives of the research to be developed by DIT-UPC group is to model and validate the effects of multiphase flow through the components of the long-term seal and at the interface between the seal and the host rock. These include the following main tasks: -Task 1: State of the art-review -Task 2: Laboratory work -Task 3: Modelling -Task 4: Code verification -Task 5: Validation From these tasks, the main research directions that have been followed are: Constitutive modelling of the mechanical behaviour of porous salt aggregates. Development of a theoretical framework for the study and charaterization of the coupled hydro-thermo-mechanical behaviour of a porous/non-porous saline system. This includes both, establishing the governing equations and the adoption of constitutive laws. The final objective is the development of a numerical simulator able to handle problems in saline environments

  19. In situ STM investigation of aromatic poly(azomethine) arrays constructed by "on-site" equilibrium polymerization.

    Science.gov (United States)

    Tanoue, Ryota; Higuchi, Rintaro; Ikebe, Kiryu; Uemura, Shinobu; Kimizuka, Nobuo; Stieg, Adam Z; Gimzewski, James K; Kunitake, Masashi

    2012-10-02

    Two-dimensional (2D) arrays of π-conjugated aromatic polymers produced by surface-selective Schiff base coupling reactions between an aromatic diamine and an aromatic dialdehyde were investigated in detail using in situ scanning tunneling microscopy. Surface-selective coupling was achieved for almost all diamine/dialdehyde combinations attempted, although several combinations did not proceed even in homogeneous aqueous alkaline solution. Most of the combinations of an aromatic diamine and a dialdehyde, except the combinations of 4,4'-azodianiline with mono/bithiophenedicarboxaldehyde, formed highly ordered π-conjugated polymer arrays on an iodine-modified Au(111) surface in aqueous solution at a suitable pH. The simplest polymer of the various combinations tested, obtained from the combination of 1,4-diaminobenzene with terephthaldicarboxaldehyde, gave a 2D array consisting of linearly connected benzene units. Poly(azomethine) adlayers caused a positive shift in the electrochemical potential of the butterfly shaped oxidative adsorption and reductive desorption of iodine. The acceleration of the reductive desorption of iodine suggests the existence of a weak interaction between the polymer layer and iodine. Not only the first polymer adlayers but also partially adsorbed secondary adlayers with "on-top" epitaxial behavior were frequently observed for all polymer systems. The alignment of the polymer chains in the adlayers possessed a certain regularity in terms of a regular interval between polymer chains because of repulsive interpolymer interactions.

  20. In Situ Radiographic Investigation of (De)Lithiation Mechanisms in a Tin-Electrode Lithium-Ion Battery.

    Science.gov (United States)

    Sun, Fu; Markötter, Henning; Zhou, Dong; Alrwashdeh, Saad Sabe Sulaiman; Hilger, Andre; Kardjilov, Nikolay; Manke, Ingo; Banhart, John

    2016-05-10

    The lithiation and delithiation mechanisms of multiple-Sn particles in a customized flat radiography cell were investigated by in situ synchrotron radiography. For the first time, four (de)lithiation phenomena in a Sn-electrode battery system are highlighted: 1) the (de)lithiation behavior varies between different Sn particles, 2) the time required to lithiate individual Sn particles is markedly different from the time needed to discharge the complete battery, 3) electrochemical deactivation of originally electrochemically active particles is reported, and 4) a change of electrochemical behavior of individual particles during cycling is found and explained by dynamic changes of (de)lithiation pathways amongst particles within the electrode. These unexpected findings fundamentaly expand the understanding of the underlying (de)lithiation mechanisms inside commercial lithium-ion batteries (LIBs) and would open new design principles for high-performance next-generation LIBs. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Preliminary investigation of the potential for transient vapor release events during in situ vitrification based on thermal- hydraulic modeling

    International Nuclear Information System (INIS)

    Roberts, J.S.; Woosley, S.L.; Lessor, D.L.; Strachan, C.

    1992-07-01

    This study investigates a possible cause of molten glass displacements that occurred during two recent in situ vitrification (ISV) tests. The study was conducted for the US Department of Energy by Pacific Northwest Laboratory. It is hypothesized that these glass displacements are caused by large gas bubbles rising up through the ISV melt and bursting at its surface. These bubbles cause the molten surface to upwell and possibly overflow. When the bubbles burst, molten glass is thrown from the melt surface and the volume of gas contained in the bubble is released into the hood. Both of these phenomena are undesirable because the molten soil ejected from the melt is dangerous to operating personnel and can damage equipment. The sudden gas release can cause a temporary pressurization of the hood, allowing potentially contaminated gas to escape to the atmosphere. This study attempts to explain the conditions necessary for formation of large gas bubbles in the melt so that future glass displacements can be avoided

  2. Preliminary investigation of the potential for transient vapor release events during in situ vitrification based on thermal- hydraulic modeling

    Energy Technology Data Exchange (ETDEWEB)

    Roberts, J.S.; Woosley, S.L.; Lessor, D.L.; Strachan, C.

    1992-07-01

    This study investigates a possible cause of molten glass displacements that occurred during two recent in situ vitrification (ISV) tests. The study was conducted for the US Department of Energy by Pacific Northwest Laboratory. It is hypothesized that these glass displacements are caused by large gas bubbles rising up through the ISV melt and bursting at its surface. These bubbles cause the molten surface to upwell and possibly overflow. When the bubbles burst, molten glass is thrown from the melt surface and the volume of gas contained in the bubble is released into the hood. Both of these phenomena are undesirable because the molten soil ejected from the melt is dangerous to operating personnel and can damage equipment. The sudden gas release can cause a temporary pressurization of the hood, allowing potentially contaminated gas to escape to the atmosphere. This study attempts to explain the conditions necessary for formation of large gas bubbles in the melt so that future glass displacements can be avoided.

  3. Investigation of the Lobular Carcinoma in Situ, Using Molecular Genetic Techniques, for the Involvement of Novel Genes

    National Research Council Canada - National Science Library

    Mastracci, Teresa

    2004-01-01

    Atypical lobular hyperplasia (ALH) and lobular carcinoma in situ (LCIS), i.e. lobular neoplasia (LN), are lesions of significance in terms of implication to the patient in the development of invasive carcinoma...

  4. Investigation of the Lobular Carcinoma in Situ, Using Molecular Genetic Techniques, for the Involvement of Novel Genes

    National Research Council Canada - National Science Library

    Mastracci, Teresa L; Andrulis, Irene L

    2005-01-01

    Atypical lobular hyperplasia (ALH) and lobular carcinoma in situ (LCIS), i.e. lobular neoplasia (LN), are lesions of significance in terms of risk to the patient in the development of invasive carcinoma...

  5. Self-ignition of coal during in-situ gasification. Thermoanalytical investigations. Selbstentzuendung von Kohlen bei der Untertagevergasung. Thermoanalytische Untersuchungen

    Energy Technology Data Exchange (ETDEWEB)

    Choi, J O

    1986-01-10

    The underground gasification of deep coal strata via boreholes presupposes flow ways for the gasifying agent and the gasified media with a sufficiently high degree of permeability. Canal burning during countercurrent flow in low depths has been tested as a technical method for linking boreholes and enhancing gas permeability. For the execution of in situ gasification the control or prevention of the spontaneous ignition of the coal under high pressure should not be ignored, because of self-ignition resulting from canal burning in the linking phase. To investigate enthalpy change during the oxidation of coal under various conditions, a device for differential thermal analysis (DTA) was developed and constructed with which temperature development as a result of oxidation in a flowing pressure-gas atmosphere could be observed. A caloric calibration of the device permitted a direct inference of enthalpic difference from differential thermal potential as a measured value. With a regression model for reaction kinetics, the intensity of heat development was linked with kinetic data; this permitted a description of the dependence of the oxidation process on temperature and material concentration. From the interconnections discovered between the carbonization degree and enthalpy change during oxidation we may conclude that the oxidation process is controlled by the emergence of thermal decomposition products. The heat tonality diagram of the DTA of coal oxidation can be divided into three phases and interpreted in connection with the different degrees of carbonization. The results of the investigation reveal that inactivation of the coal before the actual process of linking is of considerable importance. (MOS).

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

    International Nuclear Information System (INIS)

    Tanaka, Nobuo

    2008-01-01

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

  7. In Situ Investigation of the Evolution of Lattice Strain and Stresses in Austenite and Martensite During Quenching and Tempering of Steel

    DEFF Research Database (Denmark)

    Villa, M.; Niessen, F.; Somers, M. A. J.

    2018-01-01

    Energy dispersive synchrotron X-ray diffraction was applied to investigate in situ the evolution of lattice strains and stresses in austenite and martensite during quenching and tempering of a soft martensitic stainless steel. In one experiment, lattice strains in austenite and martensite were...... measured in situ in the direction perpendicular to the sample surface during an austenitization, quenching, and tempering cycle. In a second experiment, the sin2ψ method was applied in situ during the austenite-to-martensite transformation to distinguish between macro- and phase-specific micro......-stresses and to follow the evolution of these stresses during transformation. Martensite formation evokes compressive stress in austenite that is balanced by tensile stress in martensite. Tempering to 748 K (475 °C) leads to partial relaxation of these stresses. Additionally, data reveal that (elastic) lattice strain...

  8. Evolution of organic matter in Orgueil, Murchison and Renazzo during parent body aqueous alteration: In situ investigations

    Science.gov (United States)

    Le Guillou, Corentin; Bernard, Sylvain; Brearley, Adrian J.; Remusat, Laurent

    2014-04-01

    Chondrites accreted the oldest solid materials in the solar system including dust processed in the protoplanetary disk and diverse organic compounds. After accretion, asteroidal alteration may have impacted organic particles in various ways. To constrain these processes, we conducted a comprehensive study of organics disseminated within the matrices of the three carbonaceous chondrite falls, Renazzo (CR2), Murchison (CM2) and Orgueil (CI). By combining synchrotron-based STXM and TEM analyses on FIB sections of samples previously characterized by NanoSIMS, we investigated the influence of aqueous alteration on the morphology, isotopic signature, molecular structure, spatial distribution, and mineralogical environment of the organic matter within the matrices. Two different populations of materials are distinguishable: sub-micrometric individual grains, likely dominated by insoluble compounds and diffuse organic matter, finely interspersed within phyllosilicates and/or (amorphous) nanocarbonates at the nanometer scale. We suggest that this latter component, which is depleted in aromatics and enriched in carboxylic functional groups, may be dominated by soluble compounds. Organic matter in Renazzo (CR) mainly consists of chemically-homogeneous individual grains surrounded by amorphous and nanocrystalline phyllosilicates. Evidence of connectivity between organic grains and fractures indicates that redistribution has occurred: some areas containing diffuse organic matter can be observed. This diffuse organic component is more abundant in Murchison (CM) and Orgueil (CI). This is interpreted as resulting from fluid transport at the micrometer scale and encapsulation within recrystallized alteration phases. In contrast to Renazzo, organic grains in Murchison and Orgueil display strong chemical heterogeneities, likely related to chemical evolution during aqueous alteration. The observations suggest that the altering fluid was a brine with elevated concentrations of both

  9. Hydrochemical investigation and status of geochemical modeling of groundwater evolution at the Kamaishi in-situ tests site, Japan

    International Nuclear Information System (INIS)

    Sasamoto, Hiroshi; Yui, Mikazu; Arthur, Randolph C.

    1999-07-01

    The results of hydrochemical investigations of groundwaters in the Kurihashi granodiorite at JNC's Kamaishi in-situ tests site indicate that these solutions are: meteoric in origin, chemically reducing (at depths greater than a few hundreds meters), relatively young [residence times in the Kurihashi granodiorite generally less than about 40 years, but groundwaters older than several thousand years BP (before present) are also indicated by preliminary carbon-14 dating of samples obtained from the KH-1 borehole], Ca-HCO 3 type solutions near the surface, changing to Na-HCO 3 type groundwaters with increasing depth. The evolution of groundwater compositions in the Kurihashi granodiorite is modeled assuming local equilibrium for selected mineral-fluid reactions, taking into account the rainwater origin of these solutions. Results suggest it is possible to interpret approximately the 'real' groundwater chemistry (i.e., pH, Eh, total dissolved concentrations of Si, Na, Ca, K, Al, carbonate and sulfate) in the Kurihashi granodiorite if the following assumptions are adopted: CO 2 concentration in the gas phase contacting pore solutions in the overlying soil zone=10 -2 bar, minerals in the rock zone that control the solubility of respective elements in the groundwater include; chalcedony (Si), albite (Na), kaolinite (Al), calcite (Ca and carbonate), microcline (K) and pyrite (Eh and sulfate). Discussions with international experts suggest a systematic approach utilizing reaction-path models of irreversible water-rock interactions in open systems may be needed to more realistically model groundwater evolution at the Kamaishi test site. Detailed information characterizing certain site properties (e.g., fracture mineralogy) may be required to adequately constrain such models, however. (author)

  10. Structural investigations of LiFePO4 electrodes and in situ studies by Fe X-ray absorption spectroscopy

    International Nuclear Information System (INIS)

    Deb, Aniruddha; Bergmann, Uwe; Cramer, S.P.; Cairns, Elton J.

    2005-01-01

    Fe K-edge X-ray absorption near edge spectroscopy (XANES) and extended X-ray absorption fine structure (EXAFS) have been performed on electrodes containing LiFePO 4 to determine the local atomic and electronic structure and their stability with electrochemical cycling. A versatile electrochemical in situ cell has been constructed for long-term soft and hard X-ray experiments for the structural investigation on battery electrodes during the lithium-insertion/extraction processes. The device is used here for an X-ray absorption spectroscopic study of lithium insertion/extraction in a LiFePO 4 electrode, where the electrode contained about 7.7 mg of LiFePO 4 on a 20 μm thick Al-foil. Fe K-edge X-ray absorption near edge spectroscopy (XANES) and extended X-ray absorption fine structure (EXAFS) have been performed on this electrode to determine the local atomic and electronic structure and their stability with electrochemical cycling. The initial state (LiFePO 4 ) showed iron to be in the Fe 2+ state corresponding to the initial state (0.0 mAh) of the cell, whereas in the delithiated state (FePO 4 ) iron was found to be in the Fe 3+ state corresponding to the final charged state (3 mAh). XANES region of the XAS spectra revealed a high spin configuration for the two states (Fe (II), d 6 and Fe (III), d 5 ). The results confirm that the olivine structure of the LiFePO 4 and FePO 4 is retained by the electrodes in agreement with the XRD observations reported previously. These results confirm that LiFePO 4 cathode material retains good structural short-range order leading to superior cycling capability

  11. Moessbauer effect and TEM in mineralogy

    International Nuclear Information System (INIS)

    Ferrow, E.A.

    1994-01-01

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

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

    International Nuclear Information System (INIS)

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

    2015-01-01

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

  13. Electrochromic characteristics of a nickel borate thin film investigated by in situ XAFS and UV/vis spectroscopy

    International Nuclear Information System (INIS)

    Yoshida, Masaaki; Iida, Tsuyoshi; Mineo, Takehiro

    2014-01-01

    The electrochromic transition of a nickel borate thin film between colorless and brown was examined by means of in situ XAFS and UV/vis spectroscopy. The XAFS spectra showed that the average valence state of the nickel species in the film changed from +2.1 to +3.8 following the application of an electrode potential. Additionally, a broad peak at 700 nm was observed during in situ UV/vis absorption measurements on the application of a positive potential. These results suggest that the nickel borate film reversibly forms a NiOOH structure with a domain size of several nanometers during the electrochromic reaction. (author)

  14. In situ57Fe Moessbauer Investigation of Solid-State Redox Reactions of Lithium Insertion Electrodes for Advanced Batteries

    International Nuclear Information System (INIS)

    Sakai, Yoichi; Ariyoshi, Kingo; Ohzuku, Tsutomu

    2002-01-01

    A novel in situ electrochemical cell for 57 Fe Moessbauer measurements was developed in order to clarify the mechanisms of solid-state redox reactions in lithium insertion materials containing iron. Our in situ Moessbauer technique was successfully applied to the determination as to which transition metal ion was a redox center in the insertion electrodes, such as LiFe 0.5 Mn 1.5 O 4 , LiFeTiO 4 , or LiFe 0.25 Ni 0.75 O 2 , for the lithium-ion batteries.

  15. Correlation of simulated TEM images with irradiation induced damage

    International Nuclear Information System (INIS)

    Schaeublin, R.; Almeida, P. de; Almazouzi, A.; Victoria, M.

    2000-01-01

    Crystal damage induced by irradiation is investigated using transmission electron microscopy (TEM) coupled to molecular dynamics (MD) calculations. The displacement cascades are simulated for energies ranging from 10 to 50 keV in Al, Ni and Cu and for times of up to a few tens of picoseconds. Samples are then used to perform simulations of the TEM images that one could observe experimentally. Diffraction contrast is simulated using a method based on the multislice technique. It appears that the cascade induced damage in Al imaged in weak beam exhibits little contrast, which is too low to be experimentally visible, while in Ni and Cu a good contrast is observed. The number of visible clusters is always lower than the actual one. Conversely, high resolution TEM (HRTEM) imaging allows most of the defects contained in the sample to be observed, although experimental difficulties arise due to the low contrast intensity of the smallest defects. Single point defects give rise in HTREM to a contrast that is similar to that of cavities. TEM imaging of the defects is discussed in relation to the actual size of the defects and to the number of clusters deduced from MD simulations

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

    Science.gov (United States)

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

    2016-11-01

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

  17. Destructive interference of TEM and ITG turbulence

    International Nuclear Information System (INIS)

    Merz, F.; Jenko, F.

    2009-01-01

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

  18. Test for English Majors (TEM) in China

    Science.gov (United States)

    Jin, Yan; Fan, Jinsong

    2011-01-01

    The purpose of the Test for English Majors (TEM) is to measure the English proficiency of Chinese university undergraduates majoring in English Language and Literature and to examine whether these students meet the required levels of English language abilities as specified in the National College English Teaching Syllabus for English Majors…

  19. Investigation of the Failure Mechanism of HTPB/AP/Al Propellant by In-situ Uniaxial Tensile Experimentation in SEM

    NARCIS (Netherlands)

    Ramshorst, M.C.J. van; Benedetto, G.L. di; Duvalois, W.; Hooijmeijer, P.A.; Heijden, A.E.D.M. van der

    2016-01-01

    The failure mechanism of a propellant consisting of hydroxyl terminated poly-butadiene filled with ammonium perchlorate and aluminum (HTPB/AP/Al) was determined by performing in-situ uniaxial tensile tests in a scanning electron microscope (SEM). The experimental test plan contained uniaxial tensile

  20. In-situ investigation of strain-induced martensitic transformation kinetics in an austenitic stainless steel by inductive measurements

    NARCIS (Netherlands)

    Alonso de Celada Casero, C.; Kooiker, Harm; Groen, Manso; Post, J; San Martin, D

    2017-01-01

    An inductive sensor developed by Philips ATC has been used to study in-situ the austenite (γ) to martensite (α′) phase transformation kinetics during tensile testing in an AISI 301 austenitic stainless steel. A correlation between the sensor output signal and the volume fraction of α′-martensite

  1. SEM in situ laboratory investigations on damage growth in GFRP composite under three-point bending tests

    DEFF Research Database (Denmark)

    Zhou, Hong Wei; Mishnaevsky, Leon; Brøndsted, Povl

    2010-01-01

    Glass fiber-reinforced polymer (GFRP) composites are widely used in low-weight constructions. SEM (scanning electron microscopy) in situ experiments of damage growth in GFRP composite under three-point bending loads are carried out. By summarizing the experimental results of three groups of samples...

  2. In situ Sr/Sr investigation of igneous apatites and carbonates using laser-ablation MC-ICP-MS

    DEFF Research Database (Denmark)

    Bizzarro, Martin; Simonetti, A.; Stevenson, R.K.

    2003-01-01

    In situ Sr isotopic compositions of coexisting apatite and carbonate for carbonatites from the Sarfartoq alkaline complex, Greenland, have been determined by laser-ablation multicollector inductively coupled plasma mass spectrometry. This study is the first to examine the extent of Sr isotopic ho...

  3. 40 keV atomic resolution TEM

    International Nuclear Information System (INIS)

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

    2012-01-01

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

  4. XPS, TEM and NRA investigations of Zn(Se,OH)/Zn(OH){sub 2} films on Cu(In,Ga)(S,Se){sub 2} substrates for highly efficient solar cells

    Energy Technology Data Exchange (ETDEWEB)

    Eisele, W.; Ennaoui, A.; Schubert-Bischoff, P.; Giersig, M.; Pettenkofer, C.; Krauser, J.; Lux-Steiner, M. [Hahn-Meitner Inst., Berlin (Germany); Zweigart, S.; Karg, F. [Siemens and Shell Solar, Munich (Germany)

    2003-01-01

    Structural and compositional properties of Zn(Se,OH)/Zn(OH){sub 2} buffer layers deposited by chemical bath deposition(CBD) on Cu(In,Ga)(S,Se){sub 2} (CIGSS) absorbers are investigated. Due to the aqueous nature of the CBD process, oxygen and hydrogen were incorporated into the 'ZnSe' buffer layer mainly in the form of Zn(OH){sub 2} as is shown by X-ray photoelectron spectroscopy and nuclear reaction analysis (NRA) measurements leading to the nomenclature 'Zn(Se,OH)'. Prior to the deposition of Zn(Se,OH), a zinc treatment of the absorber was performed. During that treatment a layer mainly consisting of Zn(OH){sub 2} grew to a thickness of several nanometer. The whole buffer layer therefore consists of a Zn(Se,OH)/Zn(OH){sub 2} structure on CIGSS. Part of the Zn(OH){sub 2} in both layers (i.e. the Zn(Se,OH) and the Zn(OH){sub 2} layer) might be converted into ZnO during measurements or storage. Scanning electron microscopy pictures showed that a complete coverage of the absorber with the buffer layer was achieved. Transmission electron microscopy revealed the different regions of the buffer layer: An amorphous area (possibly Zn(OH){sub 2}) and a partly nanocrystalline area, where lattice planes of ZnSe could be identified. Solar cell efficiencies of ZnO/Zn(Se,OH)/Zn(OH){sub 2}/CIGSS devices exceed 14% (total area).(author)

  5. Phase separation of in situ forming poly (lactide-co-glycolide acid) implants investigated using a hydrogel-based subcutaneous tissue surrogate and UV-vis imaging.

    Science.gov (United States)

    Sun, Yu; Jensen, Henrik; Petersen, Nickolaj J; Larsen, Susan W; Østergaard, Jesper

    2017-10-25

    Phase separation of in situ forming poly (lactide-co-glycolide acid) (PLGA) implants with agarose hydrogels as the provider of nonsolvent (water) mimicking subcutaneous tissue was investigated using a novel UV-vis imaging-based analytical platform. In situ forming implants of PLGA-1-methyl-2-pyrrolidinone and PLGA-triacetin representing fast and slow phase separating systems, respectively, were evaluated using this platform. Upon contact with the agarose hydrogel, the phase separation of the systems was followed by the study of changes in light transmission and absorbance as a function of time and position. For the PLGA-1-methyl-2-pyrrolidinone system, the rate of spatial phase separation was determined and found to decrease with increasing the PLGA concentration from 20% to 40% (w/w). Hydrogels with different agarose concentrations (1% and 10% (w/v)) were prepared for providing the nonsolvent, water, to the in situ forming PLGA implants simulating the injection site environment. The resulting implant morphology depended on the stiffness of hydrogel matrix, indicating that the matrix in which implants are formed is of importance. Overall, the work showed that the UV-vis imaging-based platform with an agarose hydrogel mimicking the subcutaneous tissue holds potential in providing bio-relevant and mechanistic information on the phase separation processes of in situ forming implants. Copyright © 2017 Elsevier B.V. All rights reserved.

  6. Coupling scanning tunneling microscope and supersonic molecular beams: a unique tool for in situ investigation of the morphology of activated systems.

    Science.gov (United States)

    Smerieri, M; Reichelt, R; Savio, L; Vattuone, L; Rocca, M

    2012-09-01

    We report here on a new experimental apparatus combining a commercial low temperature scanning tunneling microscope with a supersonic molecular beam. This setup provides a unique tool for the in situ investigation of the topography of activated adsorption systems and opens thus new interesting perspectives. It has been tested towards the formation of the O/Ag(110) added rows reconstruction and of their hydroxylation, comparing data recorded upon O(2) exposure at thermal and hyperthermal energies.

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

    International Nuclear Information System (INIS)

    Zakhozheva, Marina

    2016-01-01

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

  8. Argillite / cementitious materials interaction: in-situ investigations and modeling of engineered analogues from the Tournemire experimental station

    International Nuclear Information System (INIS)

    Techer, I.; Bartier, D.; Dauzeres, A.; Boulvais, P.

    2012-01-01

    Document available in extended abstract form only. Deep geological disposal of high-activity and long-period radioactive wastes is designed by the French National Agency for Radioactive Waste Management (Andra) with a confinement system based on the multiplication of argillaceous and cement-bearing barriers called 'engineered barriers'. The role of these barriers is to avoid the release of radioelements into the biosphere, as well as to prevent the potential addition of external fluids to the waste materials. In a deep clay-rich medium, cementitious materials will compose most of the building structures and will be emplaced at the immediate contact with the natural argillaceous formation. Cementitious materials are known to produce hyper-alkaline pore fluids (with pHs ranging between 10 and 13.5) during their aging. Their introduction in a deep clayey disposal is thus expected to induce a chemical disequilibrium which imprint on the safety assessment of the storage must be characterized. One way to evaluate the potential disturbing of a clayey formation at the contact to a cementitious material and thus towards the percolation of hyper-alkaline fluids consists with the investigation of natural analogues or engineered analogues. These systems deals with clayey formations that have been maintained over several years to hundred of years at the contact with a natural or engineered cementitious material. The Tournemire Experimental Platform of the French Institute for Radioprotection and Nuclear Safety (IRSN) (Aveyron, SE France) presents many contexts of so-defined engineered analogues. For instance, exploration boreholes that were drilled vertically from the tunnel basement into the Toarcian argillite in 1990/1991 were filled soon after their drilling with CEM II cement paste and concrete. Today, the over coring of such concreted boreholes gives opportunities to examine the cementitious and the clayey materials and to discuss potential changes of their intrinsic

  9. MORPHOLOGICAL ASPECTS OF HUMAN LENS CAPSULES - A COMPARATIVE LM, SEM AND TEM EXAMINATION

    NARCIS (Netherlands)

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

    1991-01-01

    Lens capsules of patients of advanced age, obtained after extracapsular cataract surgery, were carefully prepared for a combined LM, TEM and SEM investigation, after preliminary washing and mounting onto a holder in a buffer solution. After pre-fixation with GA, samples were postfixed for LM/TEM and

  10. Crack nucleation and elastic / plastic deformation of TiAl alloys investigated by in-situ loaded atomic force microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Iqbal, F.; Pyczak, F.; Neumeier, S.; Göken, M.

    2017-03-24

    The crack propagation mechanisms of γ-titanium aluminides with fully lamellar microstructure have been studied using in-situ deformation in the Atomic Force Microscope (AFM). AFM demonstrated the unique capability to detect elastic as well as plastic deformation during in-situ tests from topography changes on the surface. It was found that the crack nucleation, which can occur at γ/γ and α{sub 2}/γ interfaces as well as inside the γ-phase, is always preceded by strong local elastic deformation. No cracking inside the α{sub 2}-phase was observed. The elastic and plastic deformation was confined inside the γ-phase and especially pronounced near interfaces which can be explained by the differences of the elastic and plastic deformation behavior of the γ- and α{sub 2}- phase.

  11. In-Situ Investigation of Strain-Induced Martensitic Transformation Kinetics in an Austenitic Stainless Steel by Inductive Measurements

    Directory of Open Access Journals (Sweden)

    Carola Celada-Casero

    2017-07-01

    Full Text Available An inductive sensor developed by Philips ATC has been used to study in-situ the austenite (γ to martensite (α′ phase transformation kinetics during tensile testing in an AISI 301 austenitic stainless steel. A correlation between the sensor output signal and the volume fraction of α′-martensite has been found by comparing the results to the ex-situ characterization by magnetization measurements, light optical microscopy, and X-ray diffraction. The sensor has allowed for the observation of the stepwise transformation behavior, a not-well-understood phenomena that takes place in large regions of the bulk material and that so far had only been observed by synchrotron X-ray diffraction.

  12. Texture evolution of orthorhombic α″ titanium alloy investigated by in situ X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Elmay, W., E-mail: wafa.elmay@ensam.eu [Laboratoire d' Etude des Microstructures et de Mécanique des Matériaux LEM3 (UMR CNRS 7239), 4 rue Augustin Fresne, 57078 Metz (France); Berveiller, S.; Patoor, E. [Laboratoire d' Etude des Microstructures et de Mécanique des Matériaux LEM3 (UMR CNRS 7239), 4 rue Augustin Fresne, 57078 Metz (France); Gloriant, T. [Chimie-Métallurgie (UMR CNRS 6226), 20, Avenue des Buttes de Coesmes, F-35043 Rennes (France); Prima, F. [Laboratoire de Physico-Chimie des Surfaces (UMR CNRS 7045), 11 Rue Pierre et Marie Curie, F-75231 Paris (France); Laheurte, P. [Laboratoire d' Etude des Microstructures et de Mécanique des Matériaux LEM3 (UMR CNRS 7239), 4 rue Augustin Fresne, 57078 Metz (France)

    2017-01-02

    The present paper deals with an in-situ X-ray diffraction analysis during cyclic tensile tests of a fully martensitic Ti-24Nb alloy. Texture evolution of martensite α″ phase was followed during loading-unloading cycles. Preferential formation and reverse transformation of particular martensite variants have been observed based on pole figure analysis. The occurrence of the deformation mechanisms for the martensitic Ti-24Nb alloy was also commented by coupling microstructural observations during in-situ experiments and additional cyclic tests followed by heating after each unloading. Through the study of the evolution of the lattice strain, it was found that under loading conditions, the {020} planes exhibit a large tension lattice strain while the {200} planes are subjected to a compression solicitation, which causes the lattice parameters a and c to be shrunk, and b to be elongated.

  13. Surface damage in TEM thick α-Fe samples by implantation with 150 keV Fe ions

    International Nuclear Information System (INIS)

    Aliaga, M.J.; Caturla, M.J.; Schäublin, R.

    2015-01-01

    We have performed molecular dynamics simulations of implantation of 150 keV Fe ions in pure bcc Fe. The thickness of the simulation box is of the same order of those used in in situ TEM analysis of irradiated materials. We assess the effect of the implantation angle and the presence of front and back surfaces. The number and type of defects, ion range, cluster distribution and primary damage morphology are studied. Results indicate that, for the very thin samples used in in situ TEM irradiation experiments the presence of surfaces affect dramatically the damage produced. At this particular energy, the ion has sufficient energy to damage both the top and the back surfaces and still leave the sample through the bottom. This provides new insights on the study of radiation damage using TEM in situ

  14. TEM investigation of ductile iron alloyed with vanadium.

    Science.gov (United States)

    Dymek, S; Blicharski, M; Morgiel, J; Fraś, E

    2010-03-01

    This article presents results of the processing and microstructure evolution of ductile cast iron, modified by an addition of vanadium. The ductile iron was austenitized closed to the solidus (1095 degrees C) for 100 h, cooled down to 640 degrees C and held on at this temperature for 16 h. The heat treatment led to the dissolution of primary vanadium-rich carbides and their subsequent re-precipitation in a more dispersed form. The result of mechanical tests indicated that addition of vanadium and an appropriate heat treatment makes age hardening of ductile iron feasible. The precipitation processes as well as the effect of Si content on the alloy microstructure were examined by scanning and transmission electron microscopy. It was shown that adjacent to uniformly spread out vanadium-rich carbides with an average size of 50 nm, a dispersoid composed of extremely small approximately 1 nm precipitates was also revealed.

  15. Preparation of Atomically Flat Si(111)-H Surfaces in Aqueous Ammonium Fluoride Solutions Investigated by Using Electrochemical, In Situ EC-STM and ATR-FTIR Spectroscopic Methods

    International Nuclear Information System (INIS)

    Bae, Sang Eun; Oh, Mi Kyung; Min, Nam Ki; Paek, Se Hwan; Hong, Suk In; Lee, Chi-Woo J.

    2004-01-01

    Electrochemical, in situ electrochemical scanning tunneling microscope (EC-STM), and attenuated total reflectance-FTIR (ATR-FTIR) spectroscopic methods were employed to investigate the preparation of atomically flat Si(111)-H surface in ammonium fluoride solutions. Electrochemical properties of atomically flat Si(111)-H surface were characterized by anodic oxidation and cathodic hydrogen evolution with the open circuit potential (OCP) of ca. .0.4 V in concentrated ammonium fluoride solutions. As soon as the natural oxide-covered Si(111) electrode was immersed in fluoride solutions, OCP quickly shifted to near .1 V, which was more negative than the flat band potential of silicon surface, indicating that the surface silicon oxide had to be dissolved into the solution. OCP changed to become less negative as the oxide layer was being removed from the silicon surface. In situ EC-STM data showed that the surface was changed from the initial oxide covered silicon to atomically rough hydrogen-terminated surface and then to atomically flat hydrogen terminated surface as the OCP moved toward less negative potentials. The atomically flat Si(111)-H structure was confirmed by in situ EC-STM and ATR-FTIR data. The dependence of atomically flat Si(111)-H terrace on mis-cut angle was investigated by STM, and the results agreed with those anticipated by calculation. Further, the stability of Si(111)-H was checked by STM in ambient laboratory conditions

  16. In-situ Observation of Fracture Behavior on Nano Structure in NITE SiC/SiC Composite by HVEM

    International Nuclear Information System (INIS)

    Shibayama, Tamaki; Hamada, Kouichi; Watanabe, Seiichi; Matsuo, Genichiro; Kishimoto, Hirotatsu

    2011-01-01

    We have been successfully done in situ observation on the sequence of fracture event at the interface of NITE SiC/SiC composite examined by using miniaturized double notched shear specimen for TEM prepared by Focused Ion Beam method. In this study, we used nano-mechanics TEM experimental apparatus to investigate not only microstructure evolution and but also load and displacement curve at once in High Voltage Electron Microscope. Our results summarize as follows. Cracks were initiated at the interface between carbon coating layer on the SiC fiber and SiC matrices, and propagated along the interface. Load drop in the load and displacement curve during in-situ TEM was clearly observed at the crack initiation. The shear strength by using the miniaturized specimen is about ten times higher than that obtained by the standard testing.

  17. In situ biomimetic synthesis, characterization and in vitro investigation of bone-like nanohydroxyapatite in starch matrix

    Energy Technology Data Exchange (ETDEWEB)

    Sadjadi, M.S., E-mail: msadjad@gmail.com [Department of Chemistry, Science and Research Branch, Islamic Azad University, Poonak, Tehran (Iran, Islamic Republic of); Meskinfam, M. [Department of Chemistry, Science and Research Branch, Islamic Azad University, Poonak, Tehran (Iran, Islamic Republic of); Sadeghi, B. [Department of Chemistry, Tonekabon Branch, Islamic Azad university, Tonekabon (Iran, Islamic Republic of); Jazdarreh, H. [Department of Mechanical Engineering, Iran University of Science and Technology, Narmak, Tehran (Iran, Islamic Republic of); Zare, K. [Department of Chemistry, Faculty of Science, Shahid Beheshti University, Tehran (Iran, Islamic Republic of)

    2010-11-01

    In this work, we report the synthesis of bone-like hydroxyapatite (HAp) nanorods in wheat starch matrix via a biomimetic process. Characterization of the samples was performed by X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FT-IR). Scanning and transmission electron microscopy (SEM and TEM) were used to determine the size, shape and morphology of nano-HAp. The results indicate that, the shape and morphology of nHAp is influenced by the presence of starch as a template agent and rod-like nHAp similar to the inorganic component in the human body is obtained at room temperature. In vitro bioactivity of the synthesized HAp nanocomposites was finally verified by comparison of the HAp's structures and morphology before and after immersion in simulated body fluid (SBF) solution for 3, 7, and 14 days.

  18. In situ investigation of formation of self-assembled nanodomain structure in lithium niobate after pulse laser irradiation

    Energy Technology Data Exchange (ETDEWEB)

    Shur, V. Ya.; Kuznetsov, D. K.; Mingaliev, E. A.; Yakunina, E. M.; Lobov, A. I.; Ievlev, A. V. [Ferroelectric Laboratory, Institute of Physics and Applied Mathematics, Ural State University, Lenin Ave. 51, Ekaterinburg 620083 (Russian Federation)

    2011-08-22

    The evolution of the self-assembled quasi-regular micro- and nanodomain structures after pulse infrared laser irradiation was studied by in situ optical observation. The average periods of the structures are much less than the sizes of the laser spots. The polarization reversal occurs through covering of the whole irradiated area by the nets of the spatially separated nanodomain chains and microdomain rays--''hatching effect.'' The main stages of the anisotropic nanodomain kinetics: nucleation, growth, and branching, have been singled out. The observed abnormal domain kinetics was attributed to the action of the pyroelectric field arising during cooling after laser heating.

  19. Nickel oxide reduction studied by environmental TEM

    DEFF Research Database (Denmark)

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

    2012-01-01

    In situ reduction of an industrial NiO powder is performed under 1.3 mbar of H2 (2 mlN/min) in a differentially pumped FEI Titan 80-300 environmental transmission electron microscope (ETEM). Images, diffraction patterns and electron energy loss spectra (EELS) are acquired to monitor the structura...

  20. Recent advances in FIB-TEM specimen preparation techniques

    International Nuclear Information System (INIS)

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

    2006-01-01

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

  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. Characterization of some biological specimens using TEM and SEM

    Science.gov (United States)

    Ghosh, Nabarun; Smith, Don W.

    2009-05-01

    The advent of novel techniques using the Transmission and Scanning Electron Microscopes improved observation on various biological specimens to characterize them. We studied some biological specimens using Transmission and Scanning Electron Microscopes. We followed negative staining technique with Phosphotungstic acid using bacterial culture of Bacillus subtilis. Negative staining is very convenient technique to view the structural morphology of different samples including bacteria, phage viruses and filaments in a cell. We could observe the bacterial cell wall and flagellum very well when trapped the negative stained biofilm from bacterial culture on a TEM grid. We cut ultra thin sections from the fixed root tips of Pisum sativum (Garden pea). Root tips were pre fixed with osmium tetroxide and post fixed with uranium acetate and placed in the BEEM capsule for block making. The ultrathin sections on the grid under TEM showed the granular chromatin in the nucleus. The protein bodies and large vacuoles with the storage materials were conspicuous. We followed fixation, critical point drying and sputter coating with gold to view the tissues with SEM after placing on stubs. SEM view of the leaf surface of a dangerous weed Tragia hispida showed the surface trichomes. These trichomes when break on touching releases poisonous content causing skin irritation. The cultured tissue from in vitro culture of Albizia lebbeck, a tree revealed the regenerative structures including leaf buds and stomata on the tissue surface. SEM and TEM allow investigating the minute details characteristic morphological features that can be used for classroom teaching.

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

    Directory of Open Access Journals (Sweden)

    Hengbo Li

    2016-06-01

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

  4. Microstructure and mechanical properties investigation of in situ TiB2 and ZrB2 reinforced Al-4Cu composites

    Science.gov (United States)

    Lutfi Anis, Ahmad; Ramli, Rosmamuhammadani; Darham, Widyani; Zakaria, Azlan; Talari, Mahesh Kumar

    2016-02-01

    Conventional Al-Cu alloys exhibit coarse grain structure leading to inferior mechanical properties in as-cast condition. Expensive thermo-mechanical treatments are needed to improve microstructure and corresponding mechanical properties. In situ Al-based composites were developed to improve mechanical properties by dispersion strengthening and grain refinement obtained by the presence of particulates in the melt during solidification. In this work Al-4Cu - 3TiB2 and Al-4Cu-3ZrB2 in situ composites were prepared by liquid casting method. XRD, electron microscopy and mechanical tests were performed on suitably sectioned and metallographically prepared surfaces to investigate the phase distribution, hardness and tensile properties. It was found that the reinforcement particles were segregated along the grain boundaries of Al dendrites. Tensile fracture morphology for both Al-4Cu - 3TiB2 and Al-4Cu-3ZrB2 were analyzed and compared to determine the fracture propagation mechanism in the composites. Al-4Cu-3ZrB2 in situ composites displayed higher strength and hardness compared to Al-4Cu-3TiB2 which could be ascribed to the stronger interfacial bonding between the Al dendrites and ZrB2 particulates as evidenced from fractographs.

  5. In Situ Investigation of the Evolution of Lattice Strain and Stresses in Austenite and Martensite During Quenching and Tempering of Steel

    Science.gov (United States)

    Villa, M.; Niessen, F.; Somers, M. A. J.

    2018-01-01

    Energy dispersive synchrotron X-ray diffraction was applied to investigate in situ the evolution of lattice strains and stresses in austenite and martensite during quenching and tempering of a soft martensitic stainless steel. In one experiment, lattice strains in austenite and martensite were measured in situ in the direction perpendicular to the sample surface during an austenitization, quenching, and tempering cycle. In a second experiment, the sin2 ψ method was applied in situ during the austenite-to-martensite transformation to distinguish between macro- and phase-specific micro-stresses and to follow the evolution of these stresses during transformation. Martensite formation evokes compressive stress in austenite that is balanced by tensile stress in martensite. Tempering to 748 K (475 °C) leads to partial relaxation of these stresses. Additionally, data reveal that (elastic) lattice strain in austenite is not hydrostatic but hkl dependent, which is ascribed to plastic deformation of this phase during martensite formation and is considered responsible for anomalous behavior of the 200 γ reflection.

  6. TEM-EELS: A personal perspective

    International Nuclear Information System (INIS)

    Egerton, R.F.

    2012-01-01

    The development of electron energy-loss spectroscopy in a transmission electron microscope (TEM-EELS) is illustrated through personal anecdote, highlighting some of the basic principles, instrumentation and personalities involved. The current state of the art is reviewed, together with some challenges for the future. -- Highlights: ► The history of EELS instrumentation is reviewed in a lighthearted manner. ► The current state of the art is summarized, together with some future possibilities. ► A couple of related mathematical puzzles are offered as a challenge to the reader.

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

    International Nuclear Information System (INIS)

    Du, Hongchu

    2015-01-01

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

  8. 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.

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

    Science.gov (United States)

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

    2017-11-01

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

  10. Revisión de investigaciones recientes sobre la aplicación de la Teoría de Respuesta al Ítem al Child Behavior Checklist Revision of recent investigations about the application of Item Response Theory to the Child Behavior Checklist

    Directory of Open Access Journals (Sweden)

    Facundo Juan Pablo Abal

    2010-12-01

    Full Text Available El Child Behavior Checklist (CBCL es un formulario que permite registrar problemas comportamentales y competencias sociales de niños y adolescentes. Si bien se construyó desde el enfoque clásico de la Teoría de los Test, investigaciones recientes mostraron la utilidad de aplicar la Teoría de Respuesta al Ítem (TRI para modelizar las variables del CBCL. El desarrollo de este trabajo revisa las consideraciones que se vieron obligados a tomar los respectivos autores para cumplir con las exigencias de los modelos de la TRI. Se describe la información que brindan las Curvas Características de los Ítems y cómo su análisis podría contribuir para optimizar el tiempo de administración del CBCL. Asimismo, se sintetizan los resultados alcanzados en relación con el estudio de la invarianza de las medidas obtenidas a través de adaptaciones transculturales de este formulario.The Child Behavior Checklist (CBCL is a questionnaire that allows the assessment of behavioral problems and social competences of children and adolescents. Although it was developed on the basis of the classical approach of the Test Theory, recent investigations have revealed the usefulness of applying the Item Response Theory (IRT to model the variables of CBCL. This paper revises the considerations made by the respective authors in order to meet the demands of the IRT models. The information provided by the Characteristic Curves of Items is described as well as the manner in which the analysis thereof might contribute to optimize the administration period of CBCL. Furthermore, the invariance of the measures obtained through transcultural adaptations of this questionnaire is analyzed and the results are summarized.

  11. 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...

  12. Investigation on microstructure and thermal properties of in-situ synthesized Cu-ZrO2 nanocomposites

    International Nuclear Information System (INIS)

    Elmahdy, Marwa; Abouelmagd, Gamal; Mazen, Asaad A.

    2017-01-01

    Cu-ZrO 2 nanocomposites were prepared by an in-situ reactive synthesis of copper nitrate Cu(NO 3 ) 2 and zirconium oxychloride ZrOCl 2 . Zirconia (ZrO 2 ) was added by 2.5, 5 and 10 wt.% to the Cu matrix to assess its effect on thermal conductivity and thermal expansion behavior. The results showed that ZrO 2 nanoparticles (30-50 nm) were homogeneously distributed in the copper matrix. The measured thermal conductivity for the Cu-ZrO 2 nanocomposites decreased from 372.8 to 94.4 W m -1 K -1 with increasing ZrO 2 content from 0 to 10 wt.%. Cu-10 wt.% ZrO 2 nanocomposite yields a low thermal conductivity of 94.4 W . m -1 K -1 along with a low coefficient of thermal expansion, 11.47 x 10 -6 K -1 .

  13. Adsorption of human insulin on single-crystal gold surfaces investigated by in situ scanning tunnelling microscopy and electrochemistry

    DEFF Research Database (Denmark)

    Welinder, Anna Christina; Zhang, Jingdong; Steensgaard, D.B.

    2010-01-01

    sweep, LSV, cyclic, CV, and square wave (SQWV) voltammetry. Multifarious electrochemical patterns were observed. Most attention was given to reductive desorption caused by insulin binding to the Au-surfaces via up to three disulfide groups per insulin monomer, presumably converted to single Au-S links....... SQWV suggested the Au-S bond strength order Au(111) > Au(110) > Au(100) based on the reductive desorption potentials. The voltammetric diversity was paralleled by different in situ STM insulin adsorption modes on the three surfaces. Single-molecule resolution was achieved in all cases. The coverage...... followed the order Au(110) > Au(100) > Au(111) and differs from the reductive desorption order that records the Au-S bonding element. Evenly distributed single molecules were scattered over large Au(111)-terraces, with intriguing molecular arrays disclosed near the terrace edges. In comparison, high...

  14. In situ DRIFTS investigation of NH3-SCR reaction over CeO2/zirconium phosphate catalyst

    Science.gov (United States)

    Zhang, Qiulin; Fan, Jie; Ning, Ping; Song, Zhongxian; Liu, Xin; Wang, Lanying; Wang, Jing; Wang, Huimin; Long, Kaixian

    2018-03-01

    A series of ceria modified zirconium phosphate catalysts were synthesized for selective catalytic reduction of NO with ammonia (NH3-SCR). Over 98% NOx conversion and 98% N2 selectivity were obtained by the CeO2/ZrP catalyst with 20 wt.% CeO2 loading at 250-425 °C. The interaction between CeO2 and zirconium phosphate enhanced the redox abilities and surface acidities of the catalysts, resulting in the improvement of NH3-SCR activity. The in situ DRIFTS results indicated that the NH3-SCR reaction over the catalysts followed both Eley-Rideal and Langmuir-Hinshelwood mechanisms. The amide (sbnd NH2) groups and the NH4+ bonded to Brønsted acid sites were the important intermediates of Eley-Rideal mechanism.

  15. In situ characterization of delamination and crack growth of a CGO–LSM multi-layer ceramic sample investigated by X-ray tomographic microscopy

    DEFF Research Database (Denmark)

    Bjørk, Rasmus; Esposito, Vincenzo; Lauridsen, Erik Mejdal

    2014-01-01

    The densification, delamination and crack growth behavior in a Ce0.9Gd0.1O1.95 (CGO) and (La0.85Sr0.15)0.9MnO3 (LSM) multi-layer ceramic sample was studied using in situ X-ray tomographic microscopy (microtomography) to investigate the critical dynamics of crack propagation and delamination...... in a multilayered sample. Naturally occurring defects, caused by the sample preparation process, are shown not to be critical in sample degradation. Instead defects are nucleated during the debinding step. Crack growth is significantly faster along the material layers than perpendicular to them, and crack growth...

  16. In situ investigation of the mechanisms of the transport to tissues of polycyclic aromatic hydrocarbons adsorbed onto the root surface of Kandelia obovata seedlings

    International Nuclear Information System (INIS)

    Li, Ruilong; Zhu, Yaxian; Zhang, Yong

    2015-01-01

    A novel method for in situ determination of the polycyclic aromatic hydrocarbons (PAHs) adsorbed onto the root surface of Kandelia obovata seedlings was established using laser-induced time-resolved nanosecond fluorescence spectroscopy (LITRF). The linear dynamic ranges for the established method were 1.5–1240 ng/spot for phenanthrene, 1.0–1360 ng/spot for pyrene and 5.0–1220 ng/spot for benzo[a]pyrene. Then, the mechanisms of PAHs transport from the Ko root surface to tissues were investigated. The three-phase model including fast, slow and very slow fractions was superior to the single or dual-phase model to describe the PAHs transport processes. Moreover, the fast fraction of PAHs transport process was mainly due to passive movement, while the slow and very slow fractions were not. Passive movement was the main process of B[a]P adsorbed onto Ko root surface transport to tissues. In addition, the extent of the PAHs transport to Ko root tissues at different salinity were evaluated. - Highlights: • A novel method in situ determination PAHs adsorbed onto root surface was established. • The mechanisms of PAHs transport from root surface to tissues are investigated. • Passive movement is the main process of B[a]P transport from root surface to tissues. • Effects of salinity on the PAHs transport from root surface to tissues are evaluated. - Passive movement for the PAHs adsorbed onto Kandelia obovata root surface to tissues was observed by a newly established in situ LITRF method

  17. A novel fabrication technology of in situ TiB2/6063Al composites: High energy ball milling and melt in situ reaction

    International Nuclear Information System (INIS)

    Zhang, S.-L.; Yang, J.; Zhang, B.-R.; Zhao, Y.-T.; Chen, G.; Shi, X.-X.; Liang, Z.-P.

    2015-01-01

    Highlights: • This paper presents a novel technology to fabricate the TiB 2 /6063Al composites. • The novel technology decreases in situ reaction temperature and shortens the time. • The reaction mechanism of in situ reaction at the low temperature is discussed. • Effect of ball milling time and in situ reaction time on the composites is studied. - Abstract: TiB 2 /6063Al matrix composites are fabricated from Al–TiO 2 –B 2 O 3 system by the technology combining high energy ball milling with melt in situ reaction. The microstructure and tensile properties of the composites are investigated by XRD, SEM, EDS, TEM and electronic tensile testing. The results indicate that high energy ball milling technology decreases the in situ reaction temperature and shortens the reaction time for Al–TiO 2 –B 2 O 3 system in contrast with the conventional melt in situ synthesis. The morphology of in situ TiB 2 particles is exhibited in irregular shape or nearly circular shape, and the average size of the particles is less than 700 nm, thereinto the minimum size is approximately 200 nm. In addition, the morphology and size of the reinforced particles are affected by the time of ball milling and in situ reaction. TEM images indicate that the interface between 6063Al matrix and TiB 2 particles is clear and no interfacial outgrowth is observed. Tensile testing results show that the as-cast TiB 2 /6063Al composites exhibit a much higher strength, reaching 191 MPa, which is 1.23 times as high as the as-cast 6063Al matrix. Besides, the tensile fracture surface of the composites displays the dimple-fracture character

  18. A novel fabrication technology of in situ TiB{sub 2}/6063Al composites: High energy ball milling and melt in situ reaction

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, S.-L.; Yang, J. [School of Materials Science and Engineering, Jiangsu University, Zhenjiang, Jiangsu 212013 (China); Zhang, B.-R. [School of Mechanical Engineering, Qilu University of Technology, Jinan, Shandong 250022 (China); Zhao, Y.-T., E-mail: 278075525@qq.com [School of Materials Science and Engineering, Jiangsu University, Zhenjiang, Jiangsu 212013 (China); Chen, G.; Shi, X.-X.; Liang, Z.-P. [School of Materials Science and Engineering, Jiangsu University, Zhenjiang, Jiangsu 212013 (China)

    2015-08-05

    Highlights: • This paper presents a novel technology to fabricate the TiB{sub 2}/6063Al composites. • The novel technology decreases in situ reaction temperature and shortens the time. • The reaction mechanism of in situ reaction at the low temperature is discussed. • Effect of ball milling time and in situ reaction time on the composites is studied. - Abstract: TiB{sub 2}/6063Al matrix composites are fabricated from Al–TiO{sub 2}–B{sub 2}O{sub 3} system by the technology combining high energy ball milling with melt in situ reaction. The microstructure and tensile properties of the composites are investigated by XRD, SEM, EDS, TEM and electronic tensile testing. The results indicate that high energy ball milling technology decreases the in situ reaction temperature and shortens the reaction time for Al–TiO{sub 2}–B{sub 2}O{sub 3} system in contrast with the conventional melt in situ synthesis. The morphology of in situ TiB{sub 2} particles is exhibited in irregular shape or nearly circular shape, and the average size of the particles is less than 700 nm, thereinto the minimum size is approximately 200 nm. In addition, the morphology and size of the reinforced particles are affected by the time of ball milling and in situ reaction. TEM images indicate that the interface between 6063Al matrix and TiB{sub 2} particles is clear and no interfacial outgrowth is observed. Tensile testing results show that the as-cast TiB{sub 2}/6063Al composites exhibit a much higher strength, reaching 191 MPa, which is 1.23 times as high as the as-cast 6063Al matrix. Besides, the tensile fracture surface of the composites displays the dimple-fracture character.

  19. Environmental TEM in an Aberration Corrected Microscope

    DEFF Research Database (Denmark)

    Hansen, Thomas Willum; Wagner, Jakob Birkedal

    ‐resolution imaging. A gaseous atmosphere in the pole‐piece gap of the objective lens of the microscope alters both the incoming electron wave prior to interaction with the sample and the outgoing wave below the sample. Whereas conventional TEM samples are usually thin (below 10‐20 nm), the gas in the environmental...... the microscope column. The effects of gas on the electron wave in the objective lens are not well understood and needs further attention. Imaging samples with a simple geometry, such as gold particles on a flat graphene substrate and analyzing the variations in contrast, provides a means for understanding...... results from imaging in various elemental as well as di‐molecular gases and their effect on imaging and spectroscopy in the environmental transmission electron microscope....

  20. Portable XRF as a valuable device for preliminary in situ pigment investigation of wooden inventory in the Trski Vrh Church in Croatia

    International Nuclear Information System (INIS)

    Desnica, V.; Skaric, K.; Mudronja, D.; Pavlicic, M.; Peranic, I.; Jembrih-Simbuerger, D.; Schreiner, M.; Fazinic, S.; Jaksic, M.

    2008-01-01

    The aim of this work was the investigation of pigments from the painted wooden inventory of the pilgrimage church of Saint Mary of Jerusalem in Trski Vrh - one of the most beautiful late-baroque sacral ensembles in Croatia. Being an object of high relevance for the national cultural heritage, an extensive research on the wooden polychromy was undertaken in order to work out a proposal for a conservation treatment. It consists mainly of two painted and gilded layers (the original one from the 18th century and a later one from 1903), partly overpainted during periodic conservation treatments in the past. The approach was to carry out extensive preliminary in situ pigment investigations using a portable XRF (X-ray fluorescence) device, and only the problems not resolved by this method on site were further analyzed using sophisticated laboratory equipment. Therefore, the XRF results acted as a valuable guideline for subsequent targeted sampling actions, thus minimizing the sampling damage. Important questions not answered by XRF (identification of organic pigments, ultramarine, etc.) were subsequently resolved using additional ex situ laboratory methods, primarily μ-PIXE (particle-induced X-ray emission) at the nuclear microprobe of the Rudjer Boskovic accelerator facility as well as μ-Raman spectroscopy at the Institute of the Academy of Fine Arts in Vienna. It is shown that by the combination of these often complementary methods a thorough characterization of each pigment can be obtained, allowing for a proper strategy of the conservation treatment. (orig.)

  1. Laetiporus sulphureus, edible mushroom from Serbia: investigation on volatile compounds, in vitro antimicrobial activity and in situ control of Aspergillus flavus in tomato paste.

    Science.gov (United States)

    Petrović, Jovana; Glamočlija, Jasmina; Stojković, Dejan S; Ćirić, Ana; Nikolić, Miloš; Bukvički, Danka; Guerzoni, Maria Elisabetta; Soković, Marina D

    2013-09-01

    The volatile compounds of fruiting bodies of wild Laetiporus sulphureus (Bull.) Murrill, growing on willow trees from Serbia, were isolated and extracted using methanol, acetone and dichloromethane and investigated by GC/MS-SPME. A total of 56 components were identified in the extracts. Hydrocarbons predominated (76.90%, 77.20%, and 43.10%) in dichloromethane, acetone and methanol extracts, respectively. Fatty acids, esters and sesquiterpenes were present in amounts equal or lower than 2.00%. Ketones were represented with moderate amount with the exception of methanol extract where it reached as much as 28.90% of the total investigated compounds. Extracts were also tested for antimicrobial activity with and without the addition of food additive - potassium disulfite in vitro against eight bacterial and eight fungal species, and in situ in tomato paste against Aspergillus flavus. All the tested extracts showed good antimicrobial activity, but methanol extract with addition of E224 showed the best antimicrobial activity in vitro. In situ results indicate complete inhibition of A. flavus growth in tomato paste after 15 days of the treatment. This study is the first report on volatile composition of L. sulphureus growing wild in Serbia. We describe for the first time the application of its extract as antifungal food preservative. Copyright © 2013 Elsevier Ltd. All rights reserved.

  2. In situ investigation by X-ray tomography of the overall and local microstructural changes occurring during partial remelting of an Al-15.8 wt.% Cu alloy

    International Nuclear Information System (INIS)

    Limodin, Nathalie; Salvo, Luc; Suery, Michel; DiMichiel, Marco

    2007-01-01

    The paper is concerned with the study of the microstructural changes occurring during holding of an Al-15.8 wt.% Cu alloy in the semi-solid state. These changes are investigated in 3D by in situ X-ray tomography carried out at the temperature of the treatment. The studies are classified in two categories: overall changes by measuring average values of characteristic parameters, and local changes by considering the evolution of individual necks between particles. It is shown in particular that the size of the solid particles or the surface area of the solid-liquid interfaces do not follow the classical power laws but rather evolve in a slower manner. Local observations confirm that these results are due to the competition of two coarsening mechanisms of the solid particles that occur simultaneously: dissolution of a small particle to the benefit of one or several bigger ones by an Ostwald-type mechanism and the growth of necks between solid particles due to their coalescence. Complex variations of neck size result from these mechanisms which can be explained only by considering the neighbourhood of the particles under investigation. These observations confirm that in situ X-ray tomography is a very powerful tool to provide data that are representative of the semi-solid state and to observe in real time the mechanisms that act on the microstructure

  3. In-situ investigation of crack propagation in {gamma}-TiAl alloys using atomic force, focus ion beam and scanning electron microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Iqbal, Farasat; Goeken, Mathias [Lehrstuhl Allgemeine Werkstoffeigenschaften, Friedrich-Alexander-Universitaet Erlangen-Nuernberg (Germany); Pyczak, Florian [GKSS Research Centre Geesthacht, Geesthacht (Germany)

    2009-07-01

    The present study is focused on crack propagation mechanism in Ti-45Al-1Cr and Ti-45Al-5Nb alloys with lamellar microstructure. Atomic force microscopy (AFM) is a versatile technique to study the crack propagation in-situ. AFM was employed to investigate the local deformations near the crack tip. Scanning electron microscopy (SEM) supplements the in-situ observations and was used to get a basic understanding of the crack propagation path over larger distances.A focused ion beam (FIB) was used to investigate the structures and deformation traces underneath the surface. It is concluded that the {gamma}/{alpha}2 interfaces act as favorable sites for new interfacial crack nucleation and also for interlamellar crack propagation. Nucleation of new cracks was often preceded by the interaction of deformation twins with interfaces and also by strong shear band activity in the {gamma}-TiAl lamellae visible as significant surface topography in AFM.Mostly the underneath crack path follows the {gamma}/{alpha}2 interface similar to the situation observed at the surface. The local misorientation measured with electron backscattered diffraction (EBSD) shows {gamma}-lamellae as the region of high deformation as compare to neighboring {alpha}2 -lamellae around the crack tip and its surroundings.

  4. Repeated sorption of water in SBA-15 investigated by means of in situ small-angle x-ray scattering

    International Nuclear Information System (INIS)

    Erko, M; Paris, O; Wallacher, D; Findenegg, G H

    2012-01-01

    The effect of repeated cycles of water adsorption/desorption on the structural stability of ordered mesoporous silica SBA-15 is studied by small-angle x-ray scattering (SAXS). In situ sorption measurements are conducted using a custom-built sorption apparatus in connection with a laboratory SAXS setup. Two striking irreversible changes are observed in the sorption isotherms as derived from the integrated SAXS intensity. First, the capillary condensation pressure shifts progressively to lower relative pressure values with increasing number of sorption cycles. This effect is attributed to chemisorption of water at the silica walls, resulting in a change of the fluid-wall interaction. Second, the sorption cycles do not close completely at vanishing vapour pressure, suggesting that progressively more water remains trapped within the porous material after each cycle. This effect is interpreted to be the result of an irreversible collapse of parts of mesopores, originating from pore wall deformation due to the large Laplace pressure of water acting on the pore walls at capillary condensation and capillary evaporation. (paper)

  5. Investigation on microstructure and thermal properties of in-situ synthesized Cu-ZrO{sub 2} nanocomposites

    Energy Technology Data Exchange (ETDEWEB)

    Elmahdy, Marwa [Higher Technological Institute, Tenth of Ramadan (Egypt). Mechanical Dept.; Abouelmagd, Gamal; Mazen, Asaad A. [Minia Univ. (Egypt). Production Engineering and Design Dept.

    2017-12-15

    Cu-ZrO{sub 2} nanocomposites were prepared by an in-situ reactive synthesis of copper nitrate Cu(NO{sub 3}){sub 2} and zirconium oxychloride ZrOCl{sub 2}. Zirconia (ZrO{sub 2}) was added by 2.5, 5 and 10 wt.% to the Cu matrix to assess its effect on thermal conductivity and thermal expansion behavior. The results showed that ZrO{sub 2} nanoparticles (30-50 nm) were homogeneously distributed in the copper matrix. The measured thermal conductivity for the Cu-ZrO{sub 2} nanocomposites decreased from 372.8 to 94.4 W m{sup -1} K{sup -1} with increasing ZrO{sub 2} content from 0 to 10 wt.%. Cu-10 wt.% ZrO{sub 2} nanocomposite yields a low thermal conductivity of 94.4 W . m{sup -1} K{sup -1} along with a low coefficient of thermal expansion, 11.47 x 10{sup -6} K{sup -1}.

  6. A new system for sodium flux growth of bulk GaN. Part II: in situ investigation of growth processes

    KAUST Repository

    Von Dollen, Paul

    2016-09-09

    We report recent results of bulk GaN crystal growth using the sodium flux method in a new crucible-free growth system. We observed a (0001) Ga face (+c-plane) growth rate >50 µm/h for growth at a N2 overpressure of ~5 MPa and 860 °C, which is the highest crystal growth rate reported for this technique to date. Omega X-ray rocking curve (ω-XRC) measurements indicated the presence of multiple grains, though full width at half maximum (FWHM) values for individual peaks were <100 arcseconds. Oxygen impurity concentrations as measured by secondary ion mass spectroscopy (SIMS) were >1020 atoms/cm3. By monitoring the nitrogen pressure decay over the course of the crystal growth, we developed an in situ method that correlates gas phase changes with precipitation of GaN from the sodium-gallium melt. Based on this analysis, the growth rate may have actually been as high as 90 µm/h, as it would suggest GaN growth ceased prior to the end of the run. We also observed gas phase behavior identified as likely characteristic of GaN polynucleation.

  7. High-voltage electron-microscope investigation of point-defect agglomerates in irradiated copper during in-situ annealing

    International Nuclear Information System (INIS)

    Jaeger, W.; Urban, K.; Frank, W.

    1980-01-01

    Thin copper foils were irradiated with 650 keV electrons at 10 K in a high-voltage electron microscope (HVEM) to doses phi in the range 2 x 10 23 electrons/m 2 approximately 25 electrons /m 2 and then annealed in situ up to room temperature and outside the HVEM between room temperature and 470 K. During irradiation visible defect clusters were formed only at phi >= 2.5 x 10 24 electrons/m 2 . At smaller doses defect clusters became visible after annealing at 50 K. Between 50 K and 120 K further clusters, mainly dislocation loops on brace111 planes, appeared. Above 120 K, particularly between 160 K and 300 K, some of the dislocation loops became glissile. They glided out of the specimens or agglomerated to larger clusters of frequently complex shapes. As a consequence between 160 K and 300 K the cluster density decreased strongly, whereas the mean cluster size increased monotonously through the entire range of annealing temperatures covered. Contrast analyses between 180 K and 400 K revealed that the great majority of the dislocation loops were of interstitial type. At 470 K a new type of small clusters emerged, presumably of vacancy type. These observations are compared with other studies on electron-irradiated copper and with the current models of radiation damage in metals. (author)

  8. A new system for sodium flux growth of bulk GaN. Part II: in situ investigation of growth processes

    KAUST Repository

    Von Dollen, Paul; Pimputkar, Siddha; Alreesh, Mohammed Abo; Nakamura, Shuji; Speck, James S.

    2016-01-01

    We report recent results of bulk GaN crystal growth using the sodium flux method in a new crucible-free growth system. We observed a (0001) Ga face (+c-plane) growth rate >50 µm/h for growth at a N2 overpressure of ~5 MPa and 860 °C, which is the highest crystal growth rate reported for this technique to date. Omega X-ray rocking curve (ω-XRC) measurements indicated the presence of multiple grains, though full width at half maximum (FWHM) values for individual peaks were <100 arcseconds. Oxygen impurity concentrations as measured by secondary ion mass spectroscopy (SIMS) were >1020 atoms/cm3. By monitoring the nitrogen pressure decay over the course of the crystal growth, we developed an in situ method that correlates gas phase changes with precipitation of GaN from the sodium-gallium melt. Based on this analysis, the growth rate may have actually been as high as 90 µm/h, as it would suggest GaN growth ceased prior to the end of the run. We also observed gas phase behavior identified as likely characteristic of GaN polynucleation.

  9. Investigation of the 2006 Alexandrium fundyense Bloom in the Gulf of Maine: In situ Observations and Numerical Modeling.

    Science.gov (United States)

    Li, Yizhen; He, Ruoying; McGillicuddy, Dennis J; Anderson, Donald M; Keafer, Bruce A

    2009-09-30

    In situ observations and a coupled bio-physical model were used to study the germination, initiation, and development of the Gulf of Maine (GOM) Alexandrium fundyense bloom in 2006. Hydrographic measurements and comparisons with GOM climatology indicate that 2006 was a year with normal coastal water temperature, salinity, current and river runoff conditions. A. fundyense cyst abundance in bottom sediments preceding the 2006 bloom was at a moderate level compared to other recent annual cyst survey data. We used the coupled bio-physical model to hindcast coastal circulation and A. fundyense cell concentrations. Field data including water temperature, salinity, velocity time series and surface A. fundyense cell concentration maps were applied to gauge the model's fidelity. The coupled model is capable of reproducing the hydrodynamics and the temporal and spatial distributions of A. fundyense cell concentration reasonably well. Model hindcast solutions were further used to diagnose physical and biological factors controlling the bloom dynamics. Surface wind fields modulated the bloom's horizontal and vertical distribution. The initial cyst distribution was found to be the dominant factor affecting the severity and the interannual variability of the A. fundyense bloom. Initial cyst abundance for the 2006 bloom was about 50% of that prior to the 2005 bloom. As the result, the time-averaged gulf-wide cell concentration in 2006 was also only about 60% of that in 2005. In addition, weaker alongshore currents and episodic upwelling-favorable winds in 2006 reduced the spatial extent of the bloom as compared with 2005.

  10. In situ x-ray diffraction investigations during low energy ion nitriding of austenitic stainless steel grade 1.4571

    International Nuclear Information System (INIS)

    Manova, D; Mändl, S; Gerlach, J W; Hirsch, D; Neumann, H; Rauschenbach, B

    2014-01-01

    Insertion of nitrogen into austenitic stainless steel leads to anomalously fast nitrogen diffusion and the formation of an expanded face-centred cubic phase which is known to contain a large amount of mechanical stress. In situ x-ray diffraction (XRD) measurements during low energy nitrogen ion implantation into steel 316Ti at 300–550 °C allow a direct view into diffusion and phase formation. While the layer growth is directly observable from the decreasing substrate reflection intensity, the time evolution of the intensities for the expanded phase reflection is much more complex: several mechanisms including at least formation and annealing of defects, twinning, reduction of the crystal symmetry, or grain rotation may be active inside the expanded phase, besides the thermally activated decay of the metastable expanded phase. This locally varying coherence length or scattering intensity from the expanded phase is furthermore a function of temperature and time, additionally complicating the deconvolution of XRD spectra for stress and concentration gradients. As no concise modelling of this coherence length is possible at present, a simple qualitative model assuming a dependence of the scattering intensity on the depth, influence by stress and plastic flow during the nitriding process is proposed for understanding the underlying processes. (paper)

  11. An Investigation of Operational Decision Making in Situ: Incident Command in the U.K. Fire and Rescue Service.

    Science.gov (United States)

    Cohen-Hatton, Sabrina R; Butler, Philip C; Honey, Robert C

    2015-08-01

    The aim of this study was to better understand the nature of decision making at operational incidents in order to inform operational guidance and training. Normative models of decision making have been adopted in the guidance and training for emergency services. In these models, it is assumed that decision makers assess the current situation, formulate plans, and then execute the plans. However, our understanding of how decision making unfolds at operational incidents remains limited. Incident commanders, attending 33 incidents across six U.K. Fire and Rescue Services, were fitted with helmet-mounted cameras, and the resulting video footage was later independently coded and used to prompt participants to provide a running commentary concerning their decisions. The analysis revealed that assessment of the operational situation was most often followed by plan execution rather than plan formulation, and there was little evidence of prospection about the potential consequences of actions. This pattern of results was consistent across different types of incident, characterized by level of risk and time pressure, but was affected by the operational experience of the participants. Decision making did not follow the sequence of phases assumed by normative models and conveyed in current operational guidance but instead was influenced by both reflective and reflexive processes. These results have clear implications for understanding operational decision making as it occurs in situ and suggest a need for future guidance and training to acknowledge the role of reflexive processes. © 2015, Human Factors and Ergonomics Society.

  12. Investigation of TL properties of sand collected from sewage sludge as an ''in situ'' dosimeter in radiation disinfection

    International Nuclear Information System (INIS)

    Benny, P.G.; Bhatt, B.C.

    1996-01-01

    Thermoluminescence (TL) properties of sand, collected from sewage sludge, were studied after extensive cleaning procedures. In the sand samples treated with either hydrogen peroxide (H 2 O 2 ) or hydrofluoric acid (HF), there was a prominent TL peak at about 220 o C after γ-irradiation and 120 o C, 20 min post-irradiation annealing treatment. The dose vs TL response curves in hydrogen-peroxide-treated and HF-treated sand samples were found to be linear up to 30 and 100 Gy, respectively, beyond which they were supra-linear. The extent of post-irradiation fading in the sand sample, which was treated with H 2 O 2 and post-irradiation annealed at 120 o C for 20 min, was observed to be 8% after 21 days, while no detectable fading was observed for the sample which was HF treated and annealed at 120 o C for 20 min after γ-irradiation. Therefore, H 2 O 2 - as well as HF-treated sludge sand samples could be considered for use as in situ TL dosimeters for radiation disinfection of sewage sludge. (Author)

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

    African Journals Online (AJOL)

    GREGO

    2007-03-05

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

  14. 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.

  15. 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....

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

    Directory of Open Access Journals (Sweden)

    Nobuo Tanaka

    2008-01-01

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

  17. In situ probing of the evolution of irradiation-induced defects in copper

    International Nuclear Information System (INIS)

    Li, N.; Hattar, K.; Misra, A.

    2013-01-01

    Through in situ Cu 3+ ion irradiation at room temperature in a transmission electron microscope (TEM), we have investigated the evolution of defect clusters as a function of the radiation dose at different distances from the 3 {1 1 2} incoherent twin boundary (ITB) in Cu. Post in situ ion irradiation, high resolution TEM was used to explore the types of defects, which are composed of a high-density of vacancy stacking fault tetrahedra (SFT) and sparsely distributed interstitial Frank loops. During irradiation, defect clusters evolve through four stages: (i) incubation, (ii) non-interaction, (iii) interaction and (iv) saturation; and the corresponding density was observed to initially increase with irradiation dose and then approach saturation. No obvious denuded zone is observed along the 3 {1 1 2} ITB and the configuration of defects at the boundary displays as truncated SFTs. Several defect evolution models have been proposed to explain the observed phenomena

  18. TEM analysis of fine sulphides dissolution and precipitation in steel

    International Nuclear Information System (INIS)

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

    2003-01-01

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

  19. Investigation of the reversible sodiation of Sn foil by ex-situ X-ray diffractometry and Mössbauer effect spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Du, Zhijia [Department of Physics and Atmospheric Science, Dalhousie University, P.O. Box 15000, Halifax, Nova Scotia B3H 4R2 (Canada); Dunlap, R.A. [Department of Physics and Atmospheric Science, Dalhousie University, P.O. Box 15000, Halifax, Nova Scotia B3H 4R2 (Canada); Institute for Research in Materials, Dalhousie University, P.O. Box 15000, Halifax, Nova Scotia B3H 4R2 (Canada); College of Sustainability, Dalhousie University, P.O. Box 15000, Halifax, Nova Scotia B3H 4R2 (Canada); Obrovac, M.N., E-mail: mobrovac@dal.ca [Department of Physics and Atmospheric Science, Dalhousie University, P.O. Box 15000, Halifax, Nova Scotia B3H 4R2 (Canada); Institute for Research in Materials, Dalhousie University, P.O. Box 15000, Halifax, Nova Scotia B3H 4R2 (Canada); Department of Chemistry, Dalhousie University, P.O. Box 15000, Halifax, Nova Scotia B3H 4R2 (Canada)

    2014-12-25

    Highlights: • Mössbauer spectra of all phases formed during sodiation measured for the first time. • Center shifts correlated with metallurgically prepared samples. • Center shift correlated with Na content in Na–Sn. - Abstract: The reversible sodiation of Sn foil was investigated using ex-situ X-ray diffractometry (XRD) and Mössbauer effect spectroscopy. The measured voltage profile indicated that the sodiation process of Sn foil proceeded in three stages. Ex-situ XRD patterns demonstrated that Na{sub 4}Sn{sub 4}, Na{sub 5}Sn{sub 2} and Na{sub 15}Sn{sub 4} phases were formed at the end of each discharge plateau. Na{sub 5}Sn{sub 2}, Na{sub 4}Sn{sub 4} and β-Sn were formed at the end of each charge plateau. Three single-phase alloys, Na{sub 4}Sn{sub 4}, Na{sub 9}Sn{sub 4} and Na{sub 15}Sn{sub 4}, were prepared by annealing stoichiometric ratios of Na and Sn. The Mössbauer spectra of ex-situ samples at the end of each discharge plateau were collected and compared with the Mössbauer spectra of the three single phase alloys. The measured parameters for the Mössbauer effect spectra were consistent with an analysis of the crystal structures. The center shift became less positive with an increase of the sodium content in Na–Sn phases and this was shown to be a useful indicator of the degree of sodiation of Sn electrodes.

  20. 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.

  1. Radiological investigations at the 'Taiga' nuclear explosion site: Site description and in situ measurements

    Energy Technology Data Exchange (ETDEWEB)

    Ramzaev, V., E-mail: V.Ramzaev@mail.ru [Institute of Radiation Hygiene, Mira str. 8, 197101 St.-Petersburg (Russian Federation); Repin, V.; Medvedev, A.; Khramtsov, E.; Timofeeva, M.; Yakovlev, V. [Institute of Radiation Hygiene, Mira str. 8, 197101 St.-Petersburg (Russian Federation)

    2011-07-15

    In the summer of 2009, we performed a field survey of the 'Taiga' peaceful underground nuclear explosion site, the Perm region, Russia (61.30{sup o} N, 56.60{sup o} E). The explosion was carried out by the USSR in 1971. This paper provides an extended summary of the available published data on the 'Taiga' experiment. A detailed description of the site is illustrated by original aerial and ground-level photos. A large artificial lake (700 m long and 350 m wide) currently occupies the central area of the experimental site. The ground lip surrounding the lake is covered by a newly grown mixed forest. In situ measurements, performed in August 2009, revealed elevated levels of the {gamma}-ray dose rate in air on the banks of the lake 'Taiga'. Two hot spots were detected on the eastern bank of the lake. The excess of the {gamma}-ray radiation is attributable to the man-made radionuclides {sup 60}Co and {sup 137}Cs. The current external {gamma}-ray dose rate to a human from the contaminations associated with the 'Taiga' experiment was between 9 and 70 {mu}Sv per week. Periodic monitoring the site is recommended. - Highlights: > We studied a radiation anomaly at the 'Taiga' underground nuclear explosion site. > The anomaly currently has an area of approximately 1 km{sup 2}. > The excess of {gamma}-ray radiation at the site is mainly attributable to {sup 60}Co and {sup 137}Cs. > The external effective dose may currently exceed the negligible value of 10 {mu}Sv y{sup -1}.

  2. Modelling the Small Throw Fault Effect on the Stability of a Mining Roadway and Its Verification by In Situ Investigation

    Directory of Open Access Journals (Sweden)

    Małkowski Piotr

    2017-12-01

    Full Text Available The small throw fault zones cause serious problems for mining engineers. The knowledge about the range of fractured zone around the roadway and about roadway’s contour deformations helps a lot with the right support design or its reinforcement. The paper presents the results of numerical analysis of the effect of a small throw fault zone on the convergence of the mining roadway and the extent of the fracturing induced around the roadway. The computations were performed on a dozen physical models featuring various parameters of rock mass and support for the purpose to select the settings that reflects most suitably the behavior of tectonically disturbed and undisturbed rocks around the roadway. Finally, the results of the calculations were verified by comparing them with in situ convergence measurements carried out in the maingate D-2 in the “Borynia-Zofiówka-Jastrzębie” coal mine. Based on the results of measurements it may be concluded that the rock mass displacements around a roadway section within a fault zone during a year were four times in average greater than in the section tectonically unaffected. The results of numerical calculations show that extent of the yielding zone in the roof reaches two times the throw of the fault, in the floor 3 times the throw, and horizontally approx. 1.5 to 1.8 times the width of modelled fault zone. Only a few elasto-plastic models or models with joints between the rock beds can be recommended for predicting the performance of a roadway which is within a fault zone. It is possible, using these models, to design the roadway support of sufficient load bearing capacity at the tectonically disturbed section.

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

    Science.gov (United States)

    Christopher, R. G.

    1981-01-01

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

  4. In-situ investigation of martensite formation in AISI 52100 bearing steel at sub-zero Celsius temperature

    DEFF Research Database (Denmark)

    Villa, Matteo; Hansen, Mikkel Fougt; Pantleon, Karen

    2013-01-01

    Martensite formation in AISI 52100 bearing steel at sub-zero Celsius temperature was investigated with Vibrating Sample Magnetometry. The investigation reports the stabilization of retained austenite in quenched samples during storage at room temperature and reveals the thermally activated nature...

  5. In-situ investigation of the order-disorder transition in Cu2ZnSnSe4 by optical transmission spectroscopy

    Directory of Open Access Journals (Sweden)

    Christiane Stroth

    2017-02-01

    Full Text Available The existence of disorder is one possible reason for the limited performance of kesterite solar cells. Therefore further knowledge of the order-disorder phase transition, of factors which influence the degree of order and of methods to determine this material property is still required. In this study we investigated the order-disorder transition in the kesterite material Cu2ZnSnSe4 by in-situ optical transmission spectroscopy during heat treatments. We show in-situ results for the temperature dependence of the band gap and its tailing properties. The influence of cooling rates on the phase transition was analyzed as well as the ordering kinetics during annealing at a constant temperature. The critical temperature of the phase transition was determined and the existence of a control temperature range is shown, which allows for controlling the degree of order by the cooling rate within this range. Additionally we performed Raman analysis to link Raman spectra to the degree of order in Cu2ZnSnSe4. A correlation between the intensity ratio of A-modes as well as B-/ E- Raman modes and the degree of order was found.

  6. Modulation of Calcium Oxalate Crystallization by Proteins and Small Molecules Investigated by In Situ Atomic Force Microscopy

    Science.gov (United States)

    Qiu, R.; Orme, C.; Cody, A. M.; Wierzbicki, A.; Hoyer, J.; Nancollas, G.; de Yoreo, J.

    2002-12-01

    Understanding the physical mechanisms by which biological inhibitors control nucleation and growth of inorganic crystals is a major focus of biomineral research. Calcium oxalate monohydrate (COM), which plays a functional role in plant physiology, is also a source of pathogenesis in humans where it causes kidney stone disease. Although a great deal of research has been carried out on the modulation COM by proteins and small molecules, the basic mechanism has not yet been understood. However, because the proteins that play a role in COM growth have been identified and sequenced, COM provides an excellent model system for research into biomineral growth. In this study, in situ atomic force microscopy (AFM) was used to monitor the COM surface under controlled growth conditions both from pure solutions and those doped with citrate and osteopontin (OPN) in order to determine their effects on surface morphology and growth dynamics at the molecular level. As with other solution-grown crystals such as calcite, COM grows on complex dislocation hillocks. In pure solution, while growth on the (010) face is isotropic, hillocks on the (-101) face exhibit anisotropic step kinetics. Steps of [-10-1] and orientation are clearly delineated with the [-10-1] being the fast growing direction. When citrate is added to the solution, both growth rate and morphology are drastically changed on (-101) face, especially along the [-10-1] direction. This results in isotropic disc-shaped hillocks a shape that is then reflected in the macroscopic growth habit. In contrast, no large growth changes were observed on the (010) facet. At the same time, molecular modeling predicts an excellent fit of the citrate ion into the (-101) plane and a poor fit to the (010) face. Here we propose a model that reconciles the step-specific interactions implied by the AFM results with the face-specific predictions of the calculations. Finally, we present the results of doping with aspartic acid as well as OPN, an

  7. In-situ Optical Spectroscopy Investigation of Water and Its influence on Forsterite Transformation in Supercritical CO2

    Science.gov (United States)

    Wang, Z.; Thompson, C. J.; Joly, A. G.; Sklarew, D. S.; Poindexter, L.; Rosso, K. M.

    2009-12-01

    Carbon capture and sequestration (CCS) from coal/gas-burning power plants is currently viewed as one of the most promising technologies for mitigating green house gas emissions. This strategy involves injection of supercritical CO2 (scCO2) into deep geological formations such as depleted oil and gas reservoirs and deep saline aquifers. The feasibility of this approach and the ultimate fate of the stored CO2 are determined by the interactions between scCO2, various minerals in the rock formations, and the host fluids. Currently, there is only limited knowledge about both the thermodynamic and kinetic aspects of the physical and chemical processes that occur between scCO2 and relevant minerals, such as metal silicates and metal aluminosilicates, and the role of water activity for catalyzing mineral transformation reactions. In this work, we have developed a modular in situ optical spectroscopic platform that integrates a scCO2 generation and manipulation system with an array of optical and laser spectroscopies including UV-visible, IR, Raman and laser fluorescence spectroscopy. We have used the system to study i) the dissolution and quantification of H2O/D2O in scCO2 and ii) interaction between scCO2 and a model metal silicate, forsterite (Mg2SiO4), and the effects of the presence of water under variable pressure, temperature and water content. Our results showed that H2O and D2O have unique IR spectral features over a broad spectral range from 700 cm-1 to ~ 2900 cm-1 in scCO2 and their concentrations are directly proportional to the characteristic IR bands that correspond to their stretching (D2O) and bending frequencies (both D2O and H2O). These bands offer a unique spectroscopic signature useful for qualitative and quantitative analysis of the properties and reactivity of small amounts of H2O in scCO2. metal carbonation reactions relevant to sequestration.

  8. In situ characterization of martian materials and detection of organic compounds with the MOMA investigation onboard the ExoMars rover

    Science.gov (United States)

    Arevalo, R. D., Jr.; Grubisic, A.; van Amerom, F. H. W.; Danell, R.; Li, X.; Kaplan, D.; Pinnick, V. T.; Brinckerhoff, W. B.; Getty, S.; Goesmann, F.

    2017-12-01

    Ground-based observations (e.g., via the NASA Infrared Telescope Facility) and in situ investigations, including flybys (e.g., Mariner Program), orbiters (most recently MAVEN and ExoMars TGO), stationary landers (i.e., Viking, Pathfinder and Phoenix), and mobile rovers (i.e., Sojourner, Spirit/Opportunity and Curiosity), have enabled the progressive exploration of the Martian surface. Evidence for liquid water, manifest as hydrated and amorphous materials representative of alteration products of primary minerals/lithologies, and geomorphological features such as recurring slope lineae (RSL), valley networks and open-basin lakes, indicates that Mars may have hosted habitable environments, at least on local scales (temporally and spatially). However, the preservation potential of molecular biosignatures in the upper meter(s) of the surface is limited by destructive cosmic radiation and oxidative chemical reactions. Moreover, the determination of indigenous versus exogenous origins, and biotic versus abiotic formation mechanisms of detected organic material, provide additional challenges for future missions to the red planet. The Mars Organic Molecule Analyzer (MOMA) onboard the ExoMars rover, set to launch in 2020, provides an unprecedented opportunity to discover unambiguous indicators of life. The MOMA instrument will investigate the compositions of materials collected during multiple vertical surveys, extending as deep as two meters below the surface, via: i) gas chromatography mass spectrometry, a method geared towards the detection of volatile organics and the determination of molecular chirality, mapping to previous in situ Mars investigations; and, ii) laser desorption mass spectrometry, a technique commonly employed in research laboratories to detect larger, more refractory organic materials, but a first for spaceflight applications. Selective ion excitation and tandem mass spectrometry (MS/MS) techniques support the isolation and disambiguation of complex

  9. 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.

  10. 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.

  11. In situ spectroscopic investigation of the cobalt-catalyzed oxidation of lignin model compounds in ionic liquids

    NARCIS (Netherlands)

    Zakzeski, J.|info:eu-repo/dai/nl/326160256; Bruijnincx, P.C.A.|info:eu-repo/dai/nl/33799529X; Weckhuysen, B.M.|info:eu-repo/dai/nl/285484397

    2011-01-01

    The cobalt-catalyzed oxidation of lignin and lignin model compounds using molecular oxygen in ionic liquids proceeds readily under mild conditions, but mechanistic insight and evidence for the species involved in the catalytic cycle is lacking. In this study, a spectroscopic investigation of the

  12. Polyolefin nanocomposites in situ polymerization

    Energy Technology Data Exchange (ETDEWEB)

    Galland, Griselda Barrera; Fim, Fabiana de C.; Milani, Marceo A.; Silva, Silene P. da; Forest, Tadeu; Radaelli, Gislaine, E-mail: griselda.barrera@ufrgs.br [Universidade Federal do Rio Grande de Sul - UFRGS, Porto Alegre, RS (Brazil); Basso, Nara R.S. [Pontificia Universidade Catolica do Rio Grande do Sul, Porto Alegre, RS (Brazil); Quijada, Raul [Universidad de Chile, Santiago (Chile)

    2011-07-01

    Polyethylene and polypropylene nanocomposites using grapheme nanosheets and treated chrysotile have been synthesized by in situ polymerization using metallocene catalysts. The fillers have been submitted to acid, thermal and/ou ultrasound treatments before to introduce them into the polymerization reactor. A complete characterization of the fillers has been done. The nanocomposites have been characterized by SEM, TEM, DRX and AFM. The thermal, mechanic -dynamic, mechanical and electrical properties of the nanocomposites are discussed. (author)

  13. Polyolefin nanocomposites in situ polymerization

    International Nuclear Information System (INIS)

    Galland, Griselda Barrera; Fim, Fabiana de C.; Milani, Marceo A.; Silva, Silene P. da; Forest, Tadeu; Radaelli, Gislaine; Basso, Nara R.S.; Quijada, Raul

    2011-01-01

    Polyethylene and polypropylene nanocomposites using grapheme nanosheets and treated chrysotile have been synthesized by in situ polymerization using metallocene catalysts. The fillers have been submitted to acid, thermal and/ou ultrasound treatments before to introduce them into the polymerization reactor. A complete characterization of the fillers has been done. The nanocomposites have been characterized by SEM, TEM, DRX and AFM. The thermal, mechanic -dynamic, mechanical and electrical properties of the nanocomposites are discussed. (author)

  14. In Situ Formation of Carbon Nanomaterials on Bulk Metallic Materials

    Directory of Open Access Journals (Sweden)

    J. Y. Xu

    2014-01-01

    Full Text Available Carbon nanomaterials were synthesized in situ on bulk 316L stainless steel, pure cobalt, and pure nickel by hybrid surface mechanical attrition treatment (SMAT. The microstructures of the treated samples and the resulted carbon nanomaterials were investigated by SEM and TEM characterizations. Different substrates resulted in different morphologies of products. The diameter of carbon nanomaterials is related to the size of the nanograins on the surface layer of substrates. The possible growth mechanism was discussed. Effects of the main parameters of the synthesis, including the carbon source and gas reactant composition, hydrogen, and the reaction temperature, were studied. Using hybrid SMAT is proved to be an effective way to synthesize carbon nanomaterials in situ on surfaces of metallic materials.

  15. In-situ investigation of adsorption of dye and coadsorbates on TiO 2 films using QCM-D, fluorescence and AFM techniques

    KAUST Repository

    Harms, Hauke A.

    2013-09-11

    Simultaneous adsorption of dye molecules and coadsorbates is important for the fabrication of high-efficiency dyesensitized solar cells, but its mechanism is not well understood. Herein, we use a quartz crystal microbalance with dissipation technique (QCM-D) to study dynamically and quantitatively the sensitization of TiO2 in situ. We investigate dye loading for a ruthenium(II) polypyridyl complex (Z907), of a triphenylamine-based D-π-A dye (Y123), and of a ullazine sensitizer (JD21), as well as the simultaneous adsorption of the latter two with the coadsorbate chenodeoxycholic acid. By combining the QCM-D technique with fluorescence measurements, we quantify molar ratios between the dye and coadsorbate. Furthermore, we will present first studies using liquid-phase AFM on the adsorbed dye monolayer, thus obtaining complementary microscopic information that may lead to understanding of the adsorption mechanism on the molecular scale. © 2013 SPIE.

  16. In situ investigations on the impact of heat production and gamma radiation with regard to high-level radioactive waste disposal in rock salt formations

    International Nuclear Information System (INIS)

    Rothfuchs, T.

    1986-01-01

    Deep geological formations especially rock salt formations, are considered worldwide as suitable media for the final disposal of radioactive high-level waste (HLW). In the Federal Republic of Germany, the Institut fur Tieflagerung of the Gesellschaft fur Strahlen- und Umweltforschung mbH Munchen operates the Asse Salt Mine as a pilot facility for testing the behavior of an underground nuclear waste repository. The tests are performed using heat and radiation sources to simulate disposed HLW canisters. The measured data obtained since 1965 show that the thermomechanical response of the salt formation and the physical/chemical changes in the vicinity of disposal boreholes are not a serious concern and that their long-term consequences can be estimated based on theoretical considerations and in-situ investigations

  17. Investigation on H-containing shallow trap of hydrogenated TiO2 with in situ Fourier transform infrared diffuse reflection spectroscopy.

    Science.gov (United States)

    Han, Bing; Hang Hu, Yun

    2017-07-28

    A novel technique, high temperature high pressure in situ Fourier transform infrared diffuse reflection spectroscopy, was successfully used to investigate the formation and stability of shallow trap states in P25 TiO 2 nanoparticles. Two types of shallow traps (with and without H atoms) were identified. The H-containing shallow trap can be easily generated by heating in H 2 atmosphere. However, the trap is unstable in vacuum at 600 °C. In contrast, the H-free shallow trap, which can be formed by heating in vacuum, is stable even at 600 °C. The energy gaps between shallow trap states and the conduction band are 0.09 eV for H-containing shallow trap and 0.13 eV for H-free shallow trap, indicating that the H-containing shallow trap state is closer to the conduction band than that without H.

  18. Investigation of Arctic mixed-phase clouds by combining airborne remote sensing and in situ observations during VERDI, RACEPAC and ACLOUD

    Science.gov (United States)

    Ehrlich, André; Bierwirth, Eike; Borrmann, Stephan; Crewell, Susanne; Herber, Andreas; Hoor, Peter; Jourdan, Olivier; Krämer, Martina; Lüpkes, Christof; Mertes, Stephan; Neuber, Roland; Petzold, Andreas; Schnaiter, Martin; Schneider, Johannes; Weigel, Ralf; Weinzierl, Bernadett; Wendisch, Manfred

    2016-04-01

    To improve our understanding of Arctic mixed-phase clouds a series of airborne research campaigns has been initiated by a collaboration of German research institutes. Clouds in areas dominated by a close sea-ice cover were observed during the research campaign Vertical distribution of ice in Arctic mixed-phase clouds (VERDI, April/May 2012) and the Radiation-Aerosol-Cloud Experiment in the Arctic Circle (RACEPAC, April/May 2014) which both were based in Inuvik, Canada. The aircraft (Polar 5 & 6, Basler BT-67) operated by the Alfred Wegener Institute for Polar and Marine Research, Germany did cover a wide area above the Canadian Beaufort with in total 149 flight hours (62h during VERDI, 87h during RACEPAC). For May/June 2017 a third campaign ACLOUD (Arctic Clouds - Characterization of Ice, aerosol Particles and Energy fluxes) with base in Svalbard is planned within the Transregional Collaborative Research Centre TR 172 ArctiC Amplification: Climate Relevant Atmospheric and SurfaCe Processes, and Feedback Mechanisms (AC)3 to investigate Arctic clouds in the transition zone between open ocean and sea ice. The aim of all campaigns is to combine remote sensing and in-situ cloud, aerosol and trace gas measurements to investigate interactions between radiation, cloud and aerosol particles. While during VERDI remote sensing and in-situ measurements were performed by one aircraft subsequently, for RACEPAC and ACLOUD two identical aircraft are coordinated at different altitudes to horizontally collocate both remote sensing and in-situ measurements. The campaign showed that in this way radiative and microphysical processes in the clouds can by studied more reliably and remote sensing methods can be validated efficiently. Here we will illustrate the scientific strategy of the projects including the progress in instrumentation. Differences in the general synoptic and sea ice situation and related changes in cloud properties at the different locations and seasons will be

  19. Investigating an organ-targeting platform based on hydroxyapatite nanoparticles using a novel in situ method of radioactive {sup 125}Iodine labeling

    Energy Technology Data Exchange (ETDEWEB)

    Ignjatović, Nenad [Centre for Fine Particles Processing and Nanotechnologies, Institute of Technical Sciences of the Serbian Academy of Science and Arts, Knez Mihailova 35/4, 11000 Belgrade (Serbia); Vranješ Djurić, Sanja [Laboratory for Radioisotopes, Vinča Institute of Nuclear Sciences, University of Belgrade, PO Box 522, 11001 Belgrade (Serbia); Mitić, Žarko [Faculty of Medicine, Department of Pharmacy, University of Niš, Bulevar dr Zorana Đinđića 81, 18000 Niš (Serbia); Janković, Drina [Laboratory for Radioisotopes, Vinča Institute of Nuclear Sciences, University of Belgrade, PO Box 522, 11001 Belgrade (Serbia); Uskoković, Dragan, E-mail: dragan.uskokovic@itn.sanu.ac.rs [Centre for Fine Particles Processing and Nanotechnologies, Institute of Technical Sciences of the Serbian Academy of Science and Arts, Knez Mihailova 35/4, 11000 Belgrade (Serbia)

    2014-10-01

    In this study, we have investigated the synthesis of nanoparticles of hydroxyapatite (HAp) and hydroxyapatite coated with chitosan (HAp/Ch) and the chitosan-poly-D,L-lactide-co-glycolide polymer blend (HAp/Ch-PLGA) as an organ-targeting system. We have examined and defined the final destination, as well as the dynamics and the pathways of the synthesized particles following intravenous administration in vivo. The XRD, ZP, FT-IR and SEM analyses have confirmed that the hydroxyapatite nanoparticles with d{sub 50} = 72 nm are coated with polymers. Radioactive 125-Iodine ({sup 125}I), a low energy gamma emitter, was used to develop a novel in situ method for the radiolabeling of particles and investigation of their biodistribution. {sup 125}I-labeled particles exhibited high stability in saline and serum over the second day, which justified their use in the following in vivo studies. The biodistribution of {sup 125}I-labeled particles after intravenous injection in rats differed significantly: HAp particles mostly targeted the liver, HAp/Ch the spleen and the liver, while HAp/Ch-PLGA targeted the lungs. Twenty-four hours post injection, HAp particles were excreted completely, while both {sup 125}I-HAp/Ch and {sup 125}I-HAp/Ch-PLGA were retained in the body for a prolonged period of time with more than 20% of radioactivity still found in different organs. - Highlights: • An organ-targeting carrier based on nano-hydroxyapatite • In situ labeling • Biodistribution of {sup 125}I-labeled HAp particles.

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

    Science.gov (United States)

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

    2006-12-01

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

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

    International Nuclear Information System (INIS)

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

    2006-01-01

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

  2. Correlation of superconducting properties and microstructure in MgB{sub 2} using SEM, EPMA and TEM

    Energy Technology Data Exchange (ETDEWEB)

    Birajdar, Balaji I.

    2008-04-14

    This thesis can be subdivided as follows: (I) Development of the quantitative electron microscopy and spectroscopy methods essential for the microstructural analysis of MgB{sub 2} and thereby assess the performance of two energy-filtered TEMs. (II) Application of these methods to few selected samples: (a) Pure and Al-alloyed MgB{sub 2} bulk samples prepared by solid-state reaction or by mechanical alloying, (b) In-situ and ex-situ MgB{sub 2} wires and tapes with and without SiC additives prepared by different variants of the powder-in-tube technology. Quantitative B analysis by EDX spectroscopy was applied in the SEM and TEM, which is a major achievement. (III) Establishing a model which quantitatively explains the correlation between microstructure and critical current density as a function of magnetic field. The actual Al mole fraction in the MgB{sub 2} matrix was found to be less than the nominal Al mole fraction and the difference increased with increasing Al mole fraction. Al is incorporated into MgB{sub 2} grains of {approx}1{mu}m size by substitution of Mg atoms causing T{sub c} and c lattice parameter to decrease at a rate of 1.56 K and 1.15 pm per at.% of Al alloying. Precipitation of Al was not detected up to highest Al mole fractions but Al was inhomogeneously distributed in the sample, which explained the broadening of the superconducting transition width ({delta}T{sub c}) with increasing Al mole fraction. For wires and tapes, significant differences were observed in the microstructure of in-situ and ex-situ samples. This holds particularly if SiC was added and yielded Mg{sub 2}Si for in-situ samples annealed at 600 -650 C and Mg-Si-O phases for ex-situ samples annealed between 900 -1050 C. Four microstructural parameters were identified as relevant for the I{sub c} of wires and tapes and these were: 1) MgB{sub 2} grain size which lies in the range of 20-1000 nm, 2) colony size (colony is a dense arrangement of MgB{sub 2} grains) which lies in the range

  3. A TEM method for analyzing local strain fields in irradiated materials

    International Nuclear Information System (INIS)

    Bennetch, J.I.; Jesser, W.A.

    1983-01-01

    Of great interest to the field of fracture mechanics is the strain field in front of a crack tip. In irradiated materials, cavities which naturally form as a result of radiation provide convenient internal markers. If a miniaturized irradiated tensile sample is pulled in situ in a transmission electron microscope (TEM), both the relative displacement of these cavities and their distortion in shape provide information on localized strain on a microscopic level. In addition, the TEM method allows direct correlation of active slip systems with crack propagation characteristics. To illustrate this method a strain field map was constructed about a crack propagating in a helium irradiated type 316 stainless steel sample containing large cavities. (orig.)

  4. Polyhydroxyalkanoate as a slow-release carbon source for in situ bioremediation of contaminated aquifers: From laboratory investigation to pilot-scale testing in the field.

    Science.gov (United States)

    Pierro, Lucia; Matturro, Bruna; Rossetti, Simona; Sagliaschi, Marco; Sucato, Salvatore; Alesi, Eduard; Bartsch, Ernst; Arjmand, Firoozeh; Papini, Marco Petrangeli

    2017-07-25

    A pilot-scale study aiming to evaluate the potential use of poly-3-hydroxy-butyrate (PHB) as an electron donor source for in situ bioremediation of chlorinated hydrocarbons in groundwater was conducted. Compared with commercially available electron donors, PHB offers a restricted fermentation pathway (i.e., through acetic acid and molecular hydrogen) by avoiding the formation of any residual carbon that could potentially spoil groundwater quality. The pilot study was carried out at an industrial site in Italy, heavily contaminated by different chlorinated aliphatic hydrocarbons (CAHs). Prior to field testing, PHB was experimentally verified as a suitable electron donor for biological reductive dechlorination processes at the investigated site by microcosm studies carried out on site aquifer material and measuring the quantitative transformation of detected CAHs to ethene. Owing to the complex geological characteristics of the aquifer, the use of a groundwater circulation well (GCW) was identified as a potential strategy to enable effective delivery and distribution of electron donors in less permeable layers and to mobilise contaminants. A 3-screened, 30-m-deep GCW coupled with an external treatment unit was installed at the site. The effect of PHB fermentation products on the in situ reductive dechlorination processes were evaluated by quantitative real-time polymerase chain reaction (qPCR). The results from the first 4 months of operation clearly demonstrated that the PHB fermentation products were effectively delivered to the aquifer and positively influenced the biological dechlorination activity. Indeed, an increased abundance of Dehalococcoides mccartyi (up to 6.6 fold) and reduced CAH concentrations at the installed monitoring wells were observed. Copyright © 2016 Elsevier B.V. All rights reserved.

  5. Numerical and in-situ investigations of water hammer effects in Drava river Kaplan turbine hydropower plants

    Science.gov (United States)

    Bergant, A.; Gregorc, B.; Gale, J.

    2012-11-01

    This paper deals with critical flow regimes that may induce unacceptable water hammer in Kaplan turbine hydropower plants. Water hammer analysis should be performed for normal, emergency and catastrophic operating conditions. Hydropower plants with Kaplan turbines are usually comprised of relatively short inlet and outlet conduits. The rigid water hammer theory can be used for this case. For hydropower plants with long penstocks the elastic water hammer should be used. Some Kaplan turbine units are installed in systems with long open channels. In this case, water level oscillations in the channels should be carefully investigated. Computational results are compared with results of measurements in recently rehabilitated seven Drava river hydroelectric power plants in Slovenia. Water hammer in the six power plants is controlled by appropriate adjustment of the wicket gates and runner blades closing/opening manoeuvres. Due to very long inflow and outflow open channels in Zlatoličje HPP a special vaned pressure regulating device attenuates extreme pressures in Kaplan turbine flow-passage system and controls unsteady flow in both open channels. Comparisons of results include normal operating regimes. The agreement between computed and measured results is reasonable.

  6. Numerical and in-situ investigations of water hammer effects in Drava river Kaplan turbine hydropower plants

    International Nuclear Information System (INIS)

    Bergant, A; Gregorc, B; Gale, J

    2012-01-01

    This paper deals with critical flow regimes that may induce unacceptable water hammer in Kaplan turbine hydropower plants. Water hammer analysis should be performed for normal, emergency and catastrophic operating conditions. Hydropower plants with Kaplan turbines are usually comprised of relatively short inlet and outlet conduits. The rigid water hammer theory can be used for this case. For hydropower plants with long penstocks the elastic water hammer should be used. Some Kaplan turbine units are installed in systems with long open channels. In this case, water level oscillations in the channels should be carefully investigated. Computational results are compared with results of measurements in recently rehabilitated seven Drava river hydroelectric power plants in Slovenia. Water hammer in the six power plants is controlled by appropriate adjustment of the wicket gates and runner blades closing/opening manoeuvres. Due to very long inflow and outflow open channels in Zlatolicje HPP a special vaned pressure regulating device attenuates extreme pressures in Kaplan turbine flow-passage system and controls unsteady flow in both open channels. Comparisons of results include normal operating regimes. The agreement between computed and measured results is reasonable.

  7. Electron beam exposure mechanisms in hydrogen silsesquioxane investigated by vibrational spectroscopy and in-situ electron beam induced desorption

    Energy Technology Data Exchange (ETDEWEB)

    Olynick, D.L.; Cord, B.; Schipotinin, A.; Ogletree, D.F.; Schuck, P.J.

    2009-11-13

    Hydrogen Silsesquioxane (HSQ) is used as a high-resolution resist with resolution down below 10nm half-pitch. This material or materials with related functionalities could have widespread impact in nanolithography and nanoscience applications if the exposure mechanism was understood and instabilities controlled. Here we have directly investigated the exposure mechanism using vibrational spectroscopy (both Raman and Fourier transform Infrared) and electron beam desorption spectrocscopy (EBDS). In the non-networked HSQ system, silicon atoms sit at the corners of a cubic structure. Each silicon is bonded to a hydrogen atom and bridges 3 oxygen atoms (formula: HSiO3/2). For the first time, we have shown, via changes in the Si-H2 peak at ~;;2200 cm -1 in the Raman spectra and the release of SiHx products in EBID, that electron-bam exposed materials crosslinks via a redistribution reaction. In addition, we observe the release of significantly more H2 than SiH2 during EBID, which is indicative of additional reaction mechanisms. Additionally, we compare the behavior of HSQ in response to both thermal and electron-beam induced reactions.

  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. Experimental study on propagation properties of large size TEM antennas

    International Nuclear Information System (INIS)

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

    2014-01-01

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

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

    Science.gov (United States)

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

    2017-06-01

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

  11. Dehydrogenation kinetics of pure and nickel-doped magnesium hydride investigated by in situ time-resolved powder X-ray diffraction

    DEFF Research Database (Denmark)

    Jensen, T.R.; Andreasen, A.; Vegge, Tejs

    2006-01-01

    The dehydrogenation kinetics of pure and nickel (Ni)-doped (2w/w%) magnesium hydride (MgH2) have been investigated by in situ time-resolved powder X-ray diffraction (PXD). Deactivated samples, i.e. air exposed, are investigated in order to focus on the effect of magnesium oxide (MgO) surface layers......, which might be unavoidable for magnesium (Mg)-based storage media for mobile applications. A curved position-sensitive detector covering 120 degrees in 20 and a rotating anode X-ray source provide a time resolution of 45 s and up to 90 powder pattems collected during an experiment under isothermal...... by the Johnson-Mehi-Avrami formalism in order to derive rate constants at different temperatures. The apparent activation energies for dehydrogenation of pure and Ni-doped magnesium hydride were E-A approximate to 300 and 250 kJ/mol, respectively. Differential scanning calorimetry gave, E-A = 270 k...

  12. Investigating an organ-targeting platform based on hydroxyapatite nanoparticles using a novel in situ method of radioactive ¹²⁵Iodine labeling.

    Science.gov (United States)

    Ignjatović, Nenad; Vranješ Djurić, Sanja; Mitić, Zarko; Janković, Drina; Uskoković, Dragan

    2014-10-01

    In this study, we have investigated the synthesis of nanoparticles of hydroxyapatite (HAp) and hydroxyapatite coated with chitosan (HAp/Ch) and the chitosan-poly-d,l-lactide-co-glycolide polymer blend (HAp/Ch-PLGA) as an organ-targeting system. We have examined and defined the final destination, as well as the dynamics and the pathways of the synthesized particles following intravenous administration in vivo. The XRD, ZP, FT-IR and SEM analyses have confirmed that the hydroxyapatite nanoparticles with d50=72 nm are coated with polymers. Radioactive 125-Iodine ((125)I), a low energy gamma emitter, was used to develop a novel in situ method for the radiolabeling of particles and investigation of their biodistribution. (125)I-labeled particles exhibited high stability in saline and serum over the second day, which justified their use in the following in vivo studies. The biodistribution of (125)I-labeled particles after intravenous injection in rats differed significantly: HAp particles mostly targeted the liver, HAp/Ch the spleen and the liver, while HAp/Ch-PLGA targeted the lungs. Twenty-four hours post injection, HAp particles were excreted completely, while both (125)I-HAp/Ch and (125)I-HAp/Ch-PLGA were retained in the body for a prolonged period of time with more than 20% of radioactivity still found in different organs. Copyright © 2014 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

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

    2017-08-03

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

  14. A new in situ technique for studying deformation and fracture in thin film ductile/brittle laminates

    International Nuclear Information System (INIS)

    Hackney, S.A.; Milligan, W.W.

    1991-01-01

    A new technique for studying deformation and fracture of thin film ductile/brittle laminates is described. The laminates are prepared by sputtering a brittle coating on top of an electropolished TEM thin foil. The composites are then strained in situ in the TEM. In this preliminary investigation, the composites consisted of a ductile aluminum substrate and a brittle silicon coating. Cracks in the brittle film grew discontinuously in bursts several micrometers in length. The crack opening displacement initiated plastic deformation in the ductile film, thus dissipating energy and allowing crack arrest. The interface was well bonded, and delamination was not observed. Due to the good interfacial bond and the crack opening behind the crack tip, it was possible to study very large plastic deformations and ductile fracture in the aluminum in situ, without buckling of the foil. The possibility of micromechanical modeling of the fracture behavior is briefly discussed. (orig.)

  15. An alternative to the TEM (Transformed Eulerian Mean) equations

    Science.gov (United States)

    Gaßmann, Almut

    2013-04-01

    The TEM equations constitute a powerful means to get access to the residual circulation. However, due to their foundation on the wave perspective, they deliver only a zonally averaged picture without access to the three-dimensional structure or the local origins of the residual circulation. Therefore it is worth to investigate whether there are alternatives. The pathway followed here is to perform a transformation of the momentum and the potential temperature equation before taking the zonal mean. This is done by removing the steady state ideal wind solution vid = ?×?B-(?±P) from the equations (? - potential temperature, B - Bernoulli function, P - Ertel's potential vorticity EPV, ?± - density). The advantage of that approach is that the total EPV-flux does no longer contain an explicitly visible 'do-nothing-flux'. This flux, ?? ×?B, does only vanish when averaging on isentropic surfaces, but not on other isosurfaces. Here we find the reason why the conventional zonal mean on isentropes delivers a direct overturning cell on each hemisphere, whereas on other isosurfaces we obtain the typical three-cell structure with Headley, Ferrel, and polar cells. It will be demonstrated and made visible through idealized climate experiments with the ICON-IAP model that the zonal averages of the nonideal wind components vnid = v - vid and wnid = w - wid constitute similar direct overturning cells on non-isentropic surfaces as obtained with the TEM-generated v* and w*. It is also interesting to inspect fields of local nonideal wind components, the very origin of the residual circulation.

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

    International Nuclear Information System (INIS)

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

    2003-01-01

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

  17. 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

  18. Focus-variation image reconstruction in field-emission TEM

    NARCIS (Netherlands)

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

    1993-01-01

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

  19. 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....

  20. TEM sample preparation by FIB for carbon nanotube interconnects

    International Nuclear Information System (INIS)

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

    2009-01-01

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

  1. TEM sample preparation by FIB for carbon nanotube interconnects

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-10-15

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

  2. 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.

  3. 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.

  4. Thermal annealing dynamics of carbon-coated LiFePO{sub 4} nanoparticles studied by in-situ analysis

    Energy Technology Data Exchange (ETDEWEB)

    Krumeich, Frank, E-mail: krumeich@inorg.chem.ethz.ch [Department of Chemistry and Applied Biosciences, ETH Zurich, Vladimir-Prelog-Weg 1, 8093 Zurich (Switzerland); Waser, Oliver; Pratsinis, Sotiris E. [Department of Mechanical and Process Engineering, ETH Zurich, Sonneggstrasse 3, 8092 Zurich (Switzerland)

    2016-10-15

    The thermal behavior of core-shell carbon-coated lithium iron phosphate (LiFePO{sub 4}-C) nanoparticles made by flame spray pyrolysis (FSP) during annealing was investigated by in-situ transmission electron microscopy (TEM), in-situ X-ray powder diffraction (XRD) as well as ex-situ diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS). Crystallization of the initially glassy LiFePO{sub 4}-C nanoparticles starts at quite low temperatures (T=400 °C), forming single crystals inside the confinement of the carbon shell. Upon increasing the temperature to T≥700 °C, LiFePO{sub 4} starts to diffuse through the carbon shell resulting in cavities inside the mostly intact carbon shell. By increasing the temperature further to T≥800 °C, the initial core-shell morphology converts into open carbon shells (flakes and cenospheres) and bulky LiFePO{sub 4} particles (diameter in the range 300–400 nm), in agreement with ex-situ experiments. - Graphical abstract: TEM images of a typical sample area recorded at room temperature and after heating in-situ heating reveal the growth of particles and the formation of empty carbon cages. - Highlights: • LiFePO{sub 4} coated by a carbon shell is produced by flame spray pyrolysis. • The amorphous LiFePO{sub 4} starts to crystallize at 400 °C as revealed by in-situ XRD. • Crystal growth was visualized by TEM heating experiments. • The formation of empty carbon cages starts at 700 °C.

  5. In-situ investigation on the oxidation behaviour of low alloyed steels annealed under N{sub 2}-5%H{sub 2} protective atmospheres

    Energy Technology Data Exchange (ETDEWEB)

    Martinez, C.; Cremer, R. [RWTH Aachen (Germany). Lehrstuhl fuer Theoretische Huettenkunde; Loison, D. [Institut de Recherches de la Siderurgie Francaise (IRSID), 57 - Maizieres-les-Metz (France); Servais, J.P. [Centre de Recherches Metallurgiques, Liege (Belgium)

    2001-12-01

    The oxidation behaviour of low alloyed steels, Fe-0.6%Mn and Fe-1.5%Mn, under different annealing conditions was studied. Due to the crucial importance of the surface state of the sample, the experiments were performed in an in-situ device to avoid any contact with air after the annealings. The annealing experiments were carried out under different conditions: high vacuum ({proportional_to}10{sup -6} mbar), N{sub 2}/H{sub 2} protective atmospheres with traces of water (dew point -30 C) and temperatures ranging from 873 to 1073 K. Under this variety of heat treatments, the reconstruction of the Fe surface and the formation of different oxides was observed and characterised, paying special attention to the selective oxidation of manganese. The surface structure and composition was investigated by means of the combined use of reflection high-energy electron diffraction (RHEED) and X-ray photoelectron spectroscopy (XPS). The analyses show that the use of RHEED is a good alternative for determining the crystallographic structure of the outermost layers of the surface. With this technique the structures of iron and manganese oxides can be distinguished despite the similar structures and lattice parameters. It is also possible to identify the crystallographic textures present on the oxidation products and to give qualitative information about the surface reconstruction of the grains. (orig.)

  6. In situ investigation of ion-induced dewetting of a thin iron-oxide film on silicon by high resolution scanning electron microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Amirthapandian, S. [Institut fuer Halbleiteroptik und Funktionelle Grenzflaechen, Universitaet Stuttgart, 70569 Stuttgart (Germany); Material Physics Division, Materials Science Group, Indira Gandhi Centre for Atomic Research, Kalpakkam 603 102 (India); Schuchart, F.; Garmatter, D.; Bolse, W. [Institut fuer Halbleiteroptik und Funktionelle Grenzflaechen, Universitaet Stuttgart, 70569 Stuttgart (Germany)

    2012-11-15

    Using our new in situ high resolution scanning electron microscope, which is integrated into the UNILAC ion beamline at the Helmholtzzentrum fuer Schwerionenforschung (GSI) in Darmstadt, Germany, we investigated the swift heavy ion induced dewetting of a thin iron oxide layer on Si. Besides heterogeneous hole nucleation at defects and spontaneous (homogeneous) hole nucleation, we could clearly identify a dewetting mechanism, which is similar to the spinodal dewetting observed for liquid films. Instead of being due to capillary waves, it is based on a stress induced surface instability. The latter results in the formation of a wavy surface with constant dominant wave-length and increasing amplitude during ion irradiation. Dewetting sets in as soon as the wave-troughs reach the film-substrate interface. Inspection of the hole radii and rim shapes indicates that removal of the material from the hole area occurs mainly by plastic deformation at the inner boundary and ion induced viscous flow in the peripheral zone due to surface tension.

  7. Spatially and time-resolved element-specific in situ corrosion investigations with an online hyphenated microcapillary flow injection inductively coupled plasma mass spectrometry set-up

    International Nuclear Information System (INIS)

    Homazava, N.; Ulrich, A.; Kraehenbuehl, U.

    2008-01-01

    A novel technique for in situ spatial, time-resolved element-specific investigations of corrosion processes is developed. The technique is based on an online hyphenation of a specially designed microflow-capillary set-up to inductively coupled plasma mass spectrometry (ICP-MS) using flow injection sample introduction. Detailed aspects of the method development, optimization of the sample microflow introduction and flow injection characteristics for the localized corrosion analysis are described. Moreover, specific challenges of the ICP-MS analysis as applied to the analysis of corrosion sample probes, e.g. high matrix load and limited sample volume, are discussed. The efficiency of the developed technique is proved by corrosion susceptibility analysis of a commercial Al alloy. Results of the corrosion experiments of the aluminum alloy AA 6111 are presented to demonstrate the influence of various factors such as exposure time and pH value of the corrosive medium on the element-specific dissolution rates of the alloy. This novel technique provides new aspects in corrosion science and sheds new light on corrosion mechanisms

  8. Mineralogical In-situ Investigation of Acid-Sulfate Samples from the Rio Tinto River, Spain, with a Portable XRD/XRF Instrument

    Science.gov (United States)

    Sarrazin, P.; Ming, D. W.; Morris, R. V.; Fernandez-Remolar, D.; Amils, R.; Arvidson, R. E.; Blake, D.; Bish, D. L.

    2007-01-01

    A field campaign was organized in September 2006 by Centro de Astobiologica (Spain) and Washington University (St Louis, USA) for the geological study of the Rio Tinto river bed sediments using a suite of in-situ instruments comprising an ASD reflectance spectrometer, an emission spectrometer, panoramic and close-up color imaging cameras, a life detection system and NASA's CheMin 4 XRD/XRF prototype. The primary objectives of the field campaign were to study the geology of the site and test the potential of the instrument suite in an astrobiological investigation context for future Mars surface robotic missions. The results of the overall campaign will be presented elsewhere. This paper focuses on the results of the XRD/XRF instrument deployment. The specific objectives of the CheMin 4 prototype in Rio Tinto were to 1) characterize the mineralogy of efflorescent salts in their native environments; 2) analyze the mineralogy of salts and oxides from the modern environment to terraces formed earlier as part of the Rio Tinto evaporative system; and 3) map the transition from hematite-dominated terraces to the mixed goethite/salt-bearing terraces where biosignatures are best preserved.

  9. Coupling in-situ X-ray micro- and nano-tomography and discrete element method for investigating high temperature sintering of metal and ceramic powders

    Directory of Open Access Journals (Sweden)

    Yan Zilin

    2017-01-01

    Full Text Available The behaviour of various powder systems during high temperature sintering has been investigated by coupling X-ray microtomography and discrete element method (DEM. Both methods are particularly relevant to analyse particle interactions and porosity changes occurring during sintering. Two examples are presented. The first one deals with a copper powder including artificially created pores which sintering has been observed in situ at the European synchrotron and simulated by DEM. 3D images with a resolution of 1.5 μm have been taken at various times of the sintering cycle. The comparison of the real displacement of particle centers with the displacement derived from the mean field assumption demonstrates significant particle rearrangement in some regions of the sample. Although DEM simulation showed less rearrangement, it has been able to accurately predict the densification kinetics. The second example concerns multilayer ceramic capacitors (MLCCs composed of hundreds of alternated metal electrode and ceramic dielectric layers. The observation of Ni-based MLCCs by synchrotron nanotomography at Argon National Laboratory with a spatial resolution between 10 and 50 nm allowed understanding the origin of heterogeneities formed in Ni layers during sintering. DEM simulations confirmed this analysis and provided clues for reducing these defects.

  10. Hybrid perovskite solar cells: In situ investigation of solution-processed PbI2 reveals metastable precursors and a pathway to producing porous thin films

    KAUST Repository

    Barrit, Dounya

    2017-04-17

    The successful and widely used two-step process of producing the hybrid organic-inorganic perovskite CH3NH3PbI3, consists of converting a solution deposited PbI2 film by reacting it with CH3NH3I. Here, we investigate the solidification of PbI2 films from a DMF solution by performing in situ grazing incidence wide angle X-ray scattering (GIWAXS) measurements. The measurements reveal an elaborate sol–gel process involving three PbI2⋅DMF solvate complexes—including disordered and ordered ones—prior to PbI2 formation. The ordered solvates appear to be metastable as they transform into the PbI2 phase in air within minutes without annealing. Morphological analysis of air-dried and annealed films reveals that the air-dried PbI2 is substantially more porous when the coating process produces one of the intermediate solvates, making this more suitable for subsequent conversion into the perovskite phase. The observation of metastable solvates on the pathway to PbI2 formation open up new opportunities for influencing the two-step conversion of metal halides into efficient light harvesting or emitting perovskite semiconductors.

  11. New Pyrazole-Hydrazone Derivatives: X-ray Analysis, Molecular Structure Investigation via Density Functional Theory (DFT) and Their High In-Situ Catecholase Activity.

    Science.gov (United States)

    Karrouchi, Khalid; Yousfi, El Bekkaye; Sebbar, Nada Kheira; Ramli, Youssef; Taoufik, Jamal; Ouzidan, Younes; Ansar, M'hammed; Mabkhot, Yahia N; Ghabbour, Hazem A; Radi, Smaail

    2017-10-25

    The development of low-cost catalytic systems that mimic the activity of tyrosinase enzymes (Catechol oxidase) is of great promise for future biochemistry technologic demands. Herein, we report the synthesis of new biomolecules systems based on hydrazone derivatives containing a pyrazole moiety ( L1 - L6 ) with superior catecholase activity. Crystal structures of L1 and L2 biomolecules were determined by X-ray single crystal diffraction (XRD). Optimized geometrical parameters were calculated by density functional theory (DFT) at B3LYP/6-31G (d, p) level and were found to be in good agreement with single crystal XRD data. Copper (II) complexes of the compounds ( L1 - L6 ), generated in-situ, were investigated for their catalytic activities towards the oxidation reaction of catechol to ortho -quinone with the atmospheric dioxygen, in an attempt to model the activity of the copper containing enzyme tyrosinase. The studies showed that the activities depend on four parameters: the nature of the ligand, the nature of counter anion, the nature of solvent and the concentration of ligand. The Cu(II)-ligands, given here, present the highest catalytic activity (72.920 μmol·L -1 ·min -1 ) among the catalysts recently reported in the existing literature.

  12. Dislocation interaction with a .SIGMA.=3 grain boundary by .I.in-situ./I. TEM

    Czech Academy of Sciences Publication Activity Database

    Vystavěl, Tomáš; Jacques, A.; Gemperle, Antonín; Gemperlová, Juliana; George, A.

    294-296, - (1999), s. 397-400 ISSN 0255-5476. [Intergranular and Interphase Boundaries in Materials(iib`98). Praha, 06.07.1998-09.07.1998] R&D Projects: GA AV ČR IAA1010702; GA ČR GA202/98/1281 Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 0.981, year: 1999

  13. Nickel oxide reduction studied by environmental TEM and in situ XRD

    DEFF Research Database (Denmark)

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

    2012-01-01

    Paar furnace and a mass spectrometer to complement and extrapolate the ETEM data to higher pressures and gas flows. Diffraction peak intensities, crystallite sizes (obtained using the Scherrer formula) and H2/H2O mass spectrometer signals are monitored. The recorded images and diffraction patterns show...... that the presence and stagnation of H2O vapour created upon reduction blocks H2 access to the reactive sites, decreasing the reaction rate at a high conversion fraction. The gas flow is low and may not evacuate the product gas efficiently around the Ni(O) particles. Complementary XRD experiments point towards...... the same conclusion and underline the impact of the pressure and gas flow on the kinetics. It is possible to determine an approximate activation energy for NiO reduction inside the ETEM using the Kissinger method [8], which is based on measurements of the shift in the temperature at which the reaction rate...

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

    Directory of Open Access Journals (Sweden)

    Magnus Hummelgård

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

  15. Customizable in situ TEM devices fabricated in freestanding membranes by focused ion beam milling

    DEFF Research Database (Denmark)

    Lei, Anders; Petersen, Dirch Hjorth; Booth, Tim

    2010-01-01

    crystalline silicon extending over the edge of a pre-fabricated silicon microchip. Four-terminal resistance measurements of FIB-defined nanowires showed at least two orders of magnitude increase in resistivity compared to bulk. We show that the initial high resistance is due to amorphization of silicon...

  16. Crystallization of TiO2 Nanotubes by In Situ Heating TEM

    KAUST Repository

    Casu, Alberto; Lamberti, Andrea; Stassi, Stefano; Falqui, Andrea

    2018-01-01

    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

  17. Molecular Gut Content Profiling to Investigate the In Situ Grazing and Selectivity of Dolioletta gegenbauri in Summer Continental Shelf Intrusion Waters of the South Atlantic Bight, USA

    Science.gov (United States)

    Walters, T. L.; Frazier, L.; Gibson, D. M.; Paffenhofer, G. A.; Frischer, M. E.

    2016-02-01

    Gelatinous metazooplankton play a crucial role in marine planktonic food webs and it has been suggested that they may become increasingly important in the Future Ocean. However, largely due to methodological challenges and reliance on laboratory cultivation approaches, the in situ diet of zooplankton with complex life histories and diverse prey choices remains poorly investigated. This is particularly true for the gelatinous zooplankton including the pelagic tunicate, Dolioletta gegenbauri that form large blooms in productive subtropical continental shelf environments. To investigate the diet of D. gegenbauri we developed a molecular gut profiling approach based on the use of a Peptide Nucleic Acid (PNA) PCR blocker. Using a doliolid-specific PNA blocker, it was possible to enrich the amplification of prey and parasite DNA from whole animal DNA extracts of doliolids. Gut contents from the water column, wild and captive-fed doliolids were profiled after PNA-PCR by denaturing HPLC (dHPLC), clone library and next generation sequencing (NGS) approaches. Studies were conducted during 5 summer cruises in the mid-shelf of the South Atlantic Bight. Comparison of gut profiles to available prey in the water column revealed evidence of prey selection towards larger prey species, including diatoms, dinoflagelletes and also metazoan prey that were likely captured as larvae and eggs. Wild-caught doliolids contained significantly more metazoan sequences than did the captive-fed doliolids. Ingestion of metazoan prey suggests that metazoans may contribute both the nutrition of doliolids and the potential role of doliolids as trophic cascade agents in continental shelf pelagic food webs.

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

    Science.gov (United States)

    Kolosov, Vladimir

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

  19. Design, development, and demonstration of a fully LabVIEW controlled in situ electrochemical Fourier transform infrared setup combined with a wall-jet electrode to investigate the electrochemical interface of nanoparticulate electrocatalysts under reaction conditions.

    Science.gov (United States)

    Nesselberger, Markus; Ashton, Sean J; Wiberg, Gustav K H; Arenz, Matthias

    2013-07-01

    We present a detailed description of the construction of an in situ electrochemical ATR-FTIR setup combined with a wall-jet electrode to investigate the electrocatalytic properties of nanoparticulate catalysts in situ under controlled mass transport conditions. The presented setup allows the electrochemical interface to be probed in combination with the simultaneous determination of reaction rates. At the same time, the high level of automation allows it to be used as a standard tool in electrocatalysis research. The performance of the setup was demonstrated by probing the oxygen reduction reaction on a platinum black catalyst in sulfuric electrolyte.

  20. 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.