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.

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

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

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

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.

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....

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

Energy Technology Data Exchange (ETDEWEB)

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

2017-09-29

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

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

Directory of Open Access Journals (Sweden)

Caitlin Anne Taylor

2017-09-01

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

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.

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.

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.

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.

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.

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.

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.

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)

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

International Nuclear Information System (INIS)

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

2015-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2015-04-15

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

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.

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.

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

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.

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.

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

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.

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)

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

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.

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

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.

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.

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.

Observation of Pt-{100}-p(2×2-O reconstruction by an environmental TEM

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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.

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.

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.

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

Energy Technology Data Exchange (ETDEWEB)

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

2017-07-15

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

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

International Nuclear Information System (INIS)

Berlin, Katja; Trampert, Achim

2017-01-01

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

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.

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

International Nuclear Information System (INIS)

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

2015-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2015-10-15

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

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.

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.

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.

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.

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.

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.

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.

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.

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.

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

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.

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.

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.

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.

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

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

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)

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.

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.

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

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...

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.

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...

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.

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.

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...

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.

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

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

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.

'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

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

Science.gov (United States)

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

2012-08-08

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

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.

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

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"

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

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.

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...

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

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.)

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.

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.

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.

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

Science.gov (United States)

Straubinger, Rainer; Beyer, Andreas; Volz, Kerstin

2016-06-01

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

In situ observation of morphological change in CdTe nano- and submicron wires

Energy Technology Data Exchange (ETDEWEB)

Davami, Keivan; Lee, Jeong-Soo; Meyyappan, M [Division of IT Convergence Engineering, Pohang University of Science and Technology, Pohang (Korea, Republic of); Ghassemi, Hessam M; Yassar, Reza S [Department of Mechanical Engineering, Michigan Technological University, Houghton, MI 49931 (United States); Sun, Xuhui, E-mail: ljs6951@postech.ac.kr, E-mail: m.meyyappan@nasa.gov [Institute of Functional Nano and Soft Materials (FUNSOM), Soochow University, Suzhou, Jiangsu 215123 (China)

2011-10-28

We report growth and characterization of CdTe wires 30-400 nm in diameter by the vapor-liquid-solid technique. Individual nanowires were placed on a movable piezotube, which allowed three-dimensional motion toward a scanning tunneling microscope (STM). A bias was applied to the STM tip in contact with the nanowire, and the morphological changes due to Joule heating were observed in situ using a transmission electron microscope (TEM) in real time. For thick CdTe wires (d > {approx} 150 nm), the process results in the growth of superfine nanowires (SFNWs) of 2-4 nm diameter on the surface of the wire. Smaller diameter nanowires, in contrast, disintegrate under the applied bias before the complete evolution of SFNWs on the surface.

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

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

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

International Nuclear Information System (INIS)

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

2008-01-01

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

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

Czech Academy of Sciences Publication Activity Database

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

2002-01-01

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

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.

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

International Nuclear Information System (INIS)

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

2010-01-01

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

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.

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.

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.

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....

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.

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

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)

TEM observations of HT-9 as-welded weldment microstructures

International Nuclear Information System (INIS)

Foulds, J.R.; Lechtenberg, T.A.

1984-01-01

TEM studies of different locations in an HT-9 weldment indicated delta-ferrite (delta) occurrence, M 23 C 6 precipitation at delta-martensite interfaces, fine carbide precipitation at prior austenite grain boundaries, and martensite lath and lath packet size to be the distinguishable microstructure features observed. Furthermore, retained austenite films were observed in the weld metal and the HAZ adjacent to the weld metal that reached the highest temperature during joining. The microstructures correlate well with the observed room temperature microhardness except for the fusion boundary in weld metal which exhibited a hardness drop and an unexpected minimum amount of delta-ferrite

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

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.

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

International Nuclear Information System (INIS)

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

2008-01-01

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

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....

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...

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

Science.gov (United States)

Grogan, Joseph M.

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

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.

Study on the fabrication of Al matrix composites strengthened by combined in-situ alumina particle and in-situ alloying elements

International Nuclear Information System (INIS)

Huang Zanjun; Yang Bin; Cui Hua; Zhang Jishan

2003-01-01

A new idea to fabricate aluminum matrix composites strengthened by combined in-situ particle strengthening and in-situ alloying has been proposed. Following the concept of in-situ alloying and in-situ particle strengthening, aluminum matrix composites reinforced by Cu and α-Al 2 O 3 particulate (material I) and the same matrix reinforced by Cu, Si alloying elements and α-Al 2 O 3 particulate (material II) have been obtained. SEM observation, EDS and XRD analysis show that the alloy elements Cu and Si exist in the two materials, respectively. In-situ Al 2 O 3 particulates are generally spherical and their mean size is less than 0.5 μm. TEM observation shows that the in-situ α-Al 2 O 3 particulates have a good cohesion with the matrix. The reaction mechanism of the Al 2 O 3 particulate obtained by this method was studied. Thermodynamic considerations are given to the in-situ reactions and the distribution characteristic of in-situ the α-Al 2 O 3 particulate in the process of solidification is also discussed

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.

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

Angstrom analysis with dynamic in-situ aberration corrected electron microscopy

International Nuclear Information System (INIS)

Gai, P L; Boyes, E D

2010-01-01

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

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.

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.

Feasibility of Observing and Characterizing Single Ion Strikes in Microelectronic Components

International Nuclear Information System (INIS)

Dingreville, Remi Philippe Michel; Hattar, Khalid Mikhiel; Bufford, Daniel Charles

2015-01-01

The transient degradation of semiconductor device performance under irradiation has long been an issue of concern. A single high-energy charged particle can degrade or permanently destroy the microelectronic component, potentially altering the course or function of the systems. Disruption of the the crystalline structure through the introduction of quasi-stable defect structures can change properties from semiconductor to conductor. Typically, the initial defect formation phase is followed by a recovery phase in which defect-defect or defect-dopant interactions modify the characteristics of the damaged structure. In this LDRD Express, in-situ ion irradiation transmission microscopy (TEM) in-situ TEM experiments combined with atomistic simulations have been conducted to determine the feasibility of imaging and characterizing the defect structure resulting from a single cascade in silicon. In-situ TEM experiments have been conducted to demonstrate that a single ion strike can be observed in Si thin films with nanometer resolution in real time using the in-situ ion irradiation transmission electron microscope (I 3 TEM). Parallel to this experimental effort, ion implantation has been numerically simulated using Molecular Dynamics (MD). This numerical framework provides detailed predictions of the damage and follow the evolution of the damage during the first nanoseconds. The experimental results demonstrate that single ion strike can be observed in prototypical semiconductors.

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.

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...

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....

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

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

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

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.

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...

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

Science.gov (United States)

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

2016-04-01

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

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

Science.gov (United States)

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

2016-12-01

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

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

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''.

Dynamical observation of lithium insertion/extraction reaction during charge-discharge processes in Li-ion batteries by in situ spatially resolved electron energy-loss spectroscopy.

Science.gov (United States)

Shimoyamada, Atsushi; Yamamoto, Kazuo; Yoshida, Ryuji; Kato, Takehisa; Iriyama, Yasutoshi; Hirayama, Tsukasa

2015-12-01

All-solid-state Li-ion batteries (LIBs) with solid electrolytes are expected to be the next generation devices to overcome serious issues facing conventional LIBs with liquid electrolytes. However, the large Li-ion transfer resistance at the electrode/solid-electrolyte interfaces causes low power density and prevents practical use. In-situ-formed negative electrodes prepared by decomposing the solid electrolyte Li(1+x+3z)Alx(Ti,Ge)(2-x)Si(3z)P(3-z)O12 (LASGTP) with an excess Li-ion insertion reaction are effective electrodes providing low Li-ion transfer resistance at the interfaces. Prior to our work, however, it had still been unclear how the negative electrodes were formed in the parent solid electrolytes. Here, we succeeded in dynamically visualizing the formation by in situ spatially resolved electron energy-loss spectroscopy in a transmission electron microscope mode (SR-TEM-EELS). The Li-ions were gradually inserted into the solid electrolyte region around 400 nm from the negative current-collector/solid-electrolyte interface in the charge process. Some of the ions were then extracted in the discharge process, and the rest were diffused such that the distribution was almost flat, resulting in the negative electrodes. The redox reaction of Ti(4+)/Ti(3+) in the solid electrolyte was also observed in situ during the Li insertion/extraction processes. The in situ SR-TEM-EELS revealed the mechanism of the electrochemical reaction in solid-state batteries. © The Author 2015. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

In-situ observation of structure formation in polymer processing

International Nuclear Information System (INIS)

Murase, Hiroki

2009-01-01

In-situ X-ray scattering in polymer processing is a crucial method to elucidate the mechanism of structure formation in the process. Fiber spinning is one such process primarily imposing extensional deformation on polymeric melt at the spin-line during rapid cooling. In-situ small-angle X-ray scattering using synchrotron radiation on the spinning process allows direct observation of the transient structure developing in the process. (author)

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

International Nuclear Information System (INIS)

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

2013-01-01

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

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.

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.

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.

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

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.

In situ observation of transformation in alpha-Fe sub 2 O sub 3 under hydrogen implantation

CERN Document Server

Watanabe, Y; Ishikawa, N; Furuya, K; Kato, M

2002-01-01

An in situ observation of the alpha-Fe sub 2 O sub 3 -to-Fe sub 3 O sub 4 transformation has been performed using a dual-ion-beam accelerator interfaced with a transmission electron microscope (TEM). During the hydrogen-ion implantation of alpha-Fe sub 2 O sub 3 , transformation into the new phase (gamma-Fe sub 2 O sub 3 or Fe sub 3 O sub 4) was observed. It was also found that the orientation relationship between alpha-Fe sub 2 O sub 3 and the new phase (gamma-Fe sub 2 O sub 3 or Fe sub 3 O sub 4) satisfies the Shoji-Nishiyama relationship, in agreement with previous experiments. It was also found that the nearest interatomic distance does not vary by the implantation until the re-stacked phase appears, although when the re-stacked phase is formed, the lattice expansion is observed in the transformed (re-stacked) phase. Judging from these results, we have concluded that the alpha-Fe sub 2 O sub 3 to Fe sub 3 O sub 4 transformation is induced during the hydrogen ion implantation of alpha-Fe sub 2 O sub 3.

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.

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.

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...

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

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.

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.

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...

Characterization of TEM1/endosialin in human and murine brain tumors

International Nuclear Information System (INIS)

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

2009-01-01

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

In-situ TEM 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.

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

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.

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

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.

The grand challenge of developing in situ observational oceanography in South Africa

CSIR Research Space (South Africa)

Roberts, M

2010-12-01

Full Text Available , underwater temperature recorders (UTRs), wave buoys, as well as locally developed in situ measurement sensor and platform prototypes (dial-out UTRs, coastal and deep ocean buoys) have been incorporated into a regional in-situ observational network. A modular...

In-situ observation of equilibrium transitions in Ni films; agglomeration and impurity effects

Energy Technology Data Exchange (ETDEWEB)

Thron, Andrew M., E-mail: AMThron@lbl.gov [Department of Chemical Engineering and Materials Science, University of California, Davis, CA 95616 (United States); Greene, Peter; Liu, Kai [Department of Physics, University of California, Davis, CA 95616 (United States); Benthem, Klaus van [Department of Chemical Engineering and Materials Science, University of California, Davis, CA 95616 (United States)

2014-02-01

Dewetting of ultra-thin Ni films deposited on SiO{sub 2} layers was observed, in cross-section, by in situ scanning transmission electron microscopy. Holes were observed to nucleate by voids which formed at the Ni/SiO{sub 2} interface rather than at triple junctions at the free surface of the Ni film. Ni islands were observed to retract, in attempt to reach equilibrium on the SiO{sub 2} layer. SiO{sub 2} layers with 120 nm thickness were found to limit in situ heating experiments due to poor thermal conductivity of SiO{sub 2}. The formation of graphite was observed during the agglomeration of ultra-thin Ni films. Graphite was observed to wet both the free surface and the Ni/SiO{sub 2} interface of the Ni islands. Cr forms surface oxide layers on the free surface of the SiO{sub 2} layer and the Ni islands. Cr does not prevent the dewetting of Ni, however it will likely alter the equilibrium shape of the Ni islands. - Highlights: • In Situ observation of dewetting in ultra-thin Ni films sputtered on SiO{sub 2} layers. • Dewetting is observed in an edge-on position by in situ STEM. • Characterization of interface structure pre and post in situ annealing by STEM and EELS. • Analyze the effects of Cr{sub 1−x}O{sub x} and graphite impurities on the Ni film agglomeration. • Examine influence of the SiO{sub 2} layers on the dewetting process.

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.

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

Science.gov (United States)

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

2013-02-01

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

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.

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.

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.

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.

In-situ observations of stress-induced thin film failures

Energy Technology Data Exchange (ETDEWEB)

Zhao, Z.B., E-mail: zzhao@firstsolar.co [Delphi Research Labs, 51786 Shelby Parkway, Shelby Twp., MI 48315 (United States); Hershberger, J. [Laird Technologies, 4707 Detroit Avenue, Cleveland, Ohio, 44102 (United States); Bilello, J.C. [Department of Materials Science and Engineering, University of Michigan, Ann Arbor, MI 48109-2136 (United States)

2010-02-01

In this work, the failure modes of thin films under thermo-mechanical treatments were observed via in-situ white beam X-ray topography. The in-situ experiments were carried out using an experimental setup on Beamline 2-2 at the Stanford Synchrotron Radiation Laboratory. Magnetron sputtered polycrystalline thin films of Ta and CrN on Si substrates were selected for the present study due to their disparate states of intrinsic residual stresses: the Ta film was anisotropically compressive and the CrN film was isotropically tensile. Under a similar heating-cooling cycle in air, the two types of films exhibited distinct failure modes, which were observed in-situ and in a quasi-real-time fashion. The failures of the samples have been interpreted based on their distinctive growth stress states, superimposed on the additional stress development associated with different forms of thermal instabilities upon heating. These included the formation of oxide for the Ta/Si sample, which led to an increase in compressive stress, and a phase change for the CrN/Si sample, which caused the isotropic stress in the film to become increasingly tensile.

In-situ observations of stress-induced thin film failures

International Nuclear Information System (INIS)

Zhao, Z.B.; Hershberger, J.; Bilello, J.C.

2010-01-01

In this work, the failure modes of thin films under thermo-mechanical treatments were observed via in-situ white beam X-ray topography. The in-situ experiments were carried out using an experimental setup on Beamline 2-2 at the Stanford Synchrotron Radiation Laboratory. Magnetron sputtered polycrystalline thin films of Ta and CrN on Si substrates were selected for the present study due to their disparate states of intrinsic residual stresses: the Ta film was anisotropically compressive and the CrN film was isotropically tensile. Under a similar heating-cooling cycle in air, the two types of films exhibited distinct failure modes, which were observed in-situ and in a quasi-real-time fashion. The failures of the samples have been interpreted based on their distinctive growth stress states, superimposed on the additional stress development associated with different forms of thermal instabilities upon heating. These included the formation of oxide for the Ta/Si sample, which led to an increase in compressive stress, and a phase change for the CrN/Si sample, which caused the isotropic stress in the film to become increasingly tensile.

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

Czech Academy of Sciences Publication Activity Database

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

2008-01-01

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

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.

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

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

International Nuclear Information System (INIS)

Zakhozheva, Marina

2016-01-01

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

A 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.)

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.

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.

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

DEFF Research Database (Denmark)

Canepa, Silvia

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

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

Science.gov (United States)

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

2006-12-01

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

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

International Nuclear Information System (INIS)

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

2006-01-01

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

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.

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.)

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....

Electrochemical synthesis, in situ spectroelectrochemistry of conducting indole-titanium dioxide and zinc oxide polymer nanocomposites for rechargeable batteries

International Nuclear Information System (INIS)

Parvin, Mohammad Hadi; Pirnia, Mahsa; Arjomandi, Jalal

2015-01-01

Highlights: • Two novel hybrid materials-based conducting PIn rechargeable batteries were developed. • The charge-discharging behavior of PIn-nanocomposite batteries were studied. • The characterization of samples has been done by in situ spectroelectrochemical method. • PIn-TiO 2 and ZnO nanocomposites were synthesized electrochemically on Au and ITO. • The PIn-TiO 2 and ZnO nanocomposites resistances were less than PIn. - Abstract: Electrochemical synthesis, in situ spectroelectrochemistry of conducting polyindole (PIn), polyindole-TiO 2 (PIn-TiO 2 ) and polyindole-ZnO (PIn-ZnO) nanocomposites were investigated. The PIn and polymer nanocomposites were tested electrochemically for rechargeable batteries. The films were characterized by means of CVs, in situ UV-visible, FT-IR spectroscopies, in situ resistivity measurements, energy dispersive X-ray (EDX), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The charge-discharging behavior of a Zn/1 M ZnSO 4 /PIn cell with a capacity of around 90 Ah Kg −1 and on open circuit potential of around 1.45 V was compared with Zn/1 M ZnSO 4 /PIn-nanocomposite. The potential differences of redox couples (ΔE) for nanocomposites films show very good reversibility. A positive shift of potential was observed for polymer nanocomposites during redox scan. A significant variability was observed for in situ conductivity of the PIn and polymer nanocomposites. During in situ UV-visible and FT-IR measurements, intermediate spectroscopic behavior and positive shifts of wavelengths were observed for PIn and polymer nanocomposites. The SEM, TEM and EDX of nanocomposite films show the presence of nano particle in PIn.

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.

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)

In situ observations of Pc1 pearl pulsations by the Van Allen Probes

Science.gov (United States)

Paulson, K. W.; Smith, C. W.; Lessard, M. R.; Engebretson, M. J.; Torbert, R. B.; Kletzing, C. A.

2014-03-01

We present in situ observations of Pc1 pearl pulsations using the Van Allen Probes. These waves are often observed using ground-based magnetometers, but are rarely observed by orbiting satellites. With the Van Allen Probes, we have seen at least 14 different pearl pulsation events during the first year of operations. These new in situ measurements allow us to identify the wave classification based on local magnetic field conditions. Additionally, by using two spacecraft, we are able to observe temporal changes in the region of observation. The waves appear to be generated at an overall central frequency, as often observed on the ground, and change polarization from left- to right-handedness as they propagate into a region where they are resonant with the crossover frequency (where R- and L-mode waves have the same phase velocity). By combining both in situ and ground-based data, we have found that the region satisfying electromagnetic ion cyclotron wave generation conditions is azimuthally large while radially narrow. The observation of a similar modulation period on the ground as in the magnetosphere contradicts the bouncing wave packet mechanism of generation.

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.

Solar Ion Processing of Major Element Surface Compositions of Mature Mare Soils: Insights from Combined XPS and Analytical TEM Observations

Science.gov (United States)

Christoffersen, R.; Dukes, C.; Keller, L. P.; Baragiola, R.

2012-01-01

Solar wind ions are capable of altering the sur-face chemistry of the lunar regolith by a number of mechanisms including preferential sputtering, radiation-enhanced diffusion and sputter erosion of space weathered surfaces containing pre-existing compositional profiles. We have previously reported in-situ ion irradiation experiments supported by X-ray photoelectron spectroscopy (XPS) and analytical TEM that show how solar ions potentially drive Fe and Ti reduction at the monolayer scale as well as the 10-100 nm depth scale in lunar soils [1]. Here we report experimental data on the effect of ion irradiation on the major element surface composition in a mature mare soil.

Synthesis and characterization of polypropylene/graphite nano composite preparation for in situ polymerization; Sintese e caracterizacao de nanocompositos polipropileno/grafite obtidos pela polimerizacao in situ

Energy Technology Data Exchange (ETDEWEB)

Montagna, L.S.; Fim, F. de C.; Galland, G.B. [Universidade Federal do Rio Grande do Sul (UFRGS), Porto Alegre, RS (Brazil). Inst. de Quimica; Basso, N.R.S., E-mail: nrbass@pucrs.b [Pontificia Universidade Catolica do Rio Grande do Sul (PUC-RS), Porto Alegre, RS (Brazil)

2010-07-01

This paper presents the synthesis of polypropylene/graphite nanocomposites through in situ polymerization, using the metallocene catalyst C{sub 20}H{sub 16}Cl{sub 2}Zr (dichloro(rac-ethylenebis(indenyl))zircon(IV)). The graphite nanosheets in nano dimensions were added to the polymer matrix in percentages of 0.6;1.0;4.2;4.8 and 6.0% (w/w). The TEM images indicated that the thickness of graphite nanosheets ranged from 4 to 60 nm and by means of XRD analysis it was observed that the physical and chemical treatment did not destroyed the graphite layers. The presence of nanosheets did not decrease the catalytic activity of the nanocomposites. TEM images and XRD analysis of nanocomposites showed a good dispersion of the graphite nanosheets in the polypropylene matrix. (author)

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

Grain rotation and lattice deformation during photoinduced chemical reactions revealed by in situ X-ray nanodiffraction.

Science.gov (United States)

Huang, Zhifeng; Bartels, Matthias; Xu, Rui; Osterhoff, Markus; Kalbfleisch, Sebastian; Sprung, Michael; Suzuki, Akihiro; Takahashi, Yukio; Blanton, Thomas N; Salditt, Tim; Miao, Jianwei

2015-07-01

In situ X-ray diffraction (XRD) and transmission electron microscopy (TEM) have been used to investigate many physical science phenomena, ranging from phase transitions, chemical reactions and crystal growth to grain boundary dynamics. A major limitation of in situ XRD and TEM is a compromise that has to be made between spatial and temporal resolution. Here, we report the development of in situ X-ray nanodiffraction to measure high-resolution diffraction patterns from single grains with up to 5 ms temporal resolution. We observed, for the first time, grain rotation and lattice deformation in chemical reactions induced by X-ray photons: Br(-) + hv → Br + e(-) and e(-) + Ag(+) → Ag(0). The grain rotation and lattice deformation associated with the chemical reactions were quantified to be as fast as 3.25 rad s(-1) and as large as 0.5 Å, respectively. The ability to measure high-resolution diffraction patterns from individual grains with a temporal resolution of several milliseconds is expected to find broad applications in materials science, physics, chemistry and nanoscience.

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

In situ Transmission Electron Microscopy of catalyst sintering

DEFF Research Database (Denmark)

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

2013-01-01

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

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.

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

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)

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

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

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

International Nuclear Information System (INIS)

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

2016-01-01

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

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

International Nuclear Information System (INIS)

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

2014-01-01

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

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.

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

In-situ observation of equilibrium transitions in Ni films; agglomeration and impurity effects.

Science.gov (United States)

Thron, Andrew M; Greene, Peter; Liu, Kai; van Benthem, Klaus

2014-02-01

Dewetting of ultra-thin Ni films deposited on SiO2 layers was observed, in cross-section, by in situ scanning transmission electron microscopy. Holes were observed to nucleate by voids which formed at the Ni/SiO2 interface rather than at triple junctions at the free surface of the Ni film. Ni islands were observed to retract, in attempt to reach equilibrium on the SiO2 layer. SiO2 layers with 120 nm thickness were found to limit in situ heating experiments due to poor thermal conductivity of SiO2. The formation of graphite was observed during the agglomeration of ultra-thin Ni films. Graphite was observed to wet both the free surface and the Ni/SiO2 interface of the Ni islands. Cr forms surface oxide layers on the free surface of the SiO2 layer and the Ni islands. Cr does not prevent the dewetting of Ni, however it will likely alter the equilibrium shape of the Ni islands. © 2013 Published by Elsevier B.V.

Are Global In-Situ Ocean Observations Fit-for-purpose? Applying the Framework for Ocean Observing in the Atlantic.

Science.gov (United States)

Visbeck, M.; Fischer, A. S.; Le Traon, P. Y.; Mowlem, M. C.; Speich, S.; Larkin, K.

2015-12-01

There are an increasing number of global, regional and local processes that are in need of integrated ocean information. In the sciences ocean information is needed to support physical ocean and climate studies for example within the World Climate Research Programme and its CLIVAR project, biogeochemical issues as articulated by the GCP, IMBER and SOLAS projects of ICSU-SCOR and Future Earth. This knowledge gets assessed in the area of climate by the IPCC and biodiversity by the IPBES processes. The recently released first World Ocean Assessment focuses more on ecosystem services and there is an expectation that the Sustainable Development Goals and in particular Goal 14 on the Ocean and Seas will generate new demands for integrated ocean observing from Climate to Fish and from Ocean Resources to Safe Navigation and on a healthy, productive and enjoyable ocean in more general terms. In recognition of those increasing needs for integrated ocean information we have recently launched the Horizon 2020 AtlantOS project to promote the transition from a loosely-coordinated set of existing ocean observing activities to a more integrated, more efficient, more sustainable and fit-for-purpose Atlantic Ocean Observing System. AtlantOS takes advantage of the Framework for Ocean observing that provided strategic guidance for the design of the project and its outcome. AtlantOS will advance the requirements and systems design, improving the readiness of observing networks and data systems, and engaging stakeholders around the Atlantic. AtlantOS will bring Atlantic nations together to strengthen their complementary contributions to and benefits from the internationally coordinated Global Ocean Observing System (GOOS) and the Blue Planet Initiative of the Global Earth Observation System of Systems (GEOSS). AtlantOS will fill gaps of the in-situ observing system networks and will ensure that their data are readily accessible and useable. AtlantOS will demonstrate the utility of

TEM studies of nanostructure in melt-spun Mg-Ni-La alloy manifesting enhanced hydrogen desorbing kinetics

International Nuclear Information System (INIS)

Tanaka, K.; Miwa, T.; Sasaki, K.; Kuroda, K.

2009-01-01

The hydrogen storage properties of a magnesium-rich Mg-Ni-La alloy prepared by melt-spinning are significantly improved by nanostructure formation during crystallization and activation. It can absorb and desorb ∼5 wt% hydrogen at temperatures as low as 200 deg. C in moderate time periods. Transmission electron microscopic (TEM) studies on this alloy indicate that the nanostructure, consisting of LaH 3 and Mg 2 NiH 4 nano-particles dispersed homogeneously in MgH 2 matrices after hydrogenation, is rather stable at temperatures below 300 deg. C but undergoes coarsening and segregation of these particles and matrices above ∼400 deg. C. These structural changes have been confirmed by electron energy-loss spectroscopic (EELS) imaging as well as high-resolution TEM techniques. A new EELS peak associated with a plasmon excitation in the MgH 2 phase (H-plasmon) is found for the first time in this study. By imaging the H-plasmon peak, the hydrogen distribution in the alloy has been clearly visualized. We have succeeded in observing the hydrogen desorption process at ∼400 deg. C in-situ in the microscope using this EELS imaging technique.

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

International Nuclear Information System (INIS)

Allen, C.W.

1994-01-01

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

In situ observation of self-assembled Fe{sub 13}Ge{sub 8} nanowires growth on anisotropic Ge (1 1 0) surface

Energy Technology Data Exchange (ETDEWEB)

Li, Zhi-Peng, E-mail: LI.Zhipeng@nims.go.jp [Department of Physics, National University of Singapore, 2 Science Drive 3, S117542 (Singapore); Global Research Center for Environment and Energy based on Nanomaterials Science, National Institute for Materials Science, 1-1 Namiki, Tsukuba, Ibaraki 305-0044 (Japan); Tok, Engsoon [Department of Physics, National University of Singapore, 2 Science Drive 3, S117542 (Singapore); Foo, Yonglim [Institute of Materials Research and Engineering, 3 Research Link, S117602 (Singapore)

2012-02-15

Highlights: Black-Right-Pointing-Pointer Epitaxial Fe{sub 13}Ge{sub 8} nanowries growth and shape evolution on Ge (1 1 0) studied by in situ UHV-TEM. Black-Right-Pointing-Pointer Single type of morphology and unique orientation of nanowires formed at elevated temperatures. Black-Right-Pointing-Pointer Uniform control of the nanowires morphology at different temperatures can be succeeded. -- Abstract: Self-assembled iron germanide nanowires (NWs) were grown by directly depositing Fe onto a Ge (1 1 0) substrate, in an in situ ultra-high vacuum transmission electron microscope from 430 to 500 Degree-Sign C. All observed NWs had a similar length/width aspect ratio ({approx}8:1) at all deposition temperatures, as well as the same elongation orientation with respect to the underlying Ge (1 1 0) substrate. The growth dynamics was investigated by real time observations of NWs growth at elevated temperatures. It is elucidated that the formation of NWs in similar shape at all deposited temperatures is attributed to the similar activation energy barriers in length and width of NWs, which can result in the constant growth rate independent of growth temperatures. Furthermore, the difference in pre-exponential factor along the length and width of growing islands arose due to the anisotropic constraint of the Ge (1 1 0) substrate, leading to the unique elongation of NWs. This growth dynamics suggests the possibility of uniform control of the morphology of self-assembled NWs, as well as other morphologies of bottom-up fabricated devices, at different deposition temperatures.

In situ observation of a soap-film catenoid-a simple educational physics experiment

International Nuclear Information System (INIS)

Ito, Masato; Sato, Taku

2010-01-01

The solution to the Euler-Lagrange equation is an extremal functional. To understand that the functional is stationary at local extrema (maxima or minima), we propose a physics experiment that involves using a soap film to form a catenoid. A catenoid is a surface that is formed between two coaxial circular rings and is classified mathematically as a minimal surface. Using the soap film, we create catenoids between two rings and characterize the catenoid in situ while varying the distance between the rings. The shape of the soap film is very interesting and can be explained using dynamic mechanics. By observing the catenoid, physics students can observe local extrema phenomena. We stress that in situ observation of soap-film catenoids is an appropriate physics experiment that combines theory and experimentation.

In situ observation of a soap-film catenoid-a simple educational physics experiment

Energy Technology Data Exchange (ETDEWEB)

Ito, Masato; Sato, Taku [Department of Physics, Aichi University of Education, Kariya, 448-8542 (Japan)], E-mail: mito@auecc.aichi-edu.ac.jp

2010-03-15

The solution to the Euler-Lagrange equation is an extremal functional. To understand that the functional is stationary at local extrema (maxima or minima), we propose a physics experiment that involves using a soap film to form a catenoid. A catenoid is a surface that is formed between two coaxial circular rings and is classified mathematically as a minimal surface. Using the soap film, we create catenoids between two rings and characterize the catenoid in situ while varying the distance between the rings. The shape of the soap film is very interesting and can be explained using dynamic mechanics. By observing the catenoid, physics students can observe local extrema phenomena. We stress that in situ observation of soap-film catenoids is an appropriate physics experiment that combines theory and experimentati0008.

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.

In situ observation of mechanical damage within a SiC-SiC ceramic matrix composite

Energy Technology Data Exchange (ETDEWEB)

Saucedo-Mora, L. [Institute Eduardo Torroja for Construction Sciences-CSIC, Madrid (Spain); Department of Materials, University of Oxford (United Kingdom); Lowe, T. [Manchester X-ray Imaging Facility, The University of Manchester (United Kingdom); Zhao, S. [Department of Materials, University of Oxford (United Kingdom); Lee, P.D. [Research Complex at Harwell, Rutherford Appleton Laboratory (United Kingdom); Mummery, P.M. [School of Mechanical, Aerospace and Civil Engineering, The University of Manchester (United Kingdom); Marrow, T.J., E-mail: james.marrow@materials.ox.ac.uk [Department of Materials, University of Oxford (United Kingdom)

2016-12-01

SiC-SiC ceramic matrix composites are candidate materials for fuel cladding in Generation IV nuclear fission reactors and as accident tolerant fuel clad in current generation plant. Experimental methods are needed that can detect and quantify the development of mechanical damage, to support modelling and qualification tests for these critical components. In situ observations of damage development have been obtained of tensile and C-ring mechanical test specimens of a braided nuclear grade SiC-SiC ceramic composite tube, using a combination of ex situ and in situ computed X-ray tomography observation and digital volume correlation analysis. The gradual development of damage by matrix cracking and also the influence of non-uniform loading are examined. - Highlights: • X-ray tomography with digital volume correlation measures 3D deformation in situ. • Cracking and damage in the microstructure can be detected using the strain field. • Fracture can initiate from the monolithic coating of a SiC-SiC ceramic composite.

In situ observation of mechanical damage within a SiC-SiC ceramic matrix composite

International Nuclear Information System (INIS)

Saucedo-Mora, L.; Lowe, T.; Zhao, S.; Lee, P.D.; Mummery, P.M.; Marrow, T.J.

2016-01-01

SiC-SiC ceramic matrix composites are candidate materials for fuel cladding in Generation IV nuclear fission reactors and as accident tolerant fuel clad in current generation plant. Experimental methods are needed that can detect and quantify the development of mechanical damage, to support modelling and qualification tests for these critical components. In situ observations of damage development have been obtained of tensile and C-ring mechanical test specimens of a braided nuclear grade SiC-SiC ceramic composite tube, using a combination of ex situ and in situ computed X-ray tomography observation and digital volume correlation analysis. The gradual development of damage by matrix cracking and also the influence of non-uniform loading are examined. - Highlights: • X-ray tomography with digital volume correlation measures 3D deformation in situ. • Cracking and damage in the microstructure can be detected using the strain field. • Fracture can initiate from the monolithic coating of a SiC-SiC ceramic composite.

Blending Satellite Observed, Model Simulated, and in Situ Measured Soil Moisture over Tibetan Plateau

Directory of Open Access Journals (Sweden)

Yijian Zeng

2016-03-01

Full Text Available The inter-comparison of different soil moisture (SM products over the Tibetan Plateau (TP reveals the inconsistency among different SM products, when compared to in situ measurement. It highlights the need to constrain the model simulated SM with the in situ measured data climatology. In this study, the in situ soil moisture networks, combined with the classification of climate zones over the TP, were used to produce the in situ measured SM climatology at the plateau scale. The generated TP scale in situ SM climatology was then used to scale the model-simulated SM data, which was subsequently used to scale the SM satellite observations. The climatology-scaled satellite and model-simulated SM were then blended objectively, by applying the triple collocation and least squares method. The final blended SM can replicate the SM dynamics across different climatic zones, from sub-humid regions to semi-arid and arid regions over the TP. This demonstrates the need to constrain the model-simulated SM estimates with the in situ measurements before their further applications in scaling climatology of SM satellite products.

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

International Nuclear Information System (INIS)

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

2011-01-01

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

First In-Situ Observations of Exospheric Response to CME Impact at Mercury

Science.gov (United States)

Raines, J. M.; Wallace, K. L.; Sarantos, M.; Jasinksi, J. M.; Tracy, P. J.; Dewey, R. M.; Weberg, M. J.; Slavin, J. A.

2018-05-01

We present the first in-situ observations of enhancements to Mercury's He exosphere generated by CME impact. These results have implications for understanding exosphere generation and loss processes, as well space weathering of the planet's surface.

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

International Nuclear Information System (INIS)

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

2014-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2014-03-10

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

Synthesis and characterization of polypropylene/graphite nano composite preparation for in situ polymerization

International Nuclear Information System (INIS)

Montagna, L.S.; Fim, F. de C.; Galland, G.B.

2010-01-01

This paper presents the synthesis of polypropylene/graphite nanocomposites through in situ polymerization, using the metallocene catalyst C 20 H 16 Cl 2 Zr (dichloro(rac-ethylenebis(indenyl))zircon(IV)). The graphite nanosheets in nano dimensions were added to the polymer matrix in percentages of 0.6;1.0;4.2;4.8 and 6.0% (w/w). The TEM images indicated that the thickness of graphite nanosheets ranged from 4 to 60 nm and by means of XRD analysis it was observed that the physical and chemical treatment did not destroyed the graphite layers. The presence of nanosheets did not decrease the catalytic activity of the nanocomposites. TEM images and XRD analysis of nanocomposites showed a good dispersion of the graphite nanosheets in the polypropylene matrix. (author)

In situ statistical observations of EMIC waves by Arase satellite

Science.gov (United States)

Nomura, R.; Matsuoka, A.; Teramoto, M.; Nose, M.; Yoshizumi, M.; Fujimoto, A.; Shinohara, M.; Tanaka, Y.

2017-12-01

We present in situ statistical survey of electromagnetic ion cyclotron (EMIC) waves observed by Arase satellite from 3 March to 16 July 2017. We identified 64 events using the fluxgate magnetometer (MGF) on the satellite. The EMIC wave is the key phenomena to understand the loss dynamics of MeV-energy electrons in the radiation belt. We will show the radial and latitudinal dependence of the wave occurance rate and the wave parameters (frequency band, coherence, polarization, and ellipticity). Especially the EMIC waves observed at localized weak background magnetic field will be discussed for the wave excitation mechanism in the deep inner magnetosphere.

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

International Nuclear Information System (INIS)

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

1986-09-01

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

In Situ Electron Microscopy of Lactomicroselenium Particles in Probiotic Bacteria

Directory of Open Access Journals (Sweden)

Gabor Nagy

2016-06-01

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

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

In situ observation of a hydrogel-glass interface during sliding friction

OpenAIRE

Yamamoto, Tetsurou; Kurokawa, Takayuki; Ahmed, Jamil; Kamita, Gen; Yashima, Shintaro; Furukawa, Yuichiro; Ota, Yuko; Furukawa, Hidemitsu; Gong, Jian Ping

2014-01-01

Direct observation of hydrogel contact with a solid surface in water is indispensable for understanding the friction, lubrication, and adhesion of hydrogels under water. However, this is a difficult task since the refractive index of hydrogels is very close to that of water. In this paper, we present a novel method to in situ observe the macroscopic contact of hydrogels with a solid surface based on the principle of critical refraction. This method was applied to investigate the sliding frict...

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

Energy Technology Data Exchange (ETDEWEB)

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

2016-12-15

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

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

Science.gov (United States)

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

2018-03-01

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

In situ observation of stress relaxation in epitaxial graphene

International Nuclear Information System (INIS)

N'Diaye, Alpha T; Coraux, Johann; Busse, Carsten; Michely, Thomas; Gastel, Raoul van; Poelsema, Bene; MartInez-Galera, Antonio J; Gomez-RodrIguez, Jose M; Hattab, Hichem; Wall, Dirk; Heringdorf, Frank-J Meyer zu; Hoegen, Michael Horn-von

2009-01-01

Upon cooling, branched line defects develop in epitaxial graphene grown at high temperature on Pt(111) and Ir(111). Using atomically resolved scanning tunneling microscopy, we demonstrate that these defects are wrinkles in the graphene layer, i.e. stripes of partially delaminated graphene. With low energy electron microscopy (LEEM), we investigate the wrinkling phenomenon in situ. Upon temperature cycling, we observe hysteresis in the appearance and disappearance of the wrinkles. Simultaneously with wrinkle formation a change in bright field imaging intensity of adjacent areas and a shift in the moire spot positions for micro diffraction of such areas takes place. The stress relieved by wrinkle formation results from the mismatch in thermal expansion coefficients of graphene and the substrate. A simple one-dimensional model taking into account the energies related to strain, delamination and bending of graphene is in qualitative agreement with our observations.

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

International Nuclear Information System (INIS)

Allen, C.W.

1992-01-01

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

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

DEFF Research Database (Denmark)

Gardini, Diego

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

Delayed formation of chromosome aberrations in mouse pachytebne spermatocytes treated with triethylenemelamine (TEM)

International Nuclear Information System (INIS)

Generoso, W.M.; Krishna, M.; Sotomayor, R.E.; Cacheiro, N.L.A.

1977-01-01

Induction of chromosome aberrations in pachytene spermatocytes of mice by 2 mg/kg TEM was compared with induction by 400 R x rays. These doses induced comparably high dominant lethal effects in pachytene spermatocytes of mice. Cytological analysis at diakinesis-metaphase I stage showed that whereas 76.4% of the cells treated with x rays at pachytene stage had aberrations, the frequencies observed in two TEM experiments were only 0.8 and 2.2%. On the other hand, 5% of the progeny from TEM-treated pachytene spermatocytes were found to be translocation heterozygotes. This is the first report on the recovery of heritable translocations from treated spermatocytes of mice. The aberration frequencies observed for TEM in diakinesis-metaphase I were much too low to account for all the lethal mutations and heritable translocations. Thus, the formation of the bulk of aberrations induced by TEM in pachytene spermatocytes was delayed--a marked contrast to the more immediate formation of x-ray-induced aberrations. It is postulated that the formation of the bulk of TEM-induced aberrations in pachytene spermatocytes and in certain postmeiotic stages occurs sometime during spermiogenesis, and not through the operation of postfertilization pronuclear DNA synthesis

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.

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)

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)

In-situ observation of crack propagation in thermally sprayed coatings

Czech Academy of Sciences Publication Activity Database

Mušálek, R.; Kovářík, O.; Matějíček, Jiří

2010-01-01

Roč. 205, č. 7 (2010), s. 1807-1811 ISSN 0257-8972 R&D Projects: GA MŠk ME 901 Institutional research plan: CEZ:AV0Z20430508 Keywords : coating fracture * in-situ observation * alumina * stainless steel * plasma spraying Subject RIV: JL - Materials Fatigue, Friction Mechanics Impact factor: 2.135, year: 2010 http://www.sciencedirect.com/science?_ob=GatewayURL&_method=citationSearch&_uoikey=B6TVV-4YTFBCY-5&_origin=SDEMFRHTML&_version=1&md5=896533bcc989ebaa374ff209558fbcf1

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

International Nuclear Information System (INIS)

Gai, P L; Boyes, E D

2014-01-01

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

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.

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...

Atomistic observations and analyses of lattice defects in transmission electron microscopes

CERN Document Server

Abe, H

2003-01-01

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

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

Current status and future directions for in situ transmission electron microscopy

Energy Technology Data Exchange (ETDEWEB)

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

2016-11-15

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

Current status and future directions for in situ transmission electron microscopy

International Nuclear Information System (INIS)

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

2016-01-01

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

In SITU Transmission Electron Microscopy on Operating Electrochemical CELLS

DEFF Research Database (Denmark)

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

2016-01-01

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

Interpretation of TOMS Observations of Tropical Tropospheric Ozone with a Global Model and In Situ Observations

Science.gov (United States)

Martin, Randall V.; Jacob, Daniel J.; Logan, Jennifer A.; Bey, Isabelle; Yantosca, Robert M.; Staudt, Amanda C.; Fiore, Arlene M.; Duncan, Bryan N.; Liu, Hongyu; Ginoux, Paul

2004-01-01

We interpret the distribution of tropical tropospheric ozone columns (TTOCs) from the Total Ozone Mapping Spectrometer (TOMS) by using a global three-dimensional model of tropospheric chemistry (GEOS-CHEM) and additional information from in situ observations. The GEOS-CHEM TTOCs capture 44% of the variance of monthly mean TOMS TTOCs from the convective cloud differential method (CCD) with no global bias. Major discrepancies are found over northern Africa and south Asia where the TOMS TTOCs do not capture the seasonal enhancements from biomass burning found in the model and in aircraft observations. A characteristic feature of these northern topical enhancements, in contrast to southern tropical enhancements, is that they are driven by the lower troposphere where the sensitivity of TOMS is poor due to Rayleigh scattering. We develop an efficiency correction to the TOMS retrieval algorithm that accounts for the variability of ozone in the lower troposphere. This efficiency correction increases TTOC's over biomass burning regions by 3-5 Dobson units (DU) and decreases them by 2-5 DU over oceanic regions, improving the agreement between CCD TTOCs and in situ observations. Applying the correction to CCD TTOCs reduces by approximately DU the magnitude of the "tropical Atlantic paradox" [Thompson et al, 2000], i.e. the presence of a TTOC enhancement over the southern tropical Atlantic during the northern African biomass burning season in December-February. We reproduce the remainder of the paradox in the model and explain it by the combination of upper tropospheric ozone production from lightning NOx, peristent subsidence over the southern tropical Atlantic as part of the Walker circulation, and cross-equatorial transport of upper tropospheric ozone from northern midlatitudes in the African "westerly duct." These processes in the model can also account for the observed 13-17 DU persistent wave-1 pattern in TTOCs with a maximum above the tropical Atlantic and a minimum

Harmonising and semantically linking key variables from in-situ observing networks of an Integrated Atlantic Ocean Observing System, AtlantOS

Science.gov (United States)

Darroch, Louise; Buck, Justin

2017-04-01

Atlantic Ocean observation is currently undertaken through loosely-coordinated, in-situ observing networks, satellite observations and data management arrangements at regional, national and international scales. The EU Horizon 2020 AtlantOS project aims to deliver an advanced framework for the development of an Integrated Atlantic Ocean Observing System that strengthens the Global Ocean Observing System (GOOS) and contributes to the aims of the Galway Statement on Atlantic Ocean Cooperation. One goal is to ensure that data from different and diverse in-situ observing networks are readily accessible and useable to a wider community, including the international ocean science community and other stakeholders in this field. To help achieve this goal, the British Oceanographic Data Centre (BODC) produced a parameter matrix to harmonise data exchange, data flow and data integration for the key variables acquired by multiple in-situ AtlantOS observing networks such as ARGO, Seafloor Mapping and OceanSITES. Our solution used semantic linking of controlled vocabularies and metadata for parameters that were "mappable" to existing EU and international standard vocabularies. An AtlantOS Essential Variables list of terms (aggregated level) based on Global Climate Observing System (GCOS) Essential Climate Variables (ECV), GOOS Essential Ocean Variables (EOV) and other key network variables was defined and published on the Natural Environment Research Council (NERC) Vocabulary Server (version 2.0) as collection A05 (http://vocab.nerc.ac.uk/collection/A05/current/). This new vocabulary was semantically linked to standardised metadata for observed properties and units that had been validated by the AtlantOS community: SeaDataNet parameters (P01), Climate and Forecast (CF) Standard Names (P07) and SeaDataNet units (P06). Observed properties were mapped to biological entities from the internationally assured AphiaID from the WOrld Register of Marine Species (WoRMS), http

Direct observation of magnetization reversal of hot-deformed Nd-Fe-B magnet

Science.gov (United States)

Zhu, Xiaoyun; Tang, Xu; Pei, Ke; Tian, Yue; Liu, Jinjun; Xia, Weixing; Zhang, Jian; Liu, J. Ping; Chen, Renjie; Yan, Aru

2018-01-01

The dynamic magnetic domain structure in magnetization and demagnetization process of hot-deformed and NdCu-diffused Nd2Fe14B magnets were in-situ observed by Lorentz transmission electron microscopy (LTEM). The demagnetization process of hot-deformed sample is dominated by domain-wall pinning, while that of NdCu-diffused sample is mainly the magnetization reversal of single grains or grain aggregations. This firstly observed result gives an explicit evidence to understand the coercivity mechanism of magnetically segregated magnet. The effect of magnetic field of TEM on decrease in domain wall energy was theoretically analyzed, which helps to understand the in-situ observation process of magnetic materials.

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.

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

3D in situ observations of glass fibre/matrix interfacial debonding

DEFF Research Database (Denmark)

Martyniuk, Karolina; Sørensen, Bent F.; Modregger, Peter

2013-01-01

X-ray microtomography was used for 3D in situ observations of the evolution of fibre/matrix interfacial debonding. A specimen with a single fibre oriented perpendicular to the tensile direction was tested at a synchrotron facility using a special loading rig which allowed for applying a load...... transverse to the fibre. Three distinguishable damage stages were observed: (i) interfacial debond initiation at the free surface, (ii) debond propagation from the surface into the specimen and (iii) unstable debonding along the full length of the scanned volume. The high resolution microtomography provides...

XRD and TEM analysis of microstructure in the welding zone of 9Cr ...

Indian Academy of Sciences (India)

Unknown

XRD and TEM analysis of microstructure in the welding zone of. 9Cr–1Mo–V–Nb ... steel, which has highest Cr content in the heat-resisting. Cr–Mo ... This research provides essential ... film samples were observed under TEM and select elec-.

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

Science.gov (United States)

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

2017-02-01

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

Structure and Properties of Nanocomposites based on PTT-block-PTMO Copolymer and Graphene Oxide prepared by in Situ Polymerization

OpenAIRE

Paszkiewicz, Sandra; Szymczyk, Anna; Špitalský, Zdenko; Mosnáček, Jaroslav; Kwiatkowski, Konrad; Rosłaniec, Zbigniew

2014-01-01

Poly(trimethylene terephthalate-block-tetramethylene oxide) (PTT-PTMO) copolymer/graphene oxide nanocomposites were prepared by in situ polymerization. From the SEM and TEM images of PTT-PTMO/GO nanocomposite, it can be seen that GO sheets are clearly well-dispersed in the PTT-PTMO matrix. TEM images also showed that graphene was well exfoliated into individual sheets, suggesting that in situ polymerization is a highly efficient method for preparing nanocomposites. The influence of GO on the ...

Gulf of Maine Harmful Algal Bloom in summer 2005 - Part 1: In Situ Observations of Coastal Hydrography and Circulation

OpenAIRE

He, Ruoying; McGillicuddy, Dennis J.

2008-01-01

An extensive Alexandrium fundyense bloom occurred along the coast of the Gulf of Maine in late spring and early summer, 2005. To understand the physical aspects of bloom?s initiation and development, in-situ observations from both a gulf-wide ship survey and the coastal observing network were used to characterize coastal circulation and hydrography during that time period. Comparisons between these in-situ observations and their respective long term means revealed anomalous ocean conditions d...

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

Science.gov (United States)

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

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

Dynamical 'in situ' observation of biological samples using variable pressure scanning electron microscope

International Nuclear Information System (INIS)

Nedela, V

2008-01-01

Possibilities of 'in-situ' observation of non-conductive biological samples free of charging artefacts in dynamically changed surrounding conditions are the topic of this work. The observed biological sample, the tongue of a rat, was placed on a cooled Peltier stage. We studied the visibility of topographical structure depending on transition between liquid and gas state of water in the specimen chamber of VP SEM.

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

Science.gov (United States)

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

2017-12-01

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

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

International Nuclear Information System (INIS)

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

2000-01-01

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

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

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.

Advanced electron holography techniques for in situ observation of solid-state lithium ion conductors

Energy Technology Data Exchange (ETDEWEB)

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

2017-05-15

Advanced techniques for overcoming problems encountered during in situ electron holography experiments in which a voltage is applied to an ionic conductor are reported. The three major problems encountered were 1) electric-field leakage from the specimen and its effect on phase images, 2) high electron conductivity of damage layers formed by the focused ion beam method, and 3) chemical reaction of the specimen with air. The first problem was overcome by comparing experimental phase distributions with simulated images in which three-dimensional leakage fields were taken into account, the second by removing the damage layers using a low-energy narrow Ar ion beam, and the third by developing an air-tight biasing specimen holder. - Highlights: • Phase distributions derived by comparing experimental and simulated measurements. • Simulations take into account leakage electric fields. • Electric potential distributions inside Li-ion conductors are obtained. • FIB damage layers are removed using a low-energy narrow Ar ion beam. • An air-tight biasing TEM holder for protecting air-sensitive specimens is reported.

The Isinglass Auroral Sounding Rocket Campaign: data synthesis incorporating remote sensing, in situ observations, and modelling

Science.gov (United States)

Lynch, K. A.; Clayton, R.; Roberts, T. M.; Hampton, D. L.; Conde, M.; Zettergren, M. D.; Burleigh, M.; Samara, M.; Michell, R.; Grubbs, G. A., II; Lessard, M.; Hysell, D. L.; Varney, R. H.; Reimer, A.

2017-12-01

The NASA auroral sounding rocket mission Isinglass was launched from Poker Flat Alaska in winter 2017. This mission consists of two separate multi-payload sounding rockets, over an array of groundbased observations, including radars and filtered cameras. The science goal is to collect two case studies, in two different auroral events, of the gradient scale sizes of auroral disturbances in the ionosphere. Data from the in situ payloads and the groundbased observations will be synthesized and fed into an ionospheric model, and the results will be studied to learn about which scale sizes of ionospheric structuring have significance for magnetosphere-ionosphere auroral coupling. The in situ instrumentation includes thermal ion sensors (at 5 points on the second flight), thermal electron sensors (at 2 points), DC magnetic fields (2 point), DC electric fields (one point, plus the 4 low-resource thermal ion RPA observations of drift on the second flight), and an auroral precipitation sensor (one point). The groundbased array includes filtered auroral imagers, the PFISR and SuperDarn radars, a coherent scatter radar, and a Fabry-Perot interferometer array. The ionospheric model to be used is a 3d electrostatic model including the effects of ionospheric chemistry. One observational and modelling goal for the mission is to move both observations and models of auroral arc systems into the third (along-arc) dimension. Modern assimilative tools combined with multipoint but low-resource observations allow a new view of the auroral ionosphere, that should allow us to learn more about the auroral zone as a coupled system. Conjugate case studies such as the Isinglass rocket flights allow for a test of the models' intepretation by comparing to in situ data. We aim to develop and improve ionospheric models to the point where they can be used to interpret remote sensing data with confidence without the checkpoint of in situ comparison.

In Situ Observation of Antisite Defect Formation during Crystal Growth

International Nuclear Information System (INIS)

Kramer, M. J.; Napolitano, R. E.; Mendelev, M. I.

2010-01-01

In situ x-ray diffraction (XRD) coupled with molecular dynamics (MD) simulations have been used to quantify antisite defect trapping during crystallization. Rietveld refinement of the XRD data revealed a marked lattice distortion which involves an a axis expansion and a c axis contraction of the stable C11b phase. The observed lattice response is proportional in magnitude to the growth rate, suggesting that the behavior is associated with the kinetic trapping of lattice defects. MD simulations demonstrate that this lattice response is due to incorporation of 1% to 2% antisite defects during growth.

Direct observation of magnetization reversal of hot-deformed Nd-Fe-B magnet

Directory of Open Access Journals (Sweden)

Xiaoyun Zhu

2018-01-01

Full Text Available The dynamic magnetic domain structure in magnetization and demagnetization process of hot-deformed and NdCu-diffused Nd2Fe14B magnets were in-situ observed by Lorentz transmission electron microscopy (LTEM. The demagnetization process of hot-deformed sample is dominated by domain-wall pinning, while that of NdCu-diffused sample is mainly the magnetization reversal of single grains or grain aggregations. This firstly observed result gives an explicit evidence to understand the coercivity mechanism of magnetically segregated magnet. The effect of magnetic field of TEM on decrease in domain wall energy was theoretically analyzed, which helps to understand the in-situ observation process of magnetic materials.

Comparison of in situ polymerization and solution-dispersion techniques in the preparation of Polyimide/Montmorillonite (MMT) Nanocomposites.

Science.gov (United States)

Ahmad, Mansor Bin; Gharayebi, Yadollah; Salit, Mohd Sapuan; Hussein, Mohd Zobir; Shameli, Kamyar

2011-01-01

In this paper, Polyimide/Montmorillonite Nanocomposites (PI/MMT NCs), based on aromatic diamine (4-Aminophenyl sulfone) (APS) and aromatic dianhydride (3,3',4,4'-benzophenonetetracarboxylic dianhydride) (BTDA) were prepared using in situ polymerization and solution-dispersion techniques. The prepared PI/MMT NCs films were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM) and thermogravimetric analysis (TGA). The XRD results showed that at the content of 1.0 wt % Organo Montmorillonite (OMMT) for two techniques and 3.0 wt % OMMT for the in situ polymerization technique, the OMMT was well-intercalated, exfoliated and dispersed into polyimide matrix. The OMMT agglomerated when its amount exceeded 10 wt % and 3.0 wt % for solution-dispersion and in situ polymerization techniques respectively. These results were confirmed by the TEM images of the prepared PI/MMT NCs. The TGA thermograms indicated that thermal stability of prepared PI/MMT NCs were increased with the increase of loading that, the effect is higher for the samples prepared by in situ polymerization technique.

Early Winter Sea Ice Dynamics in the Ross Sea from In Situ and Satellite Observations

Science.gov (United States)

Maksym, T.; Ackley, S. F.; Stammerjohn, S. E.; Tison, J. L.; Hoeppner, K.

2017-12-01

The Ross Sea sea ice cover is one of the few regions of the cryosphere that have been expanding in recent decades. However, 2017 saw a significantly delayed autumn ice advance and record low early winter sea ice extent. Understanding the causes and impacts of this variability has been hampered by a lack of in situ observations. A winter cruise into the Ross Sea in April-June 2017 provided some of the only in situ winter observations of sea ice processes in this region in almost 20 years. We present a first look at data from arrays of drifting buoys deployed in the ice pack and outflow from these polynyas, supplemented by a suite of high-resolution synthetic aperture radar (SAR) data. Additional observations included high-resolution sonar imagery of ice deformation features from an autonomous underwater vehicle, shipboard visual observations of sea ice properties, and in situ measurements of snow and thickness and structural properties. These data show that the delay in ice advance led to a thin, highly dynamic sea ice pack, with substantial ice production and export from the Ross Ice Shelf and Terra Nova Bay polynyas. Despite these high rates of ice production, the pack ice remained thin due to rapid export and northward drift. Compared to the only prior winter observations made in 1995 and 1998, the ice was thinner, with less ridging and snow cover, reflecting a younger ice cover. Granular ice was less prevalent than in these prior cruises, particularly in the outer pack, likely due to less snow ice formation and less pancake ice formation at the advancing ice edge. Despite rapid basal ice growth, the buoy data suggest that deformation may be the dominant mechanism for sea ice thickening in the pack once an initial ice cover forms.

In situ Microscopic Observation of Sodium Deposition/Dissolution on Sodium Electrode

OpenAIRE

Yuhki Yui; Masahiko Hayashi; Jiro Nakamura

2016-01-01

Electrochemical sodium deposition/dissolution behaviors in propylene carbonate-based electrolyte solution were observed by means of in situ light microscopy. First, granular sodium was deposited at pits in a sodium electrode in the cathodic process. Then, the sodium particles grew linearly from the electrode surface, becoming needle-like in shape. In the subsequent anodic process, the sodium dissolved near the base of the needles on the sodium electrode and the so-called ?dead sodium? broke a...

In-situ observation system for dual ion irradiation damage

International Nuclear Information System (INIS)

Furuno, Shigemi; Hojou, Kiichi; Otsu, Hitoshi; Sasaki, T.A.; Izui, Kazuhiko; Tukamoto, Tetsuo; Hata, Takao.

1992-01-01

We have developed an in-situ observation and analysis system during dual ion beam irradiation in an electron microscope. This system consists of an analytical electron microscope of JEM-4000FX type equipped with a parallel EELS and an EDS attachments and linked with two sets of ion accelerators of 40 kV. Hydrogen and helium dual-ion beam irradiation experiments were performed for SiC crystals. The result of dual-ion beam irradiation was compared with those of helium and hydrogen single ion irradiations. It is clearly seen that the dual-ion irradiation has the effect of suppressing bubble formation and growth in comparison with the case of single helium ion irradiation. (author)

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

Low-temperature thermal reduction of graphene oxide: In situ correlative structural, thermal desorption, and electrical transport measurements

Science.gov (United States)

Lipatov, Alexey; Guinel, Maxime J.-F.; Muratov, Dmitry S.; Vanyushin, Vladislav O.; Wilson, Peter M.; Kolmakov, Andrei; Sinitskii, Alexander

2018-01-01

Elucidation of the structural transformations in graphene oxide (GO) upon reduction remains an active and important area of research. We report the results of in situ heating experiments, during which electrical, mass spectrometry, X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, and transmission electron microscopy (TEM) measurements were carried out correlatively. The simultaneous electrical and temperature programmed desorption measurements allowed us to correlate the onset of the increase in the electrical conductivity of GO by five orders of magnitude at about 150 °C with the maxima of the rates of desorption of H2O, CO, and CO2. Interestingly, this large conductivity change happens at an intermediate level of the reduction of GO, which likely corresponds to the point when the graphitic domains become large enough to enable percolative electronic transport. We demonstrate that the gas desorption is intimately related to (i) the changes in the chemical structure of GO detected by XPS and Raman spectroscopy and (ii) the formation of nanoscopic holes in GO sheets revealed by TEM. These in situ observations provide a better understanding of the mechanism of the GO thermal reduction.

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

International Nuclear Information System (INIS)

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

2012-01-01

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

In-situ observations of nucleation in Al-0.1Mg

DEFF Research Database (Denmark)

Wu, G.L.; Ubhi, H.S.; Petrenec, M.

2015-01-01

A tensile sample of an Al-0.1Mg alloy was in-situ tested in a SEM followed by in-situ annealing to develop recrystallizing nuclei/grains. The evolution of microstructure and crystallographic orientations were characterized using the EBSD technique. Changes in the same area within the sample durin...

In situ observation of shear-driven amorphization in silicon crystals

Energy Technology Data Exchange (ETDEWEB)

He, Yang; Zhong, Li; Fan, Feifei; Wang, Chongmin; Zhu, Ting; Mao, Scott X.

2016-09-19

Amorphous materials have attracted great interest in the scientific and technological fields. An amorphous solid usually forms under the externally driven conditions of melt-quenching, irradiation and severe mechanical deformation. However, its dynamic formation process remains elusive. Here we report the in situ atomic-scale observation of dynamic amorphization processes during mechanical straining of nanoscale silicon crystals by high resolution transmission electron microscopy (HRTEM). We observe the shear-driven amorphization (SDA) occurring in a dominant shear band. The SDA involves a sequence of processes starting with the shear-induced diamond-cubic to diamond-hexagonal phase transition that is followed by dislocation nucleation and accumulation in the newly formed phase, leading to the formation of amorphous silicon. The SDA formation through diamond-hexagonal phase is rationalized by its structural conformity with the order in the paracrystalline amorphous silicon, which maybe widely applied to diamond-cubic materials. Besides, the activation of SDA is orientation-dependent through the competition between full dislocation nucleation and partial gliding.

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.

HVEM in-situ observation of formation of helical dislocations in Ag-10at.%Al

International Nuclear Information System (INIS)

Saka, H.; Kondo, T.

1982-01-01

Dissociated near-screw dislocations in Ag-10at.%Al were irradiated with 1 MeV electrons at 473K in a HVEM and the transformation of the dissociated screws into helices as a result of the interaction of point defects introduced was observed in situ using the 'weak-beam' electron microscopy. Results of observations have been analysed in terms of the 'loop-jog' model of climb of dissociated dislocations proposed by Cherns, Hirsch and Saka. (author)

Do In Situ Observations Contain Signatures of Intermittent Fast Solar Wind Acceleration?

Science.gov (United States)

Matteini, L.; Horbury, T. S.; Stansby, D.

2017-12-01

Disentangling local plasma properties and Solar origin structures in in situ data is a crucial aspect for the understanding of solar wind acceleration and evolution. This is particularly challenging at 1 AU and beyond, where structures of various origin have had time to interact and merge, smoothing out their main characteristics. Observations of more pristine plasma closer to the Sun are therefore needed. In preparation of the forthcoming Solar Orbiter and Parker Solar Probe missions, Helios observations as close as to 0.3 AU - although old, not yet fully exploited - can be used to test our expectations and make new predictions. Recent observations (Matteini et al. 2014, 2015) have outlined the presence of intense (up to 1000km/s) and short-living velocity peaks that ubiquitously characterize the typical profile of the fast solar wind at 0.3 AU, suggesting that these features could be remnants of processes occurring in the Solar atmosphere and a signature of intermittent solar wind acceleration from coronal holes. We discuss results about statistics of these events, characterizing their physical properties and trying to link them with typical Solar temporal and spatial scales. Finally we also discuss how these velocity peaks will likely affect the future in situ exploration of the inner heliosphere by Solar Orbiter and the Parker Solar Probe.

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

Energy Technology Data Exchange (ETDEWEB)

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

1997-05-27

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

Real-Time Observation of Platinum Redispersion on Ceria-Based Oxide by In-situ Turbo-XAS in Fluorescence Mode

International Nuclear Information System (INIS)

Nagai, Yasutaka; Dohmae, Kazuhiko; Tanabe, Toshitaka; Shinjoh, Hirofumi; Takagi, Nobuyuki; Ikeda, Yasuo; Guilera, Gemma; Pascarelli, Sakura; Newton, Mark; Matsumoto, Shin'ichi

2007-01-01

A real-time observation of the redispersion behavior of sintered Pt on ceria-based oxide was made possible by in-situ time-resolved Turbo-XAS in fluorescence mode. 2 wt% Pt/Ce-Zr-Y mixed oxide samples were prepared, and then treated under an aging condition. The average Pt particle size measured by CO absorption method after aging was 7 nm. Redispersion treatments of the previously aged catalyst were carried out at 600 deg. C within an in-situ XAS cell in a cyclical flow of reducing/oxidizing gases. Pt L3-edge XANES spectra were collected every 1.1 second under in-situ conditions. From a change in the XANES spectra, we observed that the Pt particle size of the aged catalyst decreased from 7 to 5 nm after 60 seconds and then to 3 nm after 1000 seconds

Improving magnetosphere in situ observations using solar sails

Science.gov (United States)

Parsay, Khashayar; Schaub, Hanspeter; Schiff, Conrad; Williams, Trevor

2018-01-01

Past and current magnetosphere missions employ conventional spacecraft formations for in situ observations of the geomagnetic tail. Conventional spacecraft flying in inertially fixed Keplerian orbits are only aligned with the geomagnetic tail once per year, since the geomagnetic tail is always aligned with the Earth-Sun line, and therefore, rotates annually. Solar sails are able to artificially create sun-synchronous orbits such that the orbit apse line remains aligned with the geomagnetic tail line throughout the entire year. This continuous presence in the geomagnetic tail can significantly increase the science phase for magnetosphere missions. In this paper, the problem of solar sail formation design is explored using nonlinear programming to design optimal two-craft, triangle, and tetrahedron solar sail formations, in terms of formation quality and formation stability. The designed formations are directly compared to the formations used in NASA's Magnetospheric Multi-Scale mission.

Fabrication of in-situ grown graphene reinforced Cu matrix composites

Science.gov (United States)

Chen, Yakun; Zhang, Xiang; Liu, Enzuo; He, Chunnian; Shi, Chunsheng; Li, Jiajun; Nash, Philip; Zhao, Naiqin

2016-01-01

Graphene/Cu composites were fabricated through a graphene in-situ grown approach, which involved ball-milling of Cu powders with PMMA as solid carbon source, in-situ growth of graphene on flaky Cu powders and vacuum hot-press sintering. SEM and TEM characterization results indicated that graphene in-situ grown on Cu powders guaranteed a homogeneous dispersion and a good combination between graphene and Cu matrix, as well as the intact structure of graphene, which was beneficial to its strengthening effect. The yield strength of 244 MPa and tensile strength of 274 MPa were achieved in the composite with 0.95 wt.% graphene, which were separately 177% and 27.4% enhancement over pure Cu. Strengthening effect of in-situ grown graphene in the matrix was contributed to load transfer and dislocation strengthening. PMID:26763313

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

International Nuclear Information System (INIS)

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

2012-01-01

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

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.

Deteriorating water clarity in shallow waters: Evidence from long term MODIS and in-situ observations

Science.gov (United States)

Shi, Kun; Zhang, Yunlin; Zhu, Guangwei; Qin, Boqiang; Pan, Delu

2018-06-01

Water clarity (Secchi disk depth: SDD), as a proxy of water transparency, provides important information on the light availability to the water or lake ecosystem. Shallow lakes have been experienced dramatic environmental and climatic change. This study demonstrated using combination of long-term MODIS and in-situ measurements to track the dynamics of SDD with these environmental and climate changes in shallow water environments. We selected a typical turbid shallow Lake Taihu as our case study. Based on MODIS-Aqua data, an empirical model for estimating SDD was developed and validated. Subsequently, we employed the proposed model to derive the spatial and temporal SDD distribution patterns of Lake Taihu from 2003 to 2015. Combining MODIS-derived SDD time series of 2003-2015 and long-term in-situ SDD observations dated back to 1993, we elucidated SDD long-term variation trends and driving mechanism. Deteriorating water clarity from the long-term SDD observations indicated that Lake Taihu became more and more turbid and water quality was decreasing. Increasing in cyanobacterial bloom area, as a result of decreasing in wind speed and eutrophication, may partially be responsible for the decreasing trend. A predicted future decrease in the wind speed in Lake Taihu region could enhance the formation of cyanobacterial blooms and consequently lead to a further decrease in water clarity. This study suggested that coupling remote sensing monitoring and long-term in-situ observations could provide robust evidence and new insights to elucidate long-term dynamics in aquatic ecosystem evolution.

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...

Identification of proangiogenic TIE2-expressing monocytes (TEMs) in human peripheral blood and cancer.

Science.gov (United States)

Venneri, Mary Anna; De Palma, Michele; Ponzoni, Maurilio; Pucci, Ferdinando; Scielzo, Cristina; Zonari, Erika; Mazzieri, Roberta; Doglioni, Claudio; Naldini, Luigi

2007-06-15

Tumor-infiltrating myeloid cells, including tumor-associated macrophages (TAMs), have been implicated in tumor progression. We recently described a lineage of mouse monocytes characterized by expression of the Tie2 angiopoietin receptor and required for the vascularization and growth of several tumor models. Here, we report that TIE2 expression in human blood identifies a subset of monocytes distinct from classical inflammatory monocytes and comprised within the less abundant "resident" population. These TIE2-expressing monocytes (TEMs) accounted for 2% to 7% of blood mononuclear cells in healthy donors and were distinct from rare circulating endothelial cells and progenitors. In human cancer patients, TEMs were observed in the blood and, intriguingly, within the tumors, where they represented the main monocyte population distinct from TAMs. Conversely, TEMs were hardly detected in nonneoplastic tissues. In vitro, TEMs migrated toward angiopoietin-2, a TIE2 ligand released by activated endothelial cells and angiogenic vessels, suggesting a homing mechanism for TEMs to tumors. Purified human TEMs, but not TEM-depleted monocytes, markedly promoted angiogenesis in xenotransplanted human tumors, suggesting a potentially critical role of TEMs in human cancer progression. Human TEMs may provide a novel, biologically relevant marker of angiogenesis and represent a previously unrecognized target of cancer therapy.

Preparation and observation of an artifact-free Ge2Sb2Te5 TEM specimen by the small angle cleavage technique

International Nuclear Information System (INIS)

Kim, M.S.; Kim, H.G.

2006-01-01

The amorphous Ge 2 Sb 2 Te 5 thin film for the application to the non-volatile memory device was prepared by the pulsed laser deposition on a SiO2/Si substrate. The amorphous Ge 2 Sb 2 Te 5 which has the T C around 150 deg. C is readily crystallized when exposed to a comparable heat such as the Ar beam irradiation during the conventional ion milling process. Retaining its amorphous initial phase is important in order to precisely observe and understand the crystallization behaviour whether it be the sample for a pure materialistic research or applied into the device. To avoid such deterioration of the film's amorphous nature, the complete mechanical TEM specimen preparation which is called the small angle cleavage technique (SACT) was adopted to show thermally undisturbed, an artifact-free amorphous Ge 2 Sb 2 Te 5 TEM specimen. The two distinctive amorphous and crystalline phases has been observed by the HRTEM study

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)

TEM1 expression in cancer-associated fibroblasts is correlated with a poor prognosis in patients with gastric cancer

International Nuclear Information System (INIS)

Fujii, Satoshi; Fujihara, Ayano; Natori, Kei; Abe, Anna; Kuboki, Yasutoshi; Higuchi, Youichi; Aizawa, Masaki; Kuwata, Takeshi; Kinoshita, Takahiro; Yasui, Wataru; Ochiai, Atsushi

2015-01-01

The cancer stroma, including cancer-associated fibroblasts (CAFs), is known to contribute to cancer cell progression and metastasis, suggesting that functional proteins expressed specifically in CAFs might be candidate molecular targets for cancer treatment. The purpose of the present study was to explore the possibility of using TEM1 (tumor endothelial marker 1), which is known to be expressed in several types of mesenchymal cells, as a molecular target by examining the impact of TEM1 expression on clinicopathological factors in gastric cancer patients. A total of 945 consecutive patients with gastric cancer who underwent surgery at the National Cancer Center Hospital East between January 2003 and July 2007 were examined using a tissue microarray approach. TEM1 expression in CAFs or vessel-associated cells was determined using immunohistochemical staining. Three items (CAF-TEM1-positivity, CAF-TEM1-intensity, and vessel-TEM1-intensity) were then examined to determine the correlations between the TEM1 expression status and the recurrence-free survival (RFS), overall survival (OS), cancer-related survival (COS), and other clinicopathological factors. Significant correlations between CAF-TEM1-positivity or CAF-TEM1-intensity and RFS, OS, or COS were observed (P < 0.001, Kaplan–Meier curves); however, no significant correlation between vessel-TEM1-intensity and RFS, OS, or COS was observed. A univariate analysis showed that CAF-TEM1-positivity and CAF-TEM1-intensity were each correlated with a scirrhous subtype, tumor depth, nodal status, distant metastasis, serosal invasion, lymphatic or venous vessel infiltrations, and pTMN stage. This study suggests that the inhibition of TEM1 expression specifically in the CAFs of gastric carcinoma might represent a new strategy for the treatment of gastric cancer

In Situ Observation of the Dislocation Structure Evolution During a Strain Path Change in Copper

DEFF Research Database (Denmark)

Wejdemann, Christian; Poulsen, Henning Friis; Lienert, Ulrich

2013-01-01

The evolution of deformation structures in individual grains embedded in polycrystalline copper specimens during strain path changes is observed in situ by high-resolution reciprocal space mapping with high-energy synchrotron radiation. A large number of individual subgrains is resolved; their be......The evolution of deformation structures in individual grains embedded in polycrystalline copper specimens during strain path changes is observed in situ by high-resolution reciprocal space mapping with high-energy synchrotron radiation. A large number of individual subgrains is resolved...... and orientation of the resolved subgrains change only slightly, while their elastic stresses are significantly altered. This indicates the existence of a microplastic regime during which only the subgrains deform plastically and no yielding of the dislocation walls occurs. After reloading above 0.3% strain......, the elastic stresses of individual subgrains are about the same as in unidirectionally deformed reference specimens. They increase only slightly during further straining—accompanied by occasional emergence of new subgrains, abundant orientation changes, and disappearance of existing subgrains....

In situ study of heavy ion induced radiation damage in NF616 (P92) alloy

International Nuclear Information System (INIS)

Topbasi, Cem; Motta, Arthur T.; Kirk, Mark A.

2012-01-01

Highlights: ► The ferritic–martensitic alloy NF616 was irradiated in situ with 1 MeV Kr ions at 50 K and 473 K. ► The defect cluster density increases with dose and saturates at ∼6 dpa at 50 K and 473 K. ► The defect size distributions do not change with dose at this temperature range. ► Results indicate that defect cluster formation and destruction is governed by cascade impact. - Abstract: NF616 is a nominal 9Cr ferritic–martensitic steel that is amongst the primary candidates for cladding and duct applications in the Sodium-Cooled Fast Reactor, one of the Generation IV nuclear energy systems. In this study, an in situ investigation of the microstructure evolution in NF616 under heavy ion irradiation has been conducted. NF616 was irradiated to 8.4 dpa at 50 K and to 7.6 dpa at 473 K with 1 MeV Kr ions. Nano-sized defects first appeared as white dots in dark-field TEM images and their areal density increased until saturation (∼6 dpa). Dynamic observations at 50 K and 473 K showed appearance and disappearance of TEM-visible defect clusters under irradiation that continued above saturation dose. Quantitative analysis showed no significant change in the average size (∼3–4 nm) and distribution of defect clusters with increasing dose at 50 K and 473 K. These results indicate a cascade-driven process of microstructure evolution under irradiation in these alloys that involves both the formation of TEM-visible defect clusters by various degrees of cascade overlap and cascade induced defect cluster elimination. According to this mechanism, saturation of defect cluster density is reached when the rate of defect cluster formation by overlap is equal to the rate of cluster elimination during irradiation.

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

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.

Study of InGaN/GaN quantum dot systems by TEM techniques and photoluminescence spectroscopy

International Nuclear Information System (INIS)

Kashtiban, R J; Bangert, U; Harvey, A J; Sherliker, B; Halsall, M P

2010-01-01

InGaN/GaN multilayer quantum dot structures produced by MOCVD techniques on c-plane sapphire were studied by transmission electron microscopy (TEM) and photoluminescence (PL) techniques. Indium fluctuations ranging from 1-4 nm were observed with both energy filtered TEM (EFTEM) and high angle annular dark field (HAADF) scanning TEM. The existence of V-shaped defects with nucleation centres at the termination of threading dislocation were observed in HAADF images. There was also evidence of the formation of large quantum dots at low densities from lattice HRTEM images. This was further confirmed by PL measurements through the observation of a single sharp line at low power with the typical saturation behaviour at higher power excitation.

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

In situ observation of structural change of nanostructured tungsten during annealing

International Nuclear Information System (INIS)

Yajima, Miyuki; Yoshida, Naoaki; Kajita, Shin; Tokitani, Masayuki; Baba, Tomotsugu; Ohno, Noriyasu

2014-01-01

Deformation of fiberform nanostructure and the dynamic behavior of helium (He) bubbles in fuzz tungsten (W) during annealing have been investigated by means of in situ cross-section observation using transmission electron microscopy and He desorption rate observation using thermal desorption spectroscopy (TDS). Thermal recovery of the nanostructure, such as shrinkage and coalescence of fine structure, annihilation of He bubbles, and large desorption of He gas, occurred around 1073–1173 K. The activation energy of He was estimated from a TDS peak that appeared around 300–400 K by using the Kissinger–Akahira–Sunose model-free-kinetics method. In addition, the TDS results of fiberform nanostructured tungsten were compared with those of tungsten samples irradiated with a high-energy He ion beam

In situ observation techniques of protective oxide layer

International Nuclear Information System (INIS)

Doi, Takashi; Adachi, Takeharu; Usuki, Noriaki

2015-01-01

In situ analyzing techniques for investigating a surface and interface change during corrosion and oxidation of metals by using Raman scattering spectroscopy (Raman), X-ray diffraction (XRD) and X-ray photoemission spectroscopy (XPS) are present. The Raman spectra revealed that a crystal structure and distribution of corrosion products varied during corrosion progress at elevated temperature and high pressure electrolyte. Time dependent XRD measurements made clear the behavior of the electrochemical reduction of a rust and the iso thermal transformation of a scale on a steel. It was demonstrated that XPS was capable of the in-situ measurements for initial stage of high temperature oxidation. (author)

Complete Tem-Tomography: 3D Structure of Gems Cluster

Science.gov (United States)

Matsuno, J.; Miyake, A.; Tsuchiyama, A.; Messenger, S.; Nakamura-Messenger, K.

2015-01-01

GEMS (glass with embedded metal and sulfide) grains in interplanetary dust particles (IDPs) are considered to be one of the ubiquitous and fundamental building blocks of solids in the Solar System. They have been considered to be interstellar silicate dust that survived various metamorphism or alteration processes in the protoplanetary disk but the elemental and isotopic composition measurements suggest that most of them have been formed in the protoplanetary disk as condensates from high temperature gas. This formation model is also supported by the formation of GEMS-like grains with respect to the size, mineral assemblage, texture and infrared spectrum by condensation experiments from mean GEMS composition materials. Previous GEMS studies were performed only with 2D observation by transmission electron microscopy (TEM) or scanning TEM (STEM). However, the 3D shape and structure of GEMS grains and the spatial distribution of Fe/FeS's has critical information about their formation and origin. Recently, the 3D structure of GEMS grains in ultrathin sections of cluster IDPs was revealed by electron tomography using a TEM/STEM (JEM-2100F, JEOL). However, CT images of thin sections mounted on Cu grids acquired by conventional TEM-tomography are limited to low tilt angles (e. g., less than absolute value of 75 deg. In fact, previous 3D TEM observations of GEMS were affected by some artifacts related to the limited tilt range in the TEM used. Complete tomographic images should be acquired by rotating the sample tilt angle over a range of more than absolute value of 80 deg otherwise the CT images lose their correct structures. In order to constrain the origin and formation process of GEMS grains more clearly, we performed complete electron tomography for GEMS grains. Here we report the sample preparation method we have developed for this study, and the preliminary results.

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.

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

Energy Technology Data Exchange (ETDEWEB)

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

2008-06-15

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

PREDICTION OF GEOMAGNETIC STORM STRENGTH FROM INNER HELIOSPHERIC IN SITU OBSERVATIONS

Energy Technology Data Exchange (ETDEWEB)

Kubicka, M.; Möstl, C.; Amerstorfer, T.; Boakes, P. D.; Törmänen, O. [Space Research Institute, Austrian Academy of Sciences, 8042 Graz (Austria); Feng, L. [Purple Mountain Observatory, Chinese Academy of Sciences, West Beijing Road 2 Nanjing, 210008 (China); Eastwood, J. P., E-mail: christian.moestl@oeaw.ac.at [Space and Atmospheric Physics, The Blackett Laboratory, Imperial College London, London SW7 2AZ (United Kingdom)

2016-12-20

Prediction of the effects of coronal mass ejections (CMEs) on Earth strongly depends on knowledge of the interplanetary magnetic field southward component, B{sub z}. Predicting the strength and duration of B{sub z} inside a CME with sufficient accuracy is currently impossible, forming the so-called B{sub z} problem. Here, we provide a proof-of-concept of a new method for predicting the CME arrival time, speed, B{sub z}, and resulting disturbance storm time ( Dst ) index on Earth based only on magnetic field data, measured in situ in the inner heliosphere (<1 au). On 2012 June 12–16, three approximately Earthward-directed and interacting CMEs were observed by the Solar Terrestrial Relations Observatory imagers and Venus Express (VEX) in situ at 0.72 au, 6° away from the Sun–Earth line. The CME kinematics are calculated using the drag-based and WSA–Enlil models, constrained by the arrival time at VEX , resulting in the CME arrival time and speed on Earth. The CME magnetic field strength is scaled with a power law from VEX to Wind . Our investigation shows promising results for the Dst forecast (predicted: −96 and −114 nT (from 2 Dst models); observed: −71 nT), for the arrival speed (predicted: 531 ± 23 km s{sup −1}; observed: 488 ± 30 km s{sup −1}), and for the timing (6 ± 1 hr after the actual arrival time). The prediction lead time is 21 hr. The method may be applied to vector magnetic field data from a spacecraft at an artificial Lagrange point between the Sun and Earth or to data taken by any spacecraft temporarily crossing the Sun–Earth line.

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

Directory of Open Access Journals (Sweden)

Mark H Rummeli

2018-05-01

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

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...

Interpretation of interfacial structures in X-ray multilayers by TEM Fresnel fringe effects

OpenAIRE

Nguyen, Tai D.; O'Keefe, Michael A.; Kilaas, Roar; Gronsky, Ronald; Kortright, Jeffrey B.

1991-01-01

Assessment of interfacial structures from high-resolution TEM images of cross-sectional specimens is difficult due to Fresnel fringe effects producing different apparent structures in the images. The effects of these fringes have been commonly over-looked in efforts of making quantitative interpretation of interfacial profiles. In this report, we present the observations of the Fresnel fringes in nanometer period Mo/Si, W/C, and WC/C multilayers in through-focus-series TEM images. Calculation...

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

DEFF Research Database (Denmark)

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

2014-01-01

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

Synthesis and characterization of PMMA/clay nanocomposites prepared by in situ polymerization assisted by sonication; Sintese e caracterizacao de nanocompositos de PMMA/MMTO via polimerizacao in situ assistida por ultrassom

Energy Technology Data Exchange (ETDEWEB)

Prado, Bruna R.; Bartoli, Julio R., E-mail: bartoli@unicamp.br [Universidade Estadual de Campinas (UNICAMP), Campinas, SP (Brazil); Ito, Edson N. [Universidade Federal do Rio Grande do Norte (UFRN), Natal, RN (Brazil)

2015-07-01

In this work is presented the synthesis of nanocomposites of poly(methyl methacrylate), PMMA, with organically montmorillonite (OMMT) modified clays by in situ polymerization assisted by sonication. A statistically designed experiment was used, central composing design (CCD), to study the effect of synthesis variables on the dispersion of nanoparticles in PMMA matrix. The processing and formulation factors studied were: energy of sonication and Flory-Huggins interaction parameter between PMMA and organoclay. The structural (XRD) and morphological (TEM) characterizations of the PMMA/OMMT nanocomposites are compared with the literature. It was observed significant exfoliation of OMMT modified with hydroxyl groups in the nanocomposites of PMMA, mainly at the low ultrasonic energy level (90 and 105 kJ) studied. (author)

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.

A century of ocean warming on Florida Keys coral reefs: historic in situ observations

Science.gov (United States)

Kuffner, Ilsa B.; Lidz, Barbara H.; Hudson, J. Harold; Anderson, Jeffery S.

2015-01-01

There is strong evidence that global climate change over the last several decades has caused shifts in species distributions, species extinctions, and alterations in the functioning of ecosystems. However, because of high variability on short (i.e., diurnal, seasonal, and annual) timescales as well as the recency of a comprehensive instrumental record, it is difficult to detect or provide evidence for long-term, site-specific trends in ocean temperature. Here we analyze five in situ datasets from Florida Keys coral reef habitats, including historic measurements taken by lighthouse keepers, to provide three independent lines of evidence supporting approximately 0.8 °C of warming in sea surface temperature (SST) over the last century. Results indicate that the warming observed in the records between 1878 and 2012 can be fully accounted for by the warming observed in recent decades (from 1975 to 2007), documented using in situ thermographs on a mid-shore patch reef. The magnitude of warming revealed here is similar to that found in other SST datasets from the region and to that observed in global mean surface temperature. The geologic context and significance of recent ocean warming to coral growth and population dynamics are discussed, as is the future prognosis for the Florida reef tract.

TEM specimen preparation of semiconductor-PMMA-metal interfaces

International Nuclear Information System (INIS)

Thangadurai, P.; Lumelsky, Yulia; Silverstein, Michael S.; Kaplan, Wayne D.

2008-01-01

Transmission electron microscopy (TEM) cross-section specimens of PMMA in contact with gold and Si were prepared by focused ion beam (FIB) and compared with plan-view PMMA specimens prepared by a dip-coating technique. The specimens were characterized by TEM and electron energy loss spectroscopy (EELS). In the cross-section specimens, the thin films of PMMA were located in a Si-PMMA-Au multilayer. Different thicknesses of PMMA films were spin-coated on the Si substrates. The thickness of the TEM specimens prepared by FIB was estimated using EELS to be 0.65 of the plasmon mean-free-path. Along the PMMA-Au interface, Au particle diffusion into the PMMA was observed, and the size of the Au particles was in the range of 2-4 nm. Dip-coating of PMMA directly on Cu TEM grids resulted in thin specimens with a granular morphology, with a thickness of 0.58 of the plasmon mean-free-path. The dip-coated specimens were free from ion milling induced artifacts, and thus serve as control specimens for comparison with the cross-sectioned specimens prepared by FIB

First in-situ observations of exospheric response to CME impact at Mercury

Science.gov (United States)

Raines, J. M.; Wallace, K. L.; Sarantos, M.; Jasinski, J. M.; Tracy, P.; Dewey, R. M.; Weberg, M. J.; Slavin, J. A.

2017-12-01

We present the first in-situ observations of enhancements to Mercury's He exosphere generated by CME impact. We analyzed both plasma and magnetic field measurements from the Mercury Surface Space Environment, Geochemistry and Mapping (MESSENGER) spacecraft over a 60-hour period as a coronal mass ejection (CME) passed by the planet. We identified the shock, magnetic cloud and cavity regions of the moderate intensity CME while MESSENGER was in the solar wind. Inside the magnetosphere just after the CME shock passage, we observed a very active dayside magnetosphere, as evident from the high flux plasma parcels passing through the dayside and a broad northern magnetospheric cusp with exceptionally high planetary ion content. All of these signatures indicate substantial reconnection at the dayside magnetopause, making conditions that were excellent for solar wind access to Mercury's surface. The CME appeared to have been particularly enriched in He2+, causing the observed density of solar wind He2+ in the cusp to rise above 0.1 cm-3 and putting it in the top 1% of the over 3200 cusps analyzed. As the low-density CME cavity passed over the planet on the next orbit, the magnetosphere appeared much quieter, with smoother magnetic fields and a smaller, less intense northern cusp but with greatly enhanced He+ content. The elevated He+ observed density continued to increase on subsequent cusp crossings, peaking at 0.1 cm-3 36 hours after CME impact, the highest observed throughout the entire MESSENGER mission. We suggest that the enhancement in He+ indicates an increase to the neutral He exosphere density from the He-enriched CME, a phenomenon observed at the moon, possibly acting as follows: Increased access to the surface from CME-enhanced reconnection, combined with high He2+ flux, enhanced surface implantation. Neutral He atoms were then liberated at an increased rate by surface processes supplying the exosphere, causing a gradual increase in He exosphere density. This

Local stress modification during in situ transmission electron microscopy straining experiments

Czech Academy of Sciences Publication Activity Database

Zárubová, Niva; Gemperle, Antonín; Gemperlová, Juliana

2007-01-01

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

In-Situ atomic force microscopic observation of ion beam bombarded plant cell envelopes

International Nuclear Information System (INIS)

Sangyuenyongpipat, S.; Yu, L.D.; Brown, I.G.; Seprom, C.; Vilaithong, T.

2007-01-01

A program in ion beam bioengineering has been established at Chiang Mai University (CMU), Thailand, and ion beam induced transfer of plasmid DNA molecules into bacterial cells (Escherichia coli) has been demonstrated. However, a good understanding of the fundamental physical processes involved is lacking. In parallel work, onion skin cells have been bombarded with Ar + ions at energy 25 keV and fluence1-2 x 10 15 ions/cm 2 , revealing the formation of microcrater-like structures on the cell wall that could serve as channels for the transfer of large macromolecules into the cell interior. An in-situ atomic force microscope (AFM) system has been designed and installed in the CMU bio-implantation facility as a tool for the observation of these microcraters during ion beam bombardment. Here we describe some of the features of the in-situ AFM and outline some of the related work

In situ observation of Ag-Cu-Ti liquid alloy/solid oxide interfaces

Energy Technology Data Exchange (ETDEWEB)

Durov, O.V. [Frantsevich Institute for Problems of Materials Science of NASU, 3 Krzhyzhanovsky Street, Kiev 142, 03680 (Ukraine)], E-mail: avdu@ukr.net; Krasovskyy, V.P. [Frantsevich Institute for Problems of Materials Science of NASU, 3 Krzhyzhanovsky Street, Kiev 142, 03680 (Ukraine)

2008-11-15

In situ investigation methods are a very interesting means for understanding high-temperature interface processes. A method of direct observation of the interactions between transparent materials (Al{sub 2}O{sub 3}, SiO{sub 2}, CaF{sub 2}) and metal melts was elaborated. For the Ag-36.65 at.%Cu-8.15 at.%Ti/sapphire system, the formation of a dark compound at the interface was observed to occur at high temperature. This result does not confirm the conclusion of a neutron spectroscopy study which indicated that titanium oxides form at the interface only during solidification of the alloy. Interactions of the same alloy with SiO{sub 2} and CaF{sub 2} were also considered.

Evaluation of surface layer flux parameterizations using in-situ observations

Science.gov (United States)

Katz, Jeremy; Zhu, Ping

2017-09-01

Appropriate calculation of surface turbulent fluxes between the atmosphere and the underlying ocean/land surface is one of the major challenges in geosciences. In practice, the surface turbulent fluxes are estimated from the mean surface meteorological variables based on the bulk transfer model combined with the Monnin-Obukhov Similarity (MOS) theory. Few studies have been done to examine the extent to which such a flux parameterization can be applied to different weather and surface conditions. A novel validation method is developed in this study to evaluate the surface flux parameterization using in-situ observations collected at a station off the coast of Gulf of Mexico. The main findings are: (a) the theoretical prediction that uses MOS theory does not match well with those directly computed from the observations. (b) The largest spread in exchange coefficients is shown in strong stable conditions with calm winds. (c) Large turbulent eddies, which depend strongly on the mean flow pattern and surface conditions, tend to break the constant flux assumption in the surface layer.

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.

In-situ observation of deuteride formation in palladium electrochemical cathode by X-ray diffraction method

International Nuclear Information System (INIS)

Yamamoto, Takao; Oka, Takashi; Taniguchi, Ryoichi

1990-01-01

In-situ X-ray diffraction observation of palladium foil cathode (10 μm) was carried out during electrolysis of 0.1N-LiOD heavy water solution in order to estimate the deuterium content in palladium during the detection of charged particles in our previous work. A complete transformation into β-palladium deuteride phase was observed, and its maximum lattice constant 4.06 A was evaluated as corresponding to D/Pd = 0.73. The deuterium concentration in the previous work was estimated as higher than this considering the difference in cell conditions. (author)

In-Situ Observation of Sintering Shrinkage of UO2 Compacts Derived from Different Powder Routes

International Nuclear Information System (INIS)

Rhee, Young Woo; Oh, Jang Soo; Kim, Dong Joo; Kim, Keon Sik; Kim, Jong Hun; Yang, Jae Ho; Koo, Yang Hyun

2015-01-01

In-situ observations on the shrinkage of green pellets with precisely controlled dimensions were carefully conducted by using TOM during H2 atmosphere sintering. The shrinkage retardation in IDR-UO 2 might be attributed to the larger primary particle size of IDRUO 2 than those of ADU- and AUC- UO 2 powders. It would be important to understand the different sintering characteristics of UO 2 powders according to the powder routes, when it comes to designing a new sintering process or choosing a sintering additive for new fuel pellet like PCI (Pellet Cladding Interaction) remedy pellet. In this paper, we have investigated the initial and intermediate sintering shrinkage of UO 2 from different powder routes by in-situ observation of green samples during H2 atmosphere sintering. Effect of powder characteristics of three different UO 2 powders on the initial and intermediate sintering were closely reviewed including crystal structure, powder size, specific surface area, primary crystal size, and O/U ratio

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.)

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.

Hysteresis in YHx films observed with in situ measurements

International Nuclear Information System (INIS)

Remhof, A.; Kerssemakers, J.W.J.; Molen, S.J. van der; Griessen, R.; Kooij, E.S.

2002-01-01

Giant hysteretic effects in the YH x hydrogen switchable mirror system are observed between x=1.9 and x=3 in pressure composition isotherms, optical and electrical properties, and mechanical stress. Polycrystalline Y films are studied by simultaneous in situ measurements of electrical resistivity, optical transmittance and x-ray diffractometry. These experiments are linked to optical microscopy of the samples. During hydrogen loading above x=1.9 the films stay in the metallic fcc phase until the optical transmittance reaches its minimum and the electrical resistance curve exhibits a characteristic feature at x=2.1. Upon further loading the system crosses the miscibility gap in which the fcc phase coexists with the hcp phase before hydrogen saturation is reached in the pure hcp phase. While the fcc phase stays at a concentration of x=2.1 in the coexistence region during loading, it remains at a concentration of x=1.9 during unloading. The hysteretic effects observed in optical transmission and electrical resistivity result from the different properties of the low concentration fcc phase YH 1.9 and the high concentration fcc phase YH 2.1 . They can be explained on the basis of the bulk phase diagram if the different stress states during loading and unloading are taken into account. These results contradict earlier interpretations of the hysteresis in thin film YH x , based on nonsimultaneous measurements of the optical and structural properties on different films

Long-Term Water Temperature Variations in Daya Bay, China Using Satellite and In Situ Observations

Directory of Open Access Journals (Sweden)

Jing Yu

2010-01-01

Full Text Available Daya Bay is a shallow, semi-en closed bay in the northern section of the South China Sea. The present study analyzed variations of water temperature in Daya Bay over the past 21 years (1985 - 2005 using Advanced Very High Resolution Radiometer (AVHRR satellite remote sensing data and in situ observations. Results showed that AVHRR readings of sea surface temperature (SST increased by 0.07°C y-1. Linear regression anal y sis for monthly SST anomalies (SSTA showed a shift from negative to positive from 1995 - 1996, when the Daya Bay nuclear power station commenced operations in 1994. The slope of linear regression analysis for SSTA nearly doubled from 0.05 (1985 - 1993 to 0.09 (1994 - 2005. Monthly AVHRR images showed a thermal plume from the power station and revealed the in crease of SST over 21 years. In situ observations in water temperature also showed an in creasing trend for the same period (1985 - 2005. Variations in water temperature in Daya Bay were connected with climatic perturbations and in creasing human activity including thermal discharge from nuclear power stations and the rapid economic development around the bay area.

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.

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

International Nuclear Information System (INIS)

Liu Hui; Yi Jianhong

2009-01-01

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

In-situ observation of irradiation quantities using a tethered balloon

Science.gov (United States)

Becker, Ralf; Gross, Steffen; Behrens, Klaus

2014-05-01

Irradiance is a key parameter in Earth's weather and climate system. Accurate observations of the components of the radiation budget are therefore essential to create reliable time series, to analyse spatial variability and to test, validate and adapt satellite-based algorithms. This holds true for near surface measurements as well as for in-situ observations in the lower troposphere. Such measurements are difficult to realise and therefore rarely performed. A tethered balloon system manufactured by Vailsala (9 cbm) is utilised as a carrier of a radiation budget sonde operating up to 1000 m above ground. Application is limited to fair weather conditions with maximum winds of 20 km/h and visibility greater than 3 km at ground level. The experimental setup is composed of a downward and upward looking pair of Kipp&Zonen CM11 (0.305-2.8 μm) and a corresponding pair of Kipp&Zonen CG4 (4.5 - 42 μm). Instruments are categorized as WMO 'secondary standard' according to ISO9660 and can be characterised as sufficiently robust and with acceptable response time for this purpose. Instrumentation is complemented by meteorological sensors (wind, temperature, humidity) flown on a dedicated suspension close (less than 50 m distance) to radiation sonde. In-situ measurements of irradiation in flowing and turbulent air are subjected to errors due to moving platform (roll/yaw/pitch). Potential deviations to near-surface measurements are discussed and an error estimate is given. Some comparisons of results of radiative transfer calculations for simple meteorological conditions have been made so far. It can be accomplished either by referring to profiles or by evaluating time series taken at elevated levels. Profiling lacks stationarity most time of a day due to high variability of shortwave downward and thus must be interpreted carefully. First results for longwave profiles as well as evaluation of time series obtained at distinct levels above ground show good correspondence.

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

Science.gov (United States)

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

2017-04-01

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

In-situ observation of damage evolution in TiC crystals during helium ion irradiation

International Nuclear Information System (INIS)

Hojou, K.; Otsu, H.; Furuno, S.; Izui, K.; Tsukamoto, T.

1994-01-01

In-situ observations were performed on bubble formation and growth in TiC during 20 keV helium ion irradiation over the wide range of irradiation temperatures from 12 to 1523 K. No amorphization occurred over this temperature range. The bubble densities and sizes were almost independent of irradiation temperatures from 12 to 1273 K. Remarkable growth and coalescence occurred during irradiation at high temperature above 1423 K and during annealing above 1373 K after irradiation. ((orig.))

Real time, in situ observation of the photocatalytic inactivation of Saccharomyces cerevisiae cells

Energy Technology Data Exchange (ETDEWEB)

Zhang, Jingtao [School of Food and Bioengineering, Zhengzhou University of Light Industry, Zhengzhou 450002 (China); Environment Functional Materials Division, Shenyang National Laboratory for Materials Science, Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016 (China); Wang, Xiaoxin [Environment Functional Materials Division, Shenyang National Laboratory for Materials Science, Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016 (China); Li, Qi, E-mail: qili@imr.ac.cn [Environment Functional Materials Division, Shenyang National Laboratory for Materials Science, Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016 (China); Shang, Jian Ku [Environment Functional Materials Division, Shenyang National Laboratory for Materials Science, Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016 (China); Department of Materials Science and Engineering, University of Illinois at Urbana-Champaign, Urbana, IL 61801 (United States)

2015-04-01

An in situ microscopy technique was developed to observe in real time the photocatalytic inactivation process of Saccharomyces cerevisiae (S. cerevisiae) cells by palladium-modified nitrogen-doped titanium oxide (TiON/PdO) under visible light illumination. The technique was based on building a photocatalytic micro-reactor on the sample stage of a fluorescence/phase contrast microscopy capable of simultaneously providing the optical excitation to activate the photocatalyst in the micro-reactor and the illumination to acquire phase contrast images of the cells undergoing the photocatalytic inactivation process. Using TiON/PdO as an example, the technique revealed for the first time the vacuolar activities inside S. cerevisiae cells subjected to a visible light photocatalytic inactivation. The vacuoles responded to the photocatalytic attack by the first expansion of the vacuolar volume and then contraction, before the vacuole disappeared and the cell structure collapsed. Consistent with the aggregate behavior observed from the cell culture experiments, the transition in the vacuolar volume provided clear evidence that photocatalytic disinfection of S. cerevisiae cells started with an initiation period in which cells struggled to offset the photocatalytic damage and moved rapidly after the photocatalytic damage overwhelmed the defense mechanisms of the cells against oxidative attack. - Highlights: • Palladium-modified nitrogen-doped titanium oxidephotocatalyst (TiON/PdO) • Effective visible-light photocatalytic disinfection of yeast cells by TiON/PdO • Real time, in situ observation technique was developed for photocatalytic disinfection. • The fluorescence/phase contrast microscope with a photocatalytic micro-reactor • Yeast cell disinfection happened before the cell structure collapsed.

Remote sensing, hydrological modeling and in situ observations in snow cover research: A review

Science.gov (United States)

Dong, Chunyu

2018-06-01

Snow is an important component of the hydrological cycle. As a major part of the cryosphere, snow cover also represents a valuable terrestrial water resource. In the context of climate change, the dynamics of snow cover play a crucial role in rebalancing the global energy and water budgets. Remote sensing, hydrological modeling and in situ observations are three techniques frequently utilized for snow cover investigations. However, the uncertainties caused by systematic errors, scale gaps, and complicated snow physics, among other factors, limit the usability of these three approaches in snow studies. In this paper, an overview of the advantages, limitations and recent progress of the three methods is presented, and more effective ways to estimate snow cover properties are evaluated. The possibility of improving remotely sensed snow information using ground-based observations is discussed. As a rapidly growing source of volunteered geographic information (VGI), web-based geotagged photos have great potential to provide ground truth data for remotely sensed products and hydrological models and thus contribute to procedures for cloud removal, correction, validation, forcing and assimilation. Finally, this review proposes a synergistic framework for the future of snow cover research. This framework highlights the cross-scale integration of in situ and remotely sensed snow measurements and the assimilation of improved remote sensing data into hydrological models.

In-situ observation of atomic self-organization processes in Xe nanocrystals embedded in Al

International Nuclear Information System (INIS)

Mitsuishi, K.; Song, M.; Furuya, K.; Birtcher, R. C.; Allen, C. W.; Donnelly, S. E.

1998-01-01

Self-organization processes in Xe nanocrystals embedded in Al are observed with in-situ high-resolution electron microscopy. Under electron irradiation, stacking fault type defects are produced in Xe nanocrystals. The defects recover in a layer by layer manner. Detailed analysis of the video reveals that the displacement of Xe atoms in the stacking fault was rather small for the Xe atoms at boundary between Xe and Al, suggesting the possibility of the stacking fault in Xe precipitate originating inside of precipitate, not at the Al/Xe interface

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

Science.gov (United States)

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

2014-12-01

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

In-situ observations of Eyjafjallajökull ash particles by hot-air balloon

Science.gov (United States)

Petäjä, T.; Laakso, L.; Grönholm, T.; Launiainen, S.; Evele-Peltoniemi, I.; Virkkula, A.; Leskinen, A.; Backman, J.; Manninen, H. E.; Sipilä, M.; Haapanala, S.; Hämeri, K.; Vanhala, E.; Tuomi, T.; Paatero, J.; Aurela, M.; Hakola, H.; Makkonen, U.; Hellén, H.; Hillamo, R.; Vira, J.; Prank, M.; Sofiev, M.; Siitari-Kauppi, M.; Laaksonen, A.; lehtinen, K. E. J.; Kulmala, M.; Viisanen, Y.; Kerminen, V.-M.

2012-03-01

The volcanic ash cloud from Eyjafjallajökull volcanic eruption seriously distracted aviation in Europe. Due to the flight ban, there were only few in-situ measurements of the properties and dispersion of the ash cloud. In this study we show in-situ observations onboard a hot air balloon conducted in Central Finland together with regional dispersion modelling with SILAM-model during the eruption. The modeled and measured mass concentrations were in a qualitative agreement but the exact elevation of the layer was slightly distorted. Some of this discrepancy can be attributed to the uncertainty in the initial emission height and strength. The observed maximum mass concentration varied between 12 and 18 μg m -3 assuming a density of 2 g m -3, whereas the gravimetric analysis of the integrated column showed a maximum of 45 μg m -3 during the first two descents through the ash plume. Ion chromatography data indicated that a large fraction of the mass was insoluble to water, which is in qualitative agreement with single particle X-ray analysis. A majority of the super-micron particles contained Si, Al, Fe, K, Na, Ca, Ti, S, Zn and Cr, which are indicative for basalt-type rock material. The number concentration profiles indicated that there was secondary production of particles possibly from volcano-emitted sulfur dioxide oxidized to sulfuric acid during the transport.

Preparation of TEM specimen by cross-section technique

International Nuclear Information System (INIS)

Hamada, Shozo

1986-01-01

Transmission electron microscopy (TEM) is applied to the direct observation of the depth dependent damage structure in ion-irradiated stainless steel by using the cross-section technique; obtaining the TEM specimen from a slice of the irradiated stainless steel with thick Ni plating. Here has been developed the specimen preparation method of cross-section technique without heat treatment, which was necessary in the conventional method to strengthen the bonding between Ni and stainless steel. Nickel plating with good bonding to stainless steel is enabled by the following manner. First, the irradiated stainless steel is immersed in the Wood's nickel solution at room temperature for 60s to activate the surface, followed by the stricking for 300s at a current density of 300 A/m 2 in the solution to make fine and homogeneous nucleation of Ni on the stainless steel. Then, the sample is plated with Ni in the Watt's nickel plating solution at 333 K with current density of 900 ∼ 1,000 A/m 2 . The TEM disc is obtained by mechanical slicing from the specimen with Ni plating of more than 3 mm thickness. Electropolishing is accomplished by using both Ballmann method and jet electropolishing to perforate the disc accurately at the aimed point for the observation of the damage structure. (author)

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.

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.

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