Designing MgFe2O4 decorated on green mediated reduced graphene oxide sheets showing photocatalytic performance and luminescence property

NASA Astrophysics Data System (ADS)

Shetty, Krushitha; Lokesh, S. V.; Rangappa, Dinesh; Nagaswarupa, H. P.; Nagabhushana, H.; Anantharaju, K. S.; Prashantha, S. C.; Vidya, Y. S.; Sharma, S. C.

2017-02-01

Here, a green route has been reported to convert Graphene Oxide (GO) to reduced graphene oxide (RGO) using clove extract. A modest and eco-accommodating sol-gel strategy has been employed to prepare MgFe2O4 nanoparticles, MgFe2O4-RGO nanocomposite samples. The samples were analyzed by Powder X-ray diffraction (PXRD), Fourier Transform Infrared Spectroscopy (FTIR), UV-Visible Spectroscopy, Scanning Electron Microcopy (SEM), Transmission Electron Microscopy (TEM), Photoluminescence (PL) and Electrochemical Impedance Spectroscopy (EIS). PXRD result revealed that the prepared samples were cubic spinel in nature. SEM results uncovered flake like surface morphology of the prepared nanomaterial. Better PL emission signature was observed when excited at 329 nm. PL studies demonstrated that the present samples were potential for the fabrication of white component of white light emitting diodes (WLEDs). Further, MgFe2O4-RGO nanocomposite showed enhanced photocatalytic movement (PCM) and photostability under Sunlight in the decomposition of Malachite Green (MG) compared to MgFe2O4. This can be attributed to the interaction of MgFe2O4 surface with RGO sheets which results in PL quenching, demonstrates that the recombination of photo-induced electrons and holes in MgFe2O4-RGO nanocomposite is more effectively inhibited. A possible mechanism for the enhanced properties of MgFe2O4-RGO nanocomposite was discussed. Moreover, MgFe2O4-RGO photocatalyst also showed easy magnetic separation with high reusability. These results unveil that the synthesized sample can be used in display applications and also as a potential photocatalyst.

Layer-by-layer assembly of graphene oxide on thermosensitive liposomes for photo-chemotherapy.

PubMed

Hashemi, Mohadeseh; Omidi, Meisam; Muralidharan, Bharadwaj; Tayebi, Lobat; Herpin, Matthew J; Mohagheghi, Mohammad Ali; Mohammadi, Javad; Smyth, Hugh D C; Milner, Thomas E

2018-01-01

Stimuli responsive polyelectrolyte nanoparticles have been developed for chemo-photothermal destruction of breast cancer cells. This novel system, called layer by layer Lipo-graph (LBL Lipo-graph), is composed of alternate layers of graphene oxide (GO) and graphene oxide conjugated poly (l-lysine) (GO-PLL) deposited on cationic liposomes encapsulating doxorubicin. Various concentrations of GO and GO-PLL were examined and the optimal LBL Lipo-graph was found to have a particle size of 267.9 ± 13 nm, zeta potential of +43.9 ± 6.9 mV and encapsulation efficiency of 86.4 ± 4.7%. The morphology of LBL Lipo-graph was examined by cryogenic-transmission electron microscopy (Cryo-TEM), atomic force microcopy (AFM) and scanning electron microscopy (SEM). The buildup of LBL Lipo-graph was confirmed via ultraviolet-visible (UV-Vis) spectrophotometry, thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) analysis. Infra-red (IR) response suggests that four layers are sufficient to induce a gel-to-liquid phase transition in response to near infra-red (NIR) laser irradiation. Light-matter interaction of LBL Lipo-graph was studied by calculating the absorption cross section in the frequency domain by utilizing Fourier analysis. Drug release assay indicates that the LBL Lipo-graph releases much faster in an acidic environment than a liposome control. A cytotoxicity assay was conducted to prove the efficacy of LBL Lipo-graph to destroy MD-MB-231 cells in response to NIR laser emission. Also, image stream flow cytometry and two photon microcopy provide supportive data for the potential application of LBL Lipo-graph for photothermal therapy. Study results suggest the novel dual-sensitive nanoparticles allow intracellular doxorubin delivery and respond to either acidic environments or NIR excitation. Stimuli sensitive hybrid nanoparticles have been synthesized using a layer-by-layer technique and demonstrated for dual chemo-photothermal destruction of breast cancer cells. The hybrid nanoparticles are composed of alternating layers of graphene oxide and graphene oxide conjugated poly-l-lysine coating the surface of a thermosensitive cationic liposome containing doxorubicin as a core. Data suggests that the hybrid nanoparticles may offer many advantages for chemo-photothermal therapy. Advantages include a decrease of the initial burst release which may result in the reduction in systemic toxicity, increase in pH responsivity around the tumor environment and improved NIR light absorption. Copyright © 2017 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

A facile route to the synthesis of magnetically separable BiOBr/NiFe2O4 composites with enhanced photocatalytic performance

NASA Astrophysics Data System (ADS)

Li, Xiaowei; Wang, Li; Zhang, Lei; Zhuo, Shuping

2017-10-01

Novel magnetically separable BiOBr/NiFe2O4 composite photocatalysts with different mass ratios were fabricated through a facile hydrothermal treatment. The phases, morphologies and photophysical properties of the as-obtained samples were characterized by X-ray diffraction (XRD), energy dispersive spectrometry (EDS), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), transmission electron microcopy (TEM) and diffuse reflection spectroscopy (DRS). Their visible light photocatalytic performances were examined by degradation of methylene blue (MB) and phenol. Compared with bare BiOBr and NiFe2O4, all heterostructured BiOBr/NiFe2O4 nanocomposites exhibited significantly enhanced photocatalytic efficiency. The BiOBr/NiFe2O4-20% composite showed the highest photodegradation capacity, which was about 3.2 and 22.4 times greater than that of individual BiOBr and NiFe2O4, respectively. The degradation efficiency of BiOBr/NiFe2O4-20% in the degradation of MB dye hardly changed after five cycles, signifying that the BiOBr/NiFe2O4-20% photocatalyst had excellent recyclability. In addition, BiOBr/NiFe2O4 composite photocatalysts could be easily separated from contaminant solution by using a magnet and recycled, exhibiting great potential for application in the fields of environmental purification of organic pollutants and wastewater treatment. In the light of experimental results, we proposed a photocatalytic mechanism which confirmed that the enhancement of photocatalytic performance for BiOBr/NiFe2O4 composites was mainly ascribed to the efficient separation of photo-induced charges resulting from the well-known "heterostructure effect" between NiFe2O4 nanorods and BiOBr nanosheets.

Mechanism of morphology transformation during annealing of nanostructured gold films on glass.

PubMed

Karakouz, Tanya; Tesler, Alexander B; Sannomiya, Takumi; Feldman, Yishay; Vaskevich, Alexander; Rubinstein, Israel

2013-04-07

Nanostructured, just-percolated gold films were prepared by evaporation on bare glass. Annealing of the films at temperatures close to or higher than the softening temperature of the glass substrate induces morphological transformation to discrete Au islands and gradual embedding of the formed islands in the glass. The mechanism and kinetics of these processes are studied here using a combination of in situ high-temperature optical spectroscopy; ex situ characterization of the island shape by high-resolution scanning electron microscopy (HRSEM), atomic force microcopy (AFM) and cross-sectional transmission electron microscopy (TEM); and numerical simulations of transmission spectra using the Multiple Multipole Program (MMP) approach. It is shown that the morphological transformation of just-percolated, 10 nm (nominal thickness) Au films evaporated on glass and annealed at 600 °C, i.e., in the vicinity of the substrate glass transition temperature (Tg = 557 °C), proceeds via three processes exhibiting different time scales: (i) fast recrystallization and dewetting, leading to formation of single-crystalline islands (minutes); the initial spectrum characteristic of a continuous Au film is transformed to that of an island film, displaying a surface plasmon (SP) absorption band. (ii) Reshaping and faceting of the single-crystalline islands accompanied by formation of circumferential glass rims around them (first few hours); the overall optical response shows a blue shift of the SP band. (iii) Gradual island embedding in the glass substrate (tens of hours), seen as a characteristic red shift of the SP band. The influence of the annealing atmosphere (air, vacuum) on the embedding process is found to be minor. Numerical modeling of the extinction cross-section corresponding to the morphological transformations during island recrystallization and embedding is in qualitative agreement with the experimental data.

Electron Losses from the Magnetosphere.

DTIC Science & Technology

1983-03-01

E 14 111=30mI~12 MICROCOPY RESOLUTION TEST CHART NATIONAL BUREAU OF STANDARDS-1963-A a’ 40 " L...34 "° ’ ’ ’ "’ ’ ’’ ’’ ’" " ’" "’" " " ’ "’ ’ " " " ’ " .. ."__ "" • °-. .. .. .. ... .. . . ,’ . e - •" . .. .. . . .. . ..- . ;. . ; ; . .. ; -. . . . .. . . - - - . . ."-.- ’’’-’:..::L...i* I .. .* . .. Ap ro e fo pu. s. .db~ t o nn iad -4" AYIT/GNE/PH/83M-4

Characterization of alteration textures in Cretaceous oceanic crust (pillow lava) from the N-Atlantic (DSDP Hole 418A) by spatially-resolved spectroscopy

NASA Astrophysics Data System (ADS)

Fliegel, Daniel; Knowles, Emily; Wirth, Richard; Templeton, Alexis; Staudigel, Hubert; Muehlenbachs, Karlis; Furnes, Harald

2012-11-01

The habit, mineralogy, crystallography, and Fe speciation of tubular and granular alteration textures in basaltic glass recovered from DSDP Hole 418A, which have previously been associated with biologically mediated alteration, were investigated using an integrated suite of microscopic and spectroscopic approaches in order to shine light on their formation and mineralization history. Two different analytical approaches were used: (1) micro scale investigations with conventional petrographic optical microcopy and microscale X-ray fluorescence mapping and X-ray absorption spectroscopy, and (2) nano scale analyses with FIB (focused ion beam milling) to prepare cross-sections for TEM (transmission electron microscopy), EELS (electron energy loss spectroscopy), and STXM (scanning transmission electron microscopy) analyses. The integrated data show that tubular and granular textures are similar in chemical, mineralogical and structural habit. Both granular and tubular alteration textures show a marked transition from ferrous iron in the glass matrix to ferric iron in the textures. Granular and tubular textures are filled with sheet silicates of similar chemistry, and both exhibit thin amorphous alteration rims ∼10-20 nm wide. The alteration rims are typically depleted in Ca and Fe. Ca is enriched at the contact between the secondary mineralization and the alteration rims, whereas Fe is enriched throughout the alteration features and is mainly present as FeIII in contrast to FeII in the host glass. Carbon is enriched only in a few areas, and could possibly be of organic origin but is not bound in carbonate. The mineralization of the features follows the sequence: dissolution of the glass; formation of a leached amorphous rim; mineralizing the cavities by smectide type clays and subsequently congruent growing of the texture diameter by diffusing of the elements through the alteration layer. None of the features could be linked solely to a biogenic origin and hence the biogenicity of the textures can neither be refuted nor supported by this micro- and nano-scale data set.

Gold catalyzed nickel disilicide formation: a new solid-liquid-solid phase growth mechanism.

PubMed

Tang, Wei; Picraux, S Tom; Huang, Jian Yu; Liu, Xiaohua; Tu, K N; Dayeh, Shadi A

2013-01-01

The vapor-liquid-solid (VLS) mechanism is the predominate growth mechanism for semiconductor nanowires (NWs). We report here a new solid-liquid-solid (SLS) growth mechanism of a silicide phase in Si NWs using in situ transmission electron microcopy (TEM). The new SLS mechanism is analogous to the VLS one in relying on a liquid-mediating growth seed, but it is fundamentally different in terms of nucleation and mass transport. In SLS growth of Ni disilicide, the Ni atoms are supplied from remote Ni particles by interstitial diffusion through a Si NW to the pre-existing Au-Si liquid alloy drop at the tip of the NW. Upon supersaturation of both Ni and Si in Au, an octahedral nucleus of Ni disilicide (NiSi2) forms at the center of the Au liquid alloy, which thereafter sweeps through the Si NW and transforms Si into NiSi2. The dissolution of Si by the Au alloy liquid mediating layer proceeds with contact angle oscillation at the triple point where Si, oxide of Si, and the Au alloy meet, whereas NiSi2 is grown from the liquid mediating layer in an atomic stepwise manner. By using in situ quenching experiments, we are able to measure the solubility of Ni and Si in the Au-Ni-Si ternary alloy. The Au-catalyzed mechanism can lower the formation temperature of NiSi2 by 100 °C compared with an all solid state reaction.

Single-molecule junction of an overcrowded ethylene with binary conductance states

NASA Astrophysics Data System (ADS)

Koike, Masato; Fujii, Shintaro; Cho, Haruna; Shoji, Yoshiaki; Nishino, Tomoaki; Fukushima, Takanori; Kiguchi, Manabu

2018-03-01

Overcrowded ethylene 1 shows mechanochromic behavior with contrasting color change between yellow and violet arising from its conformational isomerization, which should also be accompanied by the change in the electronic structure. Here, we report a single-molecule electronic study of 1 using scanning tunneling microcopy (STM) and STM-based break junction techniques. The single-molecule junction of 1 sandwiched by Au electrodes showed two distinct high- and low-conductance states with the conductance values of 0.003 and 0.0002 G 0. The high-conductance state is one order of magnitude more conductive than the low-conductance state. The two states can be ascribed to two conformational isomers of 1 in the junction.

Non-Periodic Helix TWT Study.

DTIC Science & Technology

1980-05-01

IA-A087 413 LITTON SYSTEMS INC SAN CARLOS CA ELECTRON TUBE DIV F/6 9/1 NON-PERIODIC HELIX TWT STUDY.(U) MAY 80 N00173-76C-014 UNCLASSIFIED ML...IEEEEEEmhEEI U-80 - ’l////////,, 11111 128 25 L1. = *""L 1- 1.8 MICROCOPY RESOLUTION TEST CHART ’IT-, ( (NO-PERIODIC HELIX WTSTUDY0 I EXTENSION OF CONTRACT... Helix Circuit 4 - 2 Non-Periodic Helix Structure 7 3 Unwound Tape for Non-Periodic Helix 8 4 Typical Helix Assembly 10 5 Typical Ladder Assembly 11 6

Potential Applications of Manual Games,

DTIC Science & Technology

1984-02-01

34 just because some electronic equipment is used to keep track of logistics, combat results, and force status. Even a highly computerized game like...D-A152 541 POTENTIAL APPLICATIONS OF MANUAL GAMES (U) RAND CORP ii SANTA MONICA CA T A BROW~N FEB 84 RAND/P-6957 UNCLASI7FIED F/G 12/2 N El..I 111 1...128 112.5 111 m; * _ 1.8 I1111 ’I’ll MICROCOPY RESOLUTION TEST CHART NATI NAl fii~ t1 RI 1A L4k, I POTENTIAL APPLICATIONS OF MANUJAL GAMES Lfl N Lfl

Experimental rabies in a great horned owl.

PubMed

Jorgenson, R D; Gough, P M; Graham, D L

1976-07-01

A great horned owl (Bubo virginianus) was fed the carcass of an experimentally infected rabid skunk. The bird developed antibody titer to rabies, detected by passive haemagglutination, 27 days after oral inoculation by ingestion. The owl suppressed the infection until corticosteroid administration, after which a maximum antibody titer was attained. Evidence of active rabies viral infection was seen by fluorescent antibody staining of oral swabs, corneal impression smears and histologic tissue smears, by suckling mouse inoculation of oral swab washings, and by transmission electron microcopy. No clinical signs of rabies virus infection were observed.

Self-catalytic branch growth of SnO 2 nanowire junctions

NASA Astrophysics Data System (ADS)

Chen, Y. X.; Campbell, L. J.; Zhou, W. L.

2004-10-01

Multiple branched SnO2 nanowire junctions have been synthesized by thermal evaporation of SnO powder. Their nanostructures were studied by transmission electron microscopy and field emission scanning electron microcopy. It was observed that Sn nanoparticles generated from decomposition of the SnO powder acted as self-catalysts to control the SnO2 nanojunction growth. Orthorhombic SnO2 was found as a dominate phase in nanojunction growth instead of rutile structure. The branches and stems of nanojunctions were found to be an epitaxial growth by electron diffraction analysis and high-resolution electron microscopy observation. The growth directions of the branched SnO2 nanojunctions were along the orthorhombic [1 1 0] and [ 1 1 bar 0 ] . A self-catalytic vapor-liquid-solid growth mechanism is proposed to describe the growth process of the branched SnO2 nanowire junctions.

Electron tomography of whole cultured cells using novel transmission electron imaging technique.

PubMed

Okumura, Taiga; Shoji, Minami; Hisada, Akiko; Ominami, Yusuke; Ito, Sukehiro; Ushiki, Tatsuo; Nakajima, Masato; Ohshima, Takashi

2018-01-01

Since a three-dimensional (3D) cellular ultrastructure is significant for biological functions, it has been investigated using various electron microscopic techniques. Although transmission electron microscopy (TEM)-based techniques are traditionally used, cells must be embedded in resin and sliced into ultrathin sections in sample preparation processes. Block-face observation using a scanning electron microscope (SEM) has also been recently applied to 3D observation of cellular components, but this is a destructive inspection and does not allow re-examination. Therefore, we developed electron tomography using a transmission electron imaging technique called Plate-TEM. With Plate-TEM, the cells cultured directly on a scintillator plate are inserted into a conventional SEM equipped with a Plate-TEM observation system, and their internal structures are observed by detecting scintillation light produced by electrons passing through the cells. This technology has the following four advantages. First, the cells cultured on the plate can be observed at electron-microscopic resolution since they remain on the plate. Second, both surface and internal information can be obtained simultaneously by using electron- and photo-detectors, respectively, because a Plate-TEM detector is installed in an SEM. Third, the cells on the scintillator plate can also be inspected using light microscopy because the plate has transparent features. Finally, correlative observation with other techniques, such as conventional TEM, is possible after Plate-TEM observation because Plate-TEM is a non-destructive analysis technique. We also designed a sample stage to tilt the samples for tomography with Plate-TEM, by which 3D organization of cellular structures can be visualized as a whole cell. In the present study, Mm2T cells were investigated using our tomography system, resulting in 3D visualization of cell organelles such as mitochondria, lipid droplets, and microvilli. Correlative observations with various imaging techniques were also conducted by successive observations with light microscopy, SEM, Plate-TEM, and conventional TEM. Consequently, the Plate-TEM tomography technique encourages understanding of cellular structures at high resolution, which can contribute to cellular biological research. Copyright © 2017 Elsevier Ltd. All rights reserved.

The Central Hinge Link Truncation of the Antimicrobial Peptide Fowlicidin-3 Enhances Its Cell Selectivity without Antibacterial Activity Loss

PubMed Central

Qu, Pei; Gao, Wei; Chen, Huixian; Li, Dan; Yang, Na; Zhu, Jian; Li, Zhongqiu

2016-01-01

Antimicrobial peptides (AMPs) have been paid considerable attention because of their broad-spectrum antimicrobial activity and a reduced possibility of the development of bacterial drug resistance. Fowlicidin-3 (Fow-3) is an identified type of chicken cathelicidin AMP that has exhibited considerable antimicrobial activity and cytotoxicity. To reduce cell toxicity and improve cell selectivity, several truncated peptides of fowlicidin-3, Fow-3(1-15), Fow-3(1-19), Fow-3(1-15-20-27), and Fow-3(20-27), were synthesized. Our results indicated that neither the N- nor C-terminal segment alone [Fow-3(1-15), Fow-3(1-19), Fow-3(20-27)] was sufficient to confer antibacterial activity. However, Fow-3(1-19) with the inclusion of the central hinge link (-AGIN-) retained substantial cell toxicity, which other analogs lost. Fow-3(1-15-20-27) displayed potent antimicrobial activity for a wide range of Gram-negative and Gram-positive bacteria and no obvious hemolytic activity or cytotoxicity. The central link region was shown to be critically important in the function of cell toxicity but was not relevant to antibacterial activity. Fow-3(1-15-20-27) maintained antibacterial activity in the presence of physiological concentrations of salts. The results from fluorescence spectroscopy, scanning electron microcopy, and transmission electron microcopy showed that Fow-3(1-15-20-27) as well as fowlicidin-3 killed bacterial cells by increasing membrane permeability and damaging the membrane envelope integrity. Fow-3(1-15-20-27) could be a promising antimicrobial agent for clinical application. PMID:26902768

Single-Molecule Electronics: Chemical and Analytical Perspectives.

PubMed

Nichols, Richard J; Higgins, Simon J

2015-01-01

It is now possible to measure the electrical properties of single molecules using a variety of techniques including scanning probe microcopies and mechanically controlled break junctions. Such measurements can be made across a wide range of environments including ambient conditions, organic liquids, ionic liquids, aqueous solutions, electrolytes, and ultra high vacuum. This has given new insights into charge transport across molecule electrical junctions, and these experimental methods have been complemented with increasingly sophisticated theory. This article reviews progress in single-molecule electronics from a chemical perspective and discusses topics such as the molecule-surface coupling in electrical junctions, chemical control, and supramolecular interactions in junctions and gating charge transport. The article concludes with an outlook regarding chemical analysis based on single-molecule conductance.

Single shot damage mechanism of Mo/Si multilayer optics under intense pulsed XUV-exposure.

PubMed

Khorsand, A R; Sobierajski, R; Louis, E; Bruijn, S; van Hattum, E D; van de Kruijs, R W E; Jurek, M; Klinger, D; Pelka, J B; Juha, L; Burian, T; Chalupsky, J; Cihelka, J; Hajkova, V; Vysin, L; Jastrow, U; Stojanovic, N; Toleikis, S; Wabnitz, H; Tiedtke, K; Sokolowski-Tinten, K; Shymanovich, U; Krzywinski, J; Hau-Riege, S; London, R; Gleeson, A; Gullikson, E M; Bijkerk, F

2010-01-18

We investigated single shot damage of Mo/Si multilayer coatings exposed to the intense fs XUV radiation at the Free-electron LASer facility in Hamburg - FLASH. The interaction process was studied in situ by XUV reflectometry, time resolved optical microscopy, and "post-mortem" by interference-polarizing optical microscopy (with Nomarski contrast), atomic force microscopy, and scanning transmission electron microcopy. An ultrafast molybdenum silicide formation due to enhanced atomic diffusion in melted silicon has been determined to be the key process in the damage mechanism. The influence of the energy diffusion on the damage process was estimated. The results are of significance for the design of multilayer optics for a new generation of pulsed (from atto- to nanosecond) XUV sources.

Mitochondrial and Chromosomal Damage Induced by Oxidative Stress in Zn2+ Ions, ZnO-Bulk and ZnO-NPs treated Allium cepa roots

PubMed Central

Ahmed, Bilal; Dwivedi, Sourabh; Abdin, Malik Zainul; Azam, Ameer; Al-Shaeri, Majed; Khan, Mohammad Saghir; Saquib, Quaiser; Al-Khedhairy, Abdulaziz A.; Musarrat, Javed

2017-01-01

Large-scale synthesis and release of nanomaterials in environment is a growing concern for human health and ecosystem. Therefore, we have investigated the cytotoxic and genotoxic potential of zinc oxide nanoparticles (ZnO-NPs), zinc oxide bulk (ZnO-Bulk), and zinc ions (Zn2+) in treated roots of Allium cepa, under hydroponic conditions. ZnO-NPs were characterized by UV-visible, XRD, FT-IR spectroscopy and TEM analyses. Bulbs of A. cepa exposed to ZnO-NPs (25.5 nm) for 12 h exhibited significant decrease (23 ± 8.7%) in % mitotic index and increase in chromosomal aberrations (18 ± 7.6%), in a dose-dependent manner. Transmission electron microcopy and FT-IR data suggested surface attachment, internalization and biomolecular intervention of ZnO-NPs in root cells, respectively. The levels of TBARS and antioxidant enzymes were found to be significantly greater in treated root cells vis-à-vis untreated control. Furthermore, dose-dependent increase in ROS production and alterations in ΔΨm were observed in treated roots. FT-IR analysis of root tissues demonstrated symmetric and asymmetric P=O stretching of >PO2− at 1240 cm−1 and stretching of C-O ribose at 1060 cm−1, suggestive of nuclear damage. Overall, the results elucidated A. cepa, as a good model for assessment of cytotoxicity and oxidative DNA damage with ZnO-NPs and Zn2+ in plants. PMID:28120857

Physical vs. photolithographic patterning of plasma polymers: an investigation by ToF-SSIMS and multivariate analysis

PubMed Central

Mishra, Gautam; Easton, Christopher D.; McArthur, Sally L.

2009-01-01

Physical and photolithographic techniques are commonly used to create chemical patterns for a range of technologies including cell culture studies, bioarrays and other biomedical applications. In this paper, we describe the fabrication of chemical micropatterns from commonly used plasma polymers. Atomic force microcopy (AFM) imaging, Time-of-Flight Static Secondary Ion Mass Spectrometry (ToF-SSIMS) imaging and multivariate analysis have been employed to visualize the chemical boundaries created by these patterning techniques and assess the spatial and chemical resolution of the patterns. ToF-SSIMS analysis demonstrated that well defined chemical and spatial boundaries were obtained from photolithographic patterning, while the resolution of physical patterning via a transmission electron microscopy (TEM) grid varied depending on the properties of the plasma system including the substrate material. In general, physical masking allowed diffusion of the plasma species below the mask and bleeding of the surface chemistries. Multivariate analysis techniques including Principal Component Analysis (PCA) and Region of Interest (ROI) assessment were used to investigate the ToF-SSIMS images of a range of different plasma polymer patterns. In the most challenging case, where two strongly reacting polymers, allylamine and acrylic acid were deposited, PCA confirmed the fabrication of micropatterns with defined spatial resolution. ROI analysis allowed for the identification of an interface between the two plasma polymers for patterns fabricated using the photolithographic technique which has been previously overlooked. This study clearly demonstrated the versatility of photolithographic patterning for the production of multichemistry plasma polymer arrays and highlighted the need for complimentary characterization and analytical techniques during the fabrication plasma polymer micropatterns. PMID:19950941

In-situ study of crystallization kinetics in ternary bulk metallic glass alloys with different glass forming abilities

DOE PAGES

Lan, Si; Wei, Xiaoya; Zhou, Jie; ...

2014-11-18

In-situ transmission electron microcopy and time-resolved neutron diffraction were used to study crystallization kinetics of two ternary bulk metallic glasses during isothermal annealing in the supercooled liquid region. It is found that the crystallization of Zr 56Cu 36Al 8, an average glass former, follows continuous nucleation and growth, while that of Zr 46Cu 46Al 8, a better glass former, is characterized by site-saturated nucleation, followed by slow growth. Possible mechanisms for the observed differences and the relationship to the glass forming ability are discussed.

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

PubMed

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

2014-12-01

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

Detecting single-electron events in TEM using low-cost electronics and a silicon strip sensor.

PubMed

Gontard, Lionel C; Moldovan, Grigore; Carmona-Galán, Ricardo; Lin, Chao; Kirkland, Angus I

2014-04-01

There is great interest in developing novel position-sensitive direct detectors for transmission electron microscopy (TEM) that do not rely in the conversion of electrons into photons. Direct imaging improves contrast and efficiency and allows the operation of the microscope at lower energies and at lower doses without loss in resolution, which is especially important for studying soft materials and biological samples. We investigate the feasibility of employing a silicon strip detector as an imaging detector for TEM. This device, routinely used in high-energy particle physics, can detect small variations in electric current associated with the impact of a single charged particle. The main advantages of using this type of sensor for direct imaging in TEM are its intrinsic radiation hardness and large detection area. Here, we detail design, simulation, fabrication and tests in a TEM of the front-end electronics developed using low-cost discrete components and discuss the limitations and applications of this technology for TEM.

The Central Hinge Link Truncation of the Antimicrobial Peptide Fowlicidin-3 Enhances Its Cell Selectivity without Antibacterial Activity Loss.

PubMed

Qu, Pei; Gao, Wei; Chen, Huixian; Li, Dan; Yang, Na; Zhu, Jian; Feng, Xingjun; Liu, Chunlong; Li, Zhongqiu

2016-05-01

Antimicrobial peptides (AMPs) have been paid considerable attention because of their broad-spectrum antimicrobial activity and a reduced possibility of the development of bacterial drug resistance. Fowlicidin-3 (Fow-3) is an identified type of chicken cathelicidin AMP that has exhibited considerable antimicrobial activity and cytotoxicity. To reduce cell toxicity and improve cell selectivity, several truncated peptides of fowlicidin-3, Fow-3(1-15), Fow-3(1-19), Fow-3(1-15-20-27), and Fow-3(20-27), were synthesized. Our results indicated that neither the N- nor C-terminal segment alone [Fow-3(1-15), Fow-3(1-19), Fow-3(20-27)] was sufficient to confer antibacterial activity. However, Fow-3(1-19) with the inclusion of the central hinge link (-AGIN-) retained substantial cell toxicity, which other analogs lost. Fow-3(1-15-20-27) displayed potent antimicrobial activity for a wide range of Gram-negative and Gram-positive bacteria and no obvious hemolytic activity or cytotoxicity. The central link region was shown to be critically important in the function of cell toxicity but was not relevant to antibacterial activity. Fow-3(1-15-20-27) maintained antibacterial activity in the presence of physiological concentrations of salts. The results from fluorescence spectroscopy, scanning electron microcopy, and transmission electron microcopy showed that Fow-3(1-15-20-27) as well as fowlicidin-3 killed bacterial cells by increasing membrane permeability and damaging the membrane envelope integrity. Fow-3(1-15-20-27) could be a promising antimicrobial agent for clinical application. Copyright © 2016, American Society for Microbiology. All Rights Reserved.

Structure refinement for tantalum nitrides nanocrystals with various morphologies

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, Lianyun; School of Science, Beijing Jiaotong University, 3 Shang Yuan Cun, Haidian District, Beijing 100044; Huang, Kai

2012-07-15

Graphical abstract: Tantalum nitrides nanocrystals with various phases and morphologies for the first time have been synthesized through homogenous sodium reduction under low temperature with the subsequent annealing process under high vacuum. Highlights: ► The spherical TaN, cuboidal TaN{sub 0.83} and TaN{sub 0.5} nanocrystals have been synthesized through homogenous sodium reduction under low temperature with the subsequent annealing process under high vacuum. ► The crystal structures of different tantalum nitrides were determined by Rietveld refinement on the X-ray diffraction data and the examinations of electron microcopies. ► The specific surface area of the tantalum nitrides powders was around 10 m{supmore » 2} g{sup −1}. ► Tantalum nitrides powders could be suitable for capacitor with high specific capacitance. -- Abstract: Tantalum nitrides (TaN{sub x}) nanocrystals with different phase and morphology have been synthesized through homogenous sodium reduction under low temperature with the subsequent annealing process under high vacuum. The crystal structures of tantalum nitrides were determined by Rietveld refinement based on the X-ray diffraction data. The morphologies of various tantalum nitrides nanocrystals in high quality were analyzed through the electron microcopies examinations. The spherical TaN nanoparticles, cuboidal TaN{sub 0.83} and TaN{sub 0.5} nanocrystals have been selectively prepared at different annealing temperatures. In addition, the specific surface areas of the tantalum nitrides nanocrystals measured by BET method were around 9.87–11.64 m{sup 2} g{sup −1}, indicating that such nano-sized tantalum nitrides could be suitable for capacitor with high specific capacitance.« less

Direct identification of metallic and semiconducting single-walled carbon nanotubes in scanning electron microscopy.

PubMed

Li, Jie; He, Yujun; Han, Yimo; Liu, Kai; Wang, Jiaping; Li, Qunqing; Fan, Shoushan; Jiang, Kaili

2012-08-08

Because of their excellent electrical and optical properties, carbon nanotubes have been regarded as extremely promising candidates for high-performance electronic and optoelectronic applications. However, effective and efficient distinction and separation of metallic and semiconducting single-walled carbon nanotubes are always challenges for their practical applications. Here we show that metallic and semiconducting single-walled carbon nanotubes on SiO(2) can have obviously different contrast in scanning electron microscopy due to their conductivity difference and thus can be effectively and efficiently identified. The correlation between conductivity and contrast difference has been confirmed by using voltage-contrast scanning electron microcopy, peak force tunneling atom force microscopy, and field effect transistor testing. This phenomenon can be understood via a proposed mechanism involving the e-beam-induced surface potential of insulators and the conductivity difference between metallic and semiconducting SWCNTs. This method demonstrates great promise to achieve rapid and large-scale distinguishing between metallic and semiconducting single-walled carbon nanotubes, adding a new function to conventional SEM.

Consecutive light microscopy, scanning-transmission electron microscopy and transmission electron microscopy of traumatic human brain oedema and ischaemic brain damage.

PubMed

Castejon, O J; Castejon, H V; Diaz, M; Castellano, A

2001-10-01

Cortical biopsies of 11 patients with traumatic brain oedema were consecutively studied by light microscopy (LM) using thick plastic sections, scanning-transmission electron microscopy ((S)TEM) using semithin plastic sections and transmission electron microscopy (TEM) using ultrathin sections. Samples were glutaraldehyde-osmium fixed and embedded in Araldite or Epon. Thick sections were stained with toluidine-blue for light microscopy. Semithin sections were examined unstained and uncoated for (S)TEM. Ultrathin sections were stained with uranyl and lead. Perivascular haemorrhages and perivascular extravasation of proteinaceous oedema fluid were observed in both moderate and severe oedema. Ischaemic pyramidal and non-pyramidal nerve cells appeared shrunken, electron dense and with enlargement of intracytoplasmic membrane compartment. Notably swollen astrocytes were observed in all samples examined. Glycogen-rich and glycogen-depleted astrocytes were identified in anoxic-ischaemic regions. Dark and hydropic satellite, interfascicular and perivascular oligodendrocytes were also found. The status spongiosus of severely oedematous brain parenchyma observed by LM and (S)TEM was correlated with the enlarged extracellular space and disrupted neuropil observed by TEM. The (S)TEM is recommended as a suitable technique for studying pathological processes in the central nervous system and as an informative adjunct to LM and TEM.

Characterizing Surfaces of the Wide Bandgap Semiconductor Ilmenite with Scanning Probe Microcopies

NASA Technical Reports Server (NTRS)

Wilkins, R.; Powell, Kirk St. A.

1997-01-01

Ilmenite (FeTiO3) is a wide bandgap semiconductor with an energy gap of about 2.5eV. Initial radiation studies indicate that ilmenite has properties suited for radiation tolerant applications, as well as a variety of other electronic applications. Two scanning probe microscopy methods have been used to characterize the surface of samples taken from Czochralski grown single crystals. The two methods, atomic force microscopy (AFM) and scanning tunneling microscopy (STM), are based on different physical principles and therefore provide different information about the samples. AFM provides a direct, three-dimensional image of the surface of the samples, while STM give a convolution of topographic and electronic properties of the surface. We will discuss the differences between the methods and present preliminary data of each method for ilmenite samples.

Single-particle cryo-electron microscopy of Rift Valley fever virus

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sherman, Michael B.; Sealy Center for Structural Biology and Molecular Biophysics, University of Texas Medical Branch, Galveston, TX 77555; Freiberg, Alexander N.

2009-04-25

Rift Valley fever virus (RVFV; Bunyaviridae; Phlebovirus) is an emerging human and veterinary pathogen causing acute hepatitis in ruminants and has the potential to cause hemorrhagic fever in humans. We report a three-dimensional reconstruction of RVFV vaccine strain MP-12 (RVFV MP-12) by cryo-electron microcopy using icosahedral symmetry of individual virions. Although the genomic core of RVFV MP-12 is apparently poorly ordered, the glycoproteins on the virus surface are highly symmetric and arranged on a T = 12 icosahedral lattice. Our RVFV MP-12 structure allowed clear identification of inter-capsomer contacts and definition of possible glycoprotein arrangements within capsomers. This structure providesmore » a detailed model for phleboviruses, opens new avenues for high-resolution structural studies of the bunyavirus family, and aids the design of antiviral diagnostics and effective subunit vaccines.« less

Carbon nanotube and graphene nanoribbon-coated conductive Kevlar fibers.

PubMed

Xiang, Changsheng; Lu, Wei; Zhu, Yu; Sun, Zhengzong; Yan, Zheng; Hwang, Chi-Chau; Tour, James M

2012-01-01

Conductive carbon material-coated Kevlar fibers were fabricated through layer-by-layer spray coating. Polyurethane was used as the interlayer between the Kevlar fiber and carbon materials to bind the carbon materials to the Kevlar fiber. Strongly adhering single-walled carbon nanotube coatings yielded a durable conductivity of 65 S/cm without significant mechanical degradation. In addition, the properties remained stable after bending or water washing cycles. The coated fibers were analyzed using scanning electron microcopy and a knot test. The as-produced fiber had a knot efficiency of 23%, which is more than four times higher than that of carbon fibers. The spray-coating of graphene nanoribbons onto Kevlar fibers was also investigated. These flexible coated-Kevlar fibers have the potential to be used for conductive wires in wearable electronics and battery-heated armors. © 2011 American Chemical Society

Advanced electron microscopy characterization of nanomaterials for catalysis

DOE Office of Scientific and Technical Information (OSTI.GOV)

Su, Dong

Transmission electron microscopy (TEM) has become one of the most powerful techniques in the fields of material science, inorganic chemistry and nanotechnology. In terms of resolutions, advanced TEM may reach a high spatial resolution of 0.05 nm, a high energy-resolution of 7 meV. In addition, in situ TEM can help researcher to image the process happened within 1 ms. This paper reviews the recent technical approaches of applying advanced TEM characterization on nanomaterials for catalysis. The text is organized according to the demanded information of nanocrystals from the perspective of application: for example, size, composition, phase, strain, and morphology. Themore » electron beam induced effect and in situ TEM are also introduced. As a result, I hope this review can help the scientists in related fields to take advantage of advanced TEM to their own researches.« less

Advanced electron microscopy characterization of nanomaterials for catalysis

DOE PAGES

Su, Dong

2017-04-01

Transmission electron microscopy (TEM) has become one of the most powerful techniques in the fields of material science, inorganic chemistry and nanotechnology. In terms of resolutions, advanced TEM may reach a high spatial resolution of 0.05 nm, a high energy-resolution of 7 meV. In addition, in situ TEM can help researcher to image the process happened within 1 ms. This paper reviews the recent technical approaches of applying advanced TEM characterization on nanomaterials for catalysis. The text is organized according to the demanded information of nanocrystals from the perspective of application: for example, size, composition, phase, strain, and morphology. Themore » electron beam induced effect and in situ TEM are also introduced. As a result, I hope this review can help the scientists in related fields to take advantage of advanced TEM to their own researches.« less

In situ TEM of radiation effects in complex ceramics.

PubMed

Lian, Jie; Wang, L M; Sun, Kai; Ewing, Rodney C

2009-03-01

In situ transmission electron microscopy (TEM) has been extensively applied to study radiation effects in a wide variety of materials, such as metals, ceramics and semiconductors and is an indispensable tool in obtaining a fundamental understanding of energetic beam-matter interactions, damage events, and materials' behavior under intense radiation environments. In this article, in situ TEM observations of radiation effects in complex ceramics (e.g., oxides, silicates, and phosphates) subjected to energetic ion and electron irradiations have been summarized with a focus on irradiation-induced microstructural evolution, changes in microchemistry, and the formation of nanostructures. New results for in situ TEM observation of radiation effects in pyrochlore, A(2)B(2)O(7), and zircon, ZrSiO(4), subjected to multiple beam irradiations are presented, and the effects of simultaneous irradiations of alpha-decay and beta-decay on the microstructural evolution of potential nuclear waste forms are discussed. Furthermore, in situ TEM results of radiation effects in a sodium borosilicate glass subjected to electron-beam exposure are introduced to highlight the important applications of advanced analytical TEM techniques, including Z-contrast imaging, energy filtered TEM (EFTEM), and electron energy loss spectroscopy (EELS), in studying radiation effects in materials microstructural evolution and microchemical changes. By combining ex situ TEM and advanced analytical TEM techniques with in situ TEM observations under energetic beam irradiations, one can obtain invaluable information on the phase stability and response behaviors of materials under a wide range of irradiation conditions. (c) 2009 Wiley-Liss, Inc.

Regulation of electron temperature gradient turbulence by zonal flows driven by trapped electron modes

DOE Office of Scientific and Technical Information (OSTI.GOV)

Asahi, Y., E-mail: y.asahi@nr.titech.ac.jp; Tsutsui, H.; Tsuji-Iio, S.

2014-05-15

Turbulent transport caused by electron temperature gradient (ETG) modes was investigated by means of gyrokinetic simulations. It was found that the ETG turbulence can be regulated by meso-scale zonal flows driven by trapped electron modes (TEMs), which are excited with much smaller growth rates than those of ETG modes. The zonal flows of which radial wavelengths are in between the ion and the electron banana widths are not shielded by trapped ions nor electrons, and hence they are effectively driven by the TEMs. It was also shown that an E × B shearing rate of the TEM-driven zonal flows is larger thanmore » or comparable to the growth rates of long-wavelength ETG modes and TEMs, which make a main contribution to the turbulent transport before excitation of the zonal flows.« less

Frontiers of in situ electron microscopy

DOE PAGES

Zheng, Haimei; Zhu, Yimei; Meng, Shirley Ying

2015-01-01

In situ transmission electron microscopy (TEM) has become an increasingly important tool for materials characterization. It provides key information on the structural dynamics of a material during transformations and the correlation between structure and properties of materials. With the recent advances in instrumentation, including aberration corrected optics, sample environment control, the sample stage, and fast and sensitive data acquisition, in situ TEM characterization has become more and more powerful. In this article, a brief review of the current status and future opportunities of in situ TEM is included. It also provides an introduction to the six articles covered by inmore » this issue of MRS Bulletin explore the frontiers of in situ electron microscopy, including liquid and gas environmental TEM, dynamic four-dimensional TEM, nanomechanics, ferroelectric domain switching studied by in situ TEM, and state-of-the-art atomic imaging of light elements (i.e., carbon atoms) and individual defects.« less

Optimising electron microscopy experiment through electron optics simulation.

PubMed

Kubo, Y; Gatel, C; Snoeck, E; Houdellier, F

2017-04-01

We developed a new type of electron trajectories simulation inside a complete model of a modern transmission electron microscope (TEM). Our model incorporates the precise and real design of each element constituting a TEM, i.e. the field emission (FE) cathode, the extraction optic and acceleration stages of a 300kV cold field emission gun, the illumination lenses, the objective lens, the intermediate and projection lenses. Full trajectories can be computed using magnetically saturated or non-saturated round lenses, magnetic deflectors and even non-cylindrical symmetry elements like electrostatic biprism. This multi-scale model gathers nanometer size components (FE tip) with parts of meter length (illumination and projection systems). We demonstrate that non-trivial TEM experiments requiring specific and complex optical configurations can be simulated and optimized prior to any experiment using such model. We show that all the currents set in all optical elements of the simulated column can be implemented in the real column (I2TEM in CEMES) and used as starting alignment for the requested experiment. We argue that the combination of such complete electron trajectory simulations in the whole TEM column with automatic optimization of the microscope parameters for optimal experimental data (images, diffraction, spectra) allows drastically simplifying the implementation of complex experiments in TEM and will facilitate the development of advanced use of the electron microscope in the near future. Copyright © 2017 Elsevier B.V. All rights reserved.

Single-particle cryo-electron microscopy of Rift Valley fever virus

PubMed Central

Sherman, Michael B.; Freiberg, Alexander N.; Holbrook, Michael R.; Watowich, Stanley J.

2009-01-01

Rift Valley fever virus (RVFV; Bunyaviridae; Phlebovirus) is an emerging human veterinary pathogen causing acute hepatitis in ruminants and has the potential to Single-particle cryo-EM reconstruction of RVFV MP-12 hemorrhagic fever in humans. We report a three-dimensional reconstruction of RVFV vaccine strain MP-12 (RVFV MP-12) by cryo-electron microcopy using icosahedral symmetry of individual virions. Although the genomic core of RVFV MP-12 is apparently poorly ordered, the glycoproteins on the virus surface are highly symmetric and arranged on a T=12 icosahedral lattice. Our RVFV MP-12 structure allowed clear identification of inter-capsomer contacts and definition of possible glycoprotein arrangements within capsomers. This structure provides a detailed model for phleboviruses, opens new avenues for high-resolution structural studies of the bunyavirus family, and aids the design of antiviral diagnostics and effective subunit-vaccines. PMID:19304307

Preparation of high-quality planar FeRh thin films for in situ TEM investigations

NASA Astrophysics Data System (ADS)

Almeida, Trevor P.; McGrouther, Damien; Pivak, Yevheniy; Perez Garza, Hector Hugo; Temple, Rowan; Massey, Jamie; Marrows, Christopher H.; McVitie, Stephen

2017-10-01

The preparation of a planar FeRh thin film using a focused ion beam (FIB) secondary electron microscope (SEM) for the purpose of in situ transmission electron microscopy (TEM) is presented. A custom SEM stub with 45° faces allows for the transfer and milling of the sample on a TEM heating chip, whilst Fresnel imaging within the TEM revealed the presence of the magnetic domain walls, confirming the quality of the FIB-prepared sample.

Role of zonal flows in trapped electron mode turbulence through nonlinear gyrokinetic particle and continuum simulationa)

NASA Astrophysics Data System (ADS)

Ernst, D. R.; Lang, J.; Nevins, W. M.; Hoffman, M.; Chen, Y.; Dorland, W.; Parker, S.

2009-05-01

Trapped electron mode (TEM) turbulence exhibits a rich variety of collisional and zonal flow physics. This work explores the parametric variation of zonal flows and underlying mechanisms through a series of linear and nonlinear gyrokinetic simulations, using both particle-in-cell and continuum methods. A new stability diagram for electron modes is presented, identifying a critical boundary at ηe=1, separating long and short wavelength TEMs. A novel parity test is used to separate TEMs from electron temperature gradient driven modes. A nonlinear scan of ηe reveals fine scale structure for ηe≳1, consistent with linear expectation. For ηe<1, zonal flows are the dominant saturation mechanism, and TEM transport is insensitive to ηe. For ηe>1, zonal flows are weak, and TEM transport falls inversely with a power law in ηe. The role of zonal flows appears to be connected to linear stability properties. Particle and continuum methods are compared in detail over a range of ηe=d ln Te/d ln ne values from zero to five. Linear growth rate spectra, transport fluxes, fluctuation wavelength spectra, zonal flow shearing spectra, and correlation lengths and times are in close agreement. In addition to identifying the critical parameter ηe for TEM zonal flows, this paper takes a challenging step in code verification, directly comparing very different methods of simulating simultaneous kinetic electron and ion dynamics in TEM turbulence.

High-pressure freezing for scanning transmission electron tomography analysis of cellular organelles.

PubMed

Walther, Paul; Schmid, Eberhard; Höhn, Katharina

2013-01-01

Using an electron microscope's scanning transmission mode (STEM) for collection of tomographic datasets is advantageous compared to bright field transmission electron microscopic (TEM). For image formation, inelastic scattering does not cause chromatic aberration, since in STEM mode no image forming lenses are used after the beam has passed the sample, in contrast to regular TEM. Therefore, thicker samples can be imaged. It has been experimentally demonstrated that STEM is superior to TEM and energy filtered TEM for tomography of samples as thick as 1 μm. Even when using the best electron microscope, adequate sample preparation is the key for interpretable results. We adapted protocols for high-pressure freezing of cultivated cells from a physiological state. In this chapter, we describe optimized high-pressure freezing and freeze substitution protocols for STEM tomography in order to obtain high membrane contrast.

Novel method for measurement of transistor gate length using energy-filtered transmission electron microscopy

NASA Astrophysics Data System (ADS)

Lee, Sungho; Kim, Tae-Hoon; Kang, Jonghyuk; Yang, Cheol-Woong

2016-12-01

As the feature size of devices continues to decrease, transmission electron microscopy (TEM) is becoming indispensable for measuring the critical dimension (CD) of structures. Semiconductors consist primarily of silicon-based materials such as silicon, silicon dioxide, and silicon nitride, and the electrons transmitted through a plan-view TEM sample provide diverse information about various overlapped silicon-based materials. This information is exceedingly complex, which makes it difficult to clarify the boundary to be measured. Therefore, we propose a simple measurement method using energy-filtered TEM (EF-TEM). A precise and effective measurement condition was obtained by determining the maximum value of the integrated area ratio of the electron energy loss spectrum at the boundary to be measured. This method employs an adjustable slit allowing only electrons with a certain energy range to pass. EF-TEM imaging showed a sharp transition at the boundary when the energy-filter’s passband centre was set at 90 eV, with a slit width of 40 eV. This was the optimum condition for the CD measurement of silicon-based materials involving silicon nitride. Electron energy loss spectroscopy (EELS) and EF-TEM images were used to verify this method, which makes it possible to measure the transistor gate length in a dynamic random access memory manufactured using 35 nm process technology. This method can be adapted to measure the CD of other non-silicon-based materials using the EELS area ratio of the boundary materials.

eV-TEM: Transmission electron microscopy in a low energy cathode lens instrument.

PubMed

Geelen, Daniël; Thete, Aniket; Schaff, Oliver; Kaiser, Alexander; van der Molen, Sense Jan; Tromp, Rudolf

2015-12-01

We are developing a transmission electron microscope that operates at extremely low electron energies, 0-40 eV. We call this technique eV-TEM. Its feasibility is based on the fact that at very low electron energies the number of energy loss pathways decreases. Hence, the electron inelastic mean free path increases dramatically. eV-TEM will enable us to study elastic and inelastic interactions of electrons with thin samples. With the recent development of aberration correction in cathode lens instruments, a spatial resolution of a few nm appears within range, even for these very low electron energies. Such resolution will be highly relevant to study biological samples such as proteins and cell membranes. The low electron energies minimize adverse effects due to radiation damage. Copyright © 2015. Published by Elsevier B.V.

Kinetic Transition of Crystal Morphology from Nanoparticles to Dendrites during Electron Beam Induced Deposition of Gold

NASA Astrophysics Data System (ADS)

Park, Jeung Hun; Schneider, Nicholas; Bau, Haim; Kodambaka, Suneel; Ross, Frances

2015-03-01

We studied the kinetic transition from compact nanoparticle to dendritic morphology during electron beam-induced Au deposition using in situ liquid cell-based transmission electron microcopy. Radiolysis of water by electrons generates radicals and molecular species. Hydrated electrons and hydrogen and hydroxide radicals can act as reducing agents and initiate the reduction of the water-soluble precursor, HAuCl4, resulting in the precipitation of Au as nanostructures. We tracked nucleation, growth, and morphological transition of Au from movies recorded in situ, as a function of irradiated dose and liquid thickness. We identified several distinct regimes that depend on the irradiation time: (1) nucleation; (2) linear volumetric growth; (3) formation of dendritic structures; (4) coalescence and dissolution. A diffusion and reaction model for the radiolytic species and metal ions in the confined geometry of the irradiated volume is used to understand the nucleation sites and morphological transitions. We finally describe how nanoparticles can be made to grow in a stepwise manner by switching the supply of Au ions on and off electrochemically, and discuss possibilities for creating more complex nanostructures. This research was partially funded by the National Science Foundation (DMR-1310639, CMMI-1129722, and CBET-1066573).

Preparation of carbon-free TEM microgrids by metal sputtering.

PubMed

Janbroers, S; de Kruijff, T R; Xu, Q; Kooyman, P J; Zandbergen, H W

2009-08-01

A new method for preparing carbon-free, temperature-stable Transmission Electron Microscope (TEM) grids is presented. An 80% Au/20% Pd metal film is deposited onto a 'holey' microgrid carbon supported on standard mixed-mesh Au TEM grids. Subsequently, the carbon film is selectively removed using plasma cleaning. In this way, an all-metal TEM film is made containing the 'same' microgrid as the original carbon film. Although electron transparency of the foil is reduced significantly, the open areas for TEM inspection of material over these areas are maintained. The metal foil can be prepared with various thicknesses and ensures good electrical conductivity. The new Au/Pd grids are stable to at least 775K under vacuum conditions.

Crystalline hydroxyapatite coatings synthesized under hydrothermal conditions on modified titanium substrates.

PubMed

Suchanek, Katarzyna; Bartkowiak, Amanda; Gdowik, Agnieszka; Perzanowski, Marcin; Kąc, Sławomir; Szaraniec, Barbara; Suchanek, Mateusz; Marszałek, Marta

2015-06-01

Hydroxyapatite coatings were successfully produced on modified titanium substrates via hydrothermal synthesis in a Ca(EDTA)(2-) and (NH4)2HPO4 solution. The morphology of modified titanium substrates as well as hydroxyapatite coatings was studied using scanning electron microcopy and phase identification by X-ray diffraction, and Raman and FTIR spectroscopy. The results show that the nucleation and growth of hydroxyapatite needle-like crystals with hexagonal symmetry occurred only on titanium substrates both chemically and thermally treated. No hydroxyapatite phase was detected on only acid etched Ti metal. This finding demonstrates that only a particular titanium surface treatment can effectively induce the apatite nucleation under hydrothermal conditions. Copyright © 2015 Elsevier B.V. All rights reserved.

Advantages and Disadvantages of using a Focused Ion Beam to Prepare TEM Samples From Irradiated U-10Mo Monolithic Nuclear Fuel

DOE Office of Scientific and Technical Information (OSTI.GOV)

B. D. Miller; J. Gan; J. Madden

2012-05-01

Transmission electron microscopy (TEM), scanning electron microscopy (SEM), and focused ion beam (FIB) milling were performed on an irradiated U-10Mo monolithic fuel to understand its irradiation microstructure. This is the first reported TEM work of irradiated fuel sample prepared using a FIB. Advantages and disadvantages of using the FIB to create TEM samples from this irradiated fuel will be presented along with some results from the work. Sample preparation techniques used to create SEM and FIB samples from the brittle irradiated monolithic sample will also be discussed.

A formulation of tissue- and water-equivalent materials using the stoichiometric analysis method for CT-number calibration in radiotherapy treatment planning.

PubMed

Yohannes, Indra; Kolditz, Daniel; Langner, Oliver; Kalender, Willi A

2012-03-07

Tissue- and water-equivalent materials (TEMs) are widely used in quality assurance and calibration procedures, both in radiodiagnostics and radiotherapy. In radiotherapy, particularly, the TEMs are often used for computed tomography (CT) number calibration in treatment planning systems. However, currently available TEMs may not be very accurate in the determination of the calibration curves due to their limitation in mimicking radiation characteristics of the corresponding real tissues in both low- and high-energy ranges. Therefore, we are proposing a new formulation of TEMs using a stoichiometric analysis method to obtain TEMs for the calibration purposes. We combined the stoichiometric calibration and the basic data method to compose base materials to develop TEMs matching standard real tissues from ICRU Report 44 and 46. First, the CT numbers of six materials with known elemental compositions were measured to get constants for the stoichiometric calibration. The results of the stoichiometric calibration were used together with the basic data method to formulate new TEMs. These new TEMs were scanned to validate their CT numbers. The electron density and the stopping power calibration curves were also generated. The absolute differences of the measured CT numbers of the new TEMs were less than 4 HU for the soft tissues and less than 22 HU for the bone compared to the ICRU real tissues. Furthermore, the calculated relative electron density and electron and proton stopping powers of the new TEMs differed by less than 2% from the corresponding ICRU real tissues. The new TEMs which were formulated using the proposed technique increase the simplicity of the calibration process and preserve the accuracy of the stoichiometric calibration simultaneously.

Chapter 14: Electron Microscopy on Thin Films for Solar Cells

DOE Office of Scientific and Technical Information (OSTI.GOV)

Romero, Manuel; Abou-Ras, Daniel; Nichterwitz, Melanie

2016-07-22

This chapter overviews the various techniques applied in scanning electron microscopy (SEM) and transmission electron microscopy (TEM), and highlights their possibilities and also limitations. It gives the various imaging and analysis techniques applied on a scanning electron microscope. The chapter shows that imaging is divided into that making use of secondary electrons (SEs) and of backscattered electrons (BSEs), resulting in different contrasts in the images and thus providing information on compositions, microstructures, and surface potentials. Whenever aiming for imaging and analyses at scales of down to the angstroms range, TEM and its related techniques are appropriate tools. In many cases,more » also SEM techniques provide the access to various material properties of the individual layers, not requiring specimen preparation as time consuming as TEM techniques. Finally, the chapter dedicates to cross-sectional specimen preparation for electron microscopy. The preparation decides indeed on the quality of imaging and analyses.« less

Perspectives on in situ electron microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zheng, Haimei; Zhu, Yimei

In situ transmission electron microscopy (TEM) with the ability to reveal materials dynamic processes with high spatial and temporal resolution has attracted significant interest. The recent advances in in situ methods, including liquid and gas sample environment, pump-probe ultrafast microscopy, nanomechanics and ferroelectric domain switching the aberration corrected electron optics as well as fast electron detector has opened new opportunities to extend the impact of in situ TEM in broad areas of research ranging from materials science to chemistry, physics and biology. Here in this paper, we highlight the development of liquid environment electron microscopy and its applications in themore » study of colloidal nanoparticle growth, electrochemical processes and others; in situ study of topological vortices in ferroelectric and ferromagnetic materials. At the end, perspectives of future in situ TEM are provided.« less

Perspectives on in situ electron microscopy

DOE PAGES

Zheng, Haimei; Zhu, Yimei

2017-03-29

In situ transmission electron microscopy (TEM) with the ability to reveal materials dynamic processes with high spatial and temporal resolution has attracted significant interest. The recent advances in in situ methods, including liquid and gas sample environment, pump-probe ultrafast microscopy, nanomechanics and ferroelectric domain switching the aberration corrected electron optics as well as fast electron detector has opened new opportunities to extend the impact of in situ TEM in broad areas of research ranging from materials science to chemistry, physics and biology. Here in this paper, we highlight the development of liquid environment electron microscopy and its applications in themore » study of colloidal nanoparticle growth, electrochemical processes and others; in situ study of topological vortices in ferroelectric and ferromagnetic materials. At the end, perspectives of future in situ TEM are provided.« less

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

PubMed

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.

Nanofabrication by advanced electron microscopy using intense and focused beam∗.

PubMed

Furuya, Kazuo

2008-01-01

The nanogrowth and nanofabrication of solid substances using an intense and focused electron beam are reviewed in terms of the application of scanning and transmission electron microscopy (SEM, TEM and STEM) to control the size, position and structure of nanomaterials. The first example discussed is the growth of freestanding nanotrees on insulator substrates by TEM. The growth process of the nanotrees was observed in situ and analyzed by high-resolution TEM (HRTEM) and was mainly controlled by the intensity of the electron beam. The second example is position- and size-controlled nanofabrication by STEM using a focused electron beam. The diameters of the nanostructures grown ranged from 4 to 20 nm depending on the size of the electron beam. Magnetic nanostructures were also obtained using an iron-containing precursor gas, Fe(CO) 5 . The freestanding iron nanoantennas were examined by electron holography. The magnetic field was observed to leak from the nanostructure body which appeared to act as a 'nanomagnet'. The third example described is the effect of a vacuum on the size and growth process of fabricated nanodots containing W in an ultrahigh-vacuum field-emission TEM (UHV-FE-TEM). The size of the dots can be controlled by changing the dose of electrons and the partial pressure of the precursor. The smallest particle size obtained was about 1.5 nm in diameter, which is the smallest size reported using this method. Finally, the importance of a smaller probe and a higher electron-beam current with atomic resolution is emphasized and an attempt to develop an ultrahigh-vacuum spherical aberration corrected STEM (Cs-corrected STEM) at NIMS is reported.

Nanofabrication by advanced electron microscopy using intense and focused beam∗

PubMed Central

Furuya, Kazuo

2008-01-01

The nanogrowth and nanofabrication of solid substances using an intense and focused electron beam are reviewed in terms of the application of scanning and transmission electron microscopy (SEM, TEM and STEM) to control the size, position and structure of nanomaterials. The first example discussed is the growth of freestanding nanotrees on insulator substrates by TEM. The growth process of the nanotrees was observed in situ and analyzed by high-resolution TEM (HRTEM) and was mainly controlled by the intensity of the electron beam. The second example is position- and size-controlled nanofabrication by STEM using a focused electron beam. The diameters of the nanostructures grown ranged from 4 to 20 nm depending on the size of the electron beam. Magnetic nanostructures were also obtained using an iron-containing precursor gas, Fe(CO)5. The freestanding iron nanoantennas were examined by electron holography. The magnetic field was observed to leak from the nanostructure body which appeared to act as a ‘nanomagnet’. The third example described is the effect of a vacuum on the size and growth process of fabricated nanodots containing W in an ultrahigh-vacuum field-emission TEM (UHV-FE-TEM). The size of the dots can be controlled by changing the dose of electrons and the partial pressure of the precursor. The smallest particle size obtained was about 1.5 nm in diameter, which is the smallest size reported using this method. Finally, the importance of a smaller probe and a higher electron-beam current with atomic resolution is emphasized and an attempt to develop an ultrahigh-vacuum spherical aberration corrected STEM (Cs-corrected STEM) at NIMS is reported. PMID:27877936

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

NASA Astrophysics Data System (ADS)

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

2016-06-01

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

Low-dose patterning of platinum nanoclusters on carbon nanotubes by focused-electron-beam-induced deposition as studied by TEM

PubMed Central

Bittencourt, Carla; Bals, Sara; Van Tendeloo, Gustaaf

2013-01-01

Summary Focused-electron-beam-induced deposition (FEBID) is used as a direct-write approach to decorate ultrasmall Pt nanoclusters on carbon nanotubes at selected sites in a straightforward maskless manner. The as-deposited nanostructures are studied by transmission electron microscopy (TEM) in 2D and 3D, demonstrating that the Pt nanoclusters are well-dispersed, covering the selected areas of the CNT surface completely. The ability of FEBID to graft nanoclusters on multiple sides, through an electron-transparent target within one step, is unique as a physical deposition method. Using high-resolution TEM we have shown that the CNT structure can be well preserved thanks to the low dose used in FEBID. By tuning the electron-beam parameters, the density and distribution of the nanoclusters can be controlled. The purity of as-deposited nanoclusters can be improved by low-energy electron irradiation at room temperature. PMID:23399584

4D electron microscopy: principles and applications.

PubMed

Flannigan, David J; Zewail, Ahmed H

2012-10-16

The transmission electron microscope (TEM) is a powerful tool enabling the visualization of atoms with length scales smaller than the Bohr radius at a factor of only 20 larger than the relativistic electron wavelength of 2.5 pm at 200 keV. The ability to visualize matter at these scales in a TEM is largely due to the efforts made in correcting for the imperfections in the lens systems which introduce aberrations and ultimately limit the achievable spatial resolution. In addition to the progress made in increasing the spatial resolution, the TEM has become an all-in-one characterization tool. Indeed, most of the properties of a material can be directly mapped in the TEM, including the composition, structure, bonding, morphology, and defects. The scope of applications spans essentially all of the physical sciences and includes biology. Until recently, however, high resolution visualization of structural changes occurring on sub-millisecond time scales was not possible. In order to reach the ultrashort temporal domain within which fundamental atomic motions take place, while simultaneously retaining high spatial resolution, an entirely new approach from that of millisecond-limited TEM cameras had to be conceived. As shown below, the approach is also different from that of nanosecond-limited TEM, whose resolution cannot offer the ultrafast regimes of dynamics. For this reason "ultrafast electron microscopy" is reserved for the field which is concerned with femtosecond to picosecond resolution capability of structural dynamics. In conventional TEMs, electrons are produced by heating a source or by applying a strong extraction field. Both methods result in the stochastic emission of electrons, with no control over temporal spacing or relative arrival time at the specimen. The timing issue can be overcome by exploiting the photoelectric effect and using pulsed lasers to generate precisely timed electron packets of ultrashort duration. The spatial and temporal resolutions achievable with short intense pulses containing a large number of electrons, however, are limited to tens of nanometers and nanoseconds, respectively. This is because Coulomb repulsion is significant in such a pulse, and the electrons spread in space and time, thus limiting the beam coherence. It is therefore not possible to image the ultrafast elementary dynamics of complex transformations. The challenge was to retain the high spatial resolution of a conventional TEM while simultaneously enabling the temporal resolution required to visualize atomic-scale motions. In this Account, we discuss the development of four-dimensional ultrafast electron microscopy (4D UEM) and summarize techniques and applications that illustrate the power of the approach. In UEM, images are obtained either stroboscopically with coherent single-electron packets or with a single electron bunch. Coulomb repulsion is absent under the single-electron condition, thus permitting imaging, diffraction, and spectroscopy, all with high spatiotemporal resolution, the atomic scale (sub-nanometer and femtosecond). The time resolution is limited only by the laser pulse duration and energy carried by the electron packets; the CCD camera has no bearing on the temporal resolution. In the regime of single pulses of electrons, the temporal resolution of picoseconds can be attained when hundreds of electrons are in the bunch. The applications given here are selected to highlight phenomena of different length and time scales, from atomic motions during structural dynamics to phase transitions and nanomechanical oscillations. We conclude with a brief discussion of emerging methods, which include scanning ultrafast electron microscopy (S-UEM), scanning transmission ultrafast electron microscopy (ST-UEM) with convergent beams, and time-resolved imaging of biological structures at ambient conditions with environmental cells.

Correlated Optical Spectroscopy and Transmission Electron Microscopy of Individual Hollow Nanoparticles and their Dimers

PubMed Central

Yang, Linglu; Yan, Bo; Reinhard, Björn M.

2009-01-01

The optical spectra of individual Ag-Au alloy hollow particles were correlated with the particles’ structures obtained by transmission electron microscopy (TEM). The TEM provided direct experimental access to the dimension of the cavity, thickness of the metal shell, and the interparticle distance of hollow particle dimers with high spatial resolution. The analysis of correlated spectral and structural information enabled the quantification of the influence of the core-shell structure on the resonance energy, plasmon lifetime, and plasmon coupling efficiency. Electron beam exposure during TEM inspection was observed to affect plasmon wavelength and lifetime, making optical inspection prior to structural characterization mandatory. PMID:19768108

1D Piezoelectric Material Based Nanogenerators: Methods, Materials and Property Optimization

PubMed Central

Li, Xing; Sun, Mei; Wei, Xianlong; Shan, Chongxin

2018-01-01

Due to the enhanced piezoelectric properties, excellent mechanical properties and tunable electric properties, one-dimensional (1D) piezoelectric materials have shown their promising applications in nanogenerators (NG), sensors, actuators, electronic devices etc. To present a clear view about 1D piezoelectric materials, this review mainly focuses on the characterization and optimization of the piezoelectric properties of 1D nanomaterials, including semiconducting nanowires (NWs) with wurtzite and/or zinc blend phases, perovskite NWs and 1D polymers. Specifically, the piezoelectric coefficients, performance of single NW-based NG and structure-dependent electromechanical properties of 1D nanostructured materials can be respectively investigated through piezoresponse force microscopy, atomic force microscopy and the in-situ scanning/transmission electron microcopy. Along with the introduction of the mechanism and piezoelectric properties of 1D semiconductor, perovskite materials and polymers, their performance improvement strategies are summarized from the view of microstructures, including size-effect, crystal structure, orientation and defects. Finally, the extension of 1D piezoelectric materials in field effect transistors and optoelectronic devices are simply introduced. PMID:29570639

Fabrication and electric measurements of nanostructures inside transmission electron microscope.

PubMed

Chen, Qing; Peng, Lian-Mao

2011-06-01

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

Cross section TEM characterization of high-energy-Xe-irradiated U-Mo

DOE PAGES

Ye, B.; Jamison, L.; Miao, Y.; ...

2017-03-09

U-Mo alloys irradiated with 84 MeV Xe ions to various doses were characterized with transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM) techniques. The TEM thin foils were prepared perpendicular to the irradiated surface to allow a direct observation of the entire region modified by ions. Furthermore, depth-selective microstructural information was revealed. Varied irradiation-induced phenomena such as gas bubble formation, phase reversal, and recrystallization were observed at different ion penetration depths in U-Mo.

A new oxidation based technique for artifact free TEM specimen preparation of nuclear graphite

NASA Astrophysics Data System (ADS)

Johns, Steve; Shin, Wontak; Kane, Joshua J.; Windes, William E.; Ubic, Rick; Karthik, Chinnathambi

2018-07-01

Graphite is a key component in designs of current and future nuclear reactors whose in-service lifetimes are dependent upon the mechanical performance of the graphite. Irradiation damage from fast neutrons creates lattice defects which have a dynamic effect on the microstructure and mechanical properties of graphite. Transmission electron microscopy (TEM) can offer real-time monitoring of the dynamic atomic-level response of graphite subjected to irradiation; however, conventional TEM specimen-preparation techniques, such as argon ion milling itself, damage the graphite specimen and introduce lattice defects. It is impossible to distinguish these defects from the ones created by electron or neutron irradiation. To ensure that TEM specimens are artifact-free, a new oxidation-based technique has been developed. Bulk nuclear grades of graphite (IG-110 and NBG-18) and highly oriented pyrolytic graphite (HOPG) were initially mechanically thinned to ∼60 μm. Discs 3 mm in diameter were then oxidized at temperatures between 575 °C and 625 °C in oxidizing gasses using a new jet-polisher-like set-up in order to achieve optimal oxidation conditions to create self-supporting electron-transparent TEM specimens. The quality of these oxidized specimens were established using optical and electron microscopy. Samples oxidized at 575 °C exhibited large areas of electron transparency and the corresponding lattice imaging showed no apparent damage to the graphite lattice.

A new oxidation based technique for artifact free TEM specimen preparation of nuclear graphite

DOE Office of Scientific and Technical Information (OSTI.GOV)

Johns, Steve; Shin, Wontak; Kane, Joshua J.

Graphite is a key component in designs of current and future nuclear reactors whose in-service lifetimes are dependent upon the mechanical performance of the graphite. Irradiation damage from fast neutrons creates lattice defects which have a dynamic effect on the microstructure and mechanical properties of graphite. Transmission electron microscopy (TEM) can offer real-time monitoring of the dynamic atomic-level response of graphite subjected to irradiation; however, conventional TEM specimen-preparation techniques, such as argon ion milling itself, damage the graphite specimen and introduce lattice defects. It is impossible to distinguish these defects from the ones created by electron or neutron irradiation. Thus,tomore » ensure that TEM specimens are artifact-free, a new oxidation-based technique has been developed. Bulk nuclear grades of graphite (IG-110 and NBG-18) and highly oriented pyrolytic graphite (HOPG) were initially mechanically thinned to ~60μm. Discs 3mm in diameter were then oxidized at temperatures between 575°C and 625°C in oxidizing gasses using a new jet-polisher-like set-up in order to achieve optimal oxidation conditions to create self-supporting electron-transparent TEM specimens. The quality of these oxidized specimens were established using optical and electron microscopy. Samples oxidized at 575°C exhibited large areas of electron transparency and the corresponding lattice imaging showed no apparent damage to the graphite lattice.« less

A new oxidation based technique for artifact free TEM specimen preparation of nuclear graphite

DOE PAGES

Johns, Steve; Shin, Wontak; Kane, Joshua J.; ...

2018-04-03

Graphite is a key component in designs of current and future nuclear reactors whose in-service lifetimes are dependent upon the mechanical performance of the graphite. Irradiation damage from fast neutrons creates lattice defects which have a dynamic effect on the microstructure and mechanical properties of graphite. Transmission electron microscopy (TEM) can offer real-time monitoring of the dynamic atomic-level response of graphite subjected to irradiation; however, conventional TEM specimen-preparation techniques, such as argon ion milling itself, damage the graphite specimen and introduce lattice defects. It is impossible to distinguish these defects from the ones created by electron or neutron irradiation. Thus,tomore » ensure that TEM specimens are artifact-free, a new oxidation-based technique has been developed. Bulk nuclear grades of graphite (IG-110 and NBG-18) and highly oriented pyrolytic graphite (HOPG) were initially mechanically thinned to ~60μm. Discs 3mm in diameter were then oxidized at temperatures between 575°C and 625°C in oxidizing gasses using a new jet-polisher-like set-up in order to achieve optimal oxidation conditions to create self-supporting electron-transparent TEM specimens. The quality of these oxidized specimens were established using optical and electron microscopy. Samples oxidized at 575°C exhibited large areas of electron transparency and the corresponding lattice imaging showed no apparent damage to the graphite lattice.« less

Scanning electron microscopy imaging of dislocations in bulk materials, using electron channeling contrast.

PubMed

Crimp, Martin A

2006-05-01

The imaging and characterization of dislocations is commonly carried out by thin foil transmission electron microscopy (TEM) using diffraction contrast imaging. However, the thin foil approach is limited by difficult sample preparation, thin foil artifacts, relatively small viewable areas, and constraints on carrying out in situ studies. Electron channeling imaging of electron channeling contrast imaging (ECCI) offers an alternative approach for imaging crystalline defects, including dislocations. Because ECCI is carried out with field emission gun scanning electron microscope (FEG-SEM) using bulk specimens, many of the limitations of TEM thin foil analysis are overcome. This paper outlines the development of electron channeling patterns and channeling imaging to the current state of the art. The experimental parameters and set up necessary to carry out routine channeling imaging are reviewed. A number of examples that illustrate some of the advantages of ECCI over thin foil TEM are presented along with a discussion of some of the limitations on carrying out channeling contrast analysis of defect structures. Copyright (c) 2006 Wiley-Liss, Inc.

Focused Ion Beam (FIB) combined with SEM (FIB/SEM) and TEM: Advanced tools for nano-analysis in Geosciences

NASA Astrophysics Data System (ADS)

Wirth, R.; Morales, L. G.

2011-12-01

Focused ion beam (FIB) techniques have been successfully applied to the preparation of site-specific electron transparent membranes for transmission electron microscopy (TEM) investigations in Geosciences since several years. For example, systematic TEM studies of nano-inclusions in diamond foils prepared with FIB have improved our knowledge on diamond formation. However, FIB is not exclusively used for sample preparation for TEM application because it has been proved that one and the same TEM foil can also be used for Synchrotron IR, Synchrotron X-Ray fluorescence (XRF), scanning transmission X-Ray microscopy (STXM) and NanoSIMS analysis. In addition, FIB milling turned out to be very useful for sample preparation of Brillouin scattering experiments and has a strong potential for preparation of highly-polished, micrometer-scale samples. However, a real break through in FIB application was achieved combining a Ga-ion source of the FIB with an electron source of a scanning electron microscope (SEM) in one single instrument. The combination of FIB/SEM renders access to the third dimension of the sample possible. A cavity normal to the sample surface is sputtered with Ga-ions and this newly created inner surface is imaged with the electron beam. Alternating slicing and viewing along these cavities allow the acquisition of a sequence of images that allows the observation in 3 dimensions. Recently, this technique has been successfully applied to image the structure of grain or phase boundaries in metamorphic rocks as well as micro- and nanoporosity in shales, but its applicability goes far beyond these few examples. Combining slicing and viewing with X-Ray and electron backscatter diffraction (EBSD) analysis can provide 3D elemental mapping and 3D crystallographic orientation mapping of crystalline materials. Combined FIB/SEM devices also facilitate the preparation of substantially thinner and cleaner TEM foils (approximately 30 nm) because electron beam imaging controls the progress of the sputtering process without sputtering the sample during imaging. Electron induce sputtering is substantially smaller than ion induced sputtering. Finally, the amorphous layers created by Ga-ion sputtering and Ga-ion implantation can be removed from the foil surfaces by subsequent argon ion bombardment under a low angle of incidence and low acceleration voltage thus permitting TEM high-resolution imaging and electron energy-loss spectroscopy (EELS). Additionally, ultra-thin foils have the advantage that they are electron transparent even at 30 keV, the common operational voltage of a SEM. Therefore the electron column of the FIB/SEM system can be used as a TEM at low voltage and images can be made either in bright-field, dark field and through a high-angle annular dark field (HAADF) detector. The HAADF detector provides information about the chemical composition of the specimen with high spatial resolution because it is Z-contrast sensitive.

GHz laser-free time-resolved transmission electron microscopy: A stroboscopic high-duty-cycle method.

PubMed

Qiu, Jiaqi; Ha, Gwanghui; Jing, Chunguang; Baryshev, Sergey V; Reed, Bryan W; Lau, June W; Zhu, Yimei

2016-02-01

A device and a method for producing ultrashort electron pulses with GHz repetition rates via pulsing an input direct current (dc) electron beam are provided. The device and the method are based on an electromagnetic-mechanical pulser (EMMP) that consists of a series of transverse deflecting cavities and magnetic quadrupoles. The EMMP modulates and chops the incoming dc electron beam and converts it into pico- and sub-pico-second electron pulse sequences (pulse trains) at >1GHz repetition rates, as well as controllably manipulates the resulting pulses. Ultimately, it leads to negligible electron pulse phase-space degradation compared to the incoming dc beam parameters. The temporal pulse length and repetition rate for the EMMP can be continuously tunable over wide ranges. Applying the EMMP to a transmission electron microscope (TEM) with any dc electron source (e.g. thermionic, Schottky, or field-emission source), a GHz stroboscopic high-duty-cycle TEM can be realized. Unlike in many recent developments in time-resolved TEM that rely on a sample pumping laser paired with a laser launching electrons from a photocathode to probe the sample, there is no laser in the presented experimental set-up. This is expected to be a significant relief for electron microscopists who are not familiar with laser systems. The EMMP and the sample are externally driven by a radiofrequency (RF) source synchronized through a delay line. With no laser pumping the sample, the problem of the pump laser induced residual heating/damaging the sample is eliminated. As many RF-driven processes can be cycled indefinitely, sampling rates of 1-50GHz become accessible. Such a GHz stroboscopic TEM would open up a new paradigm for in situ and in operando experiments to study samples externally driven electromagnetically. Complementary to the lower (MHz) repetition rates experiments enabled by laser photocathode TEM, new experiments in the multi-GHz regime will be enabled by the proposed RF design. Because TEM is also a platform for various analytical methods, there are infinite application opportunities in energy and electronics to resolve charge (electronic and ionic) transport, and magnetic, plasmonic and excitonic dynamics in advanced functional materials. In addition, because the beam duty-cycle can be as high as ~10(-1) (or 10%), detection can be accomplished by commercially available detectors. In this article, we report an optimal design of the EMMP. The optimal design was found using an analytical generalized matrix approach in the thin lens approximation along with detailed beam dynamics taking actual realistic dc beam parameters in a TEM operating at 200keV. Copyright © 2015 Elsevier B.V. All rights reserved.

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

PubMed Central

Bittencourt, Carla; Van Tendeloo, Gustaaf

2015-01-01

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

Nanoparticle Immobilization for Controllable Experiments in Liquid-Cell Transmission Electron Microscopy.

PubMed

Robertson, Alex W; Zhu, Guomin; Mehdi, B Layla; Jacobs, Robert M J; De Yoreo, James; Browning, Nigel D

2018-06-22

We demonstrate that silanization can control the adhesion of nanostructures to the SiN windows compatible with liquid-cell transmission electron microscopy (LC-TEM). Formation of an (3-aminopropyl)triethoxysilane (APTES) self-assembled monolayer on a SiN window, producing a surface decorated with amino groups, permits strong adhesion of Au nanoparticles to the window. Many of these nanoparticles remain static, undergoing minimal translation or rotation during LC-TEM up to high electron beam current densities due to the strong interaction between the APTES amino group and Au. We then use this technique to perform a direct comparative LC-TEM study on the behavior of ligand and nonligand-coated Au nanoparticles in a Au growth solution. While the ligand coated nanoparticles remain consistent even under high electron beam current densities, the naked nanoparticles acted as sites for secondary Au nucleation. These nucleated particles decorated the parent nanoparticle surface, forming consecutive monolayer assemblies of ∼2 nm diameter nanoparticles, which sinter into the parent particle when the electron beam was shut off. This method for facile immobilization of nanostructures for LC-TEM study will permit more sophisticated and controlled in situ experiments into the properties of solid-liquid interfaces in the future.

Operando observations of solid-state electrochemical reactions in Li-ion batteries by spatially resolved TEM EELS and electron holography.

PubMed

Yamamoto, Kazuo; Iriyama, Yasutoshi; Hirayama, Tsukasa

2017-02-08

All-solid-state Li-ion batteries having incombustible solid electrolytes are promising energy storage devices because they have significant advantages in terms of safety, lifetime and energy density. Electrochemical reactions, namely, Li-ion insertion/extraction reactions, commonly occur around the nanometer-scale interfaces between the electrodes and solid electrolytes. Thus, transmission electron microscopy (TEM) is an appropriate technique to directly observe such reactions, providing important information for understanding the fundamental solid-state electrochemistry and improving battery performance. In this review, we introduce two types of TEM techniques for operando observations of battery reactions, spatially resolved electron energy-loss spectroscopy in a TEM mode for direct detection of the Li concentration profiles and electron holography for observing the electric potential changes due to Li-ion insertion/extraction reactions. We visually show how Li-ion insertion/extractions affect the crystal structures, electronic structures, and local electric potential during the charge-discharge processes in these batteries. © 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.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Buck, E.C.; Dietz, N.L.; Bates, J.K.

Uranium contaminated soils from the Fernald Operation Site, Ohio, have been examined by a combination of optical microscopy, scanning electron microscopy with backscattered electron detection (SEM/BSE), and analytical electron microscopy (AEM). A method is described for preparing of transmission electron microscopy (TEM) thin sections by ultramicrotomy. By using these thin sections, SEM and TEM images can be compared directly. Uranium was found in iron oxides, silicates (soddyite), phosphates (autunites), and fluorite. Little uranium was associated with clays. The distribution of uranium phases was found to be inhomogeneous at the microscopic level.

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

PubMed

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

2018-04-01

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

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Moser, Trevor H.; Mehta, Hardeep; Park, Chiwoo

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

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Moser, Trevor H.; Mehta, Hardeep; Park, Chiwoo

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

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

PubMed Central

Mehta, Hardeep

2018-01-01

In situ liquid cell transmission electron microscopy (LC-TEM) allows dynamic nanoscale characterization of systems in a hydrated state. Although powerful, this technique remains impaired by issues of repeatability that limit experimental fidelity and hinder the identification and control of some variables underlying observed dynamics. We detail new LC-TEM devices that improve experimental reproducibility by expanding available imaging area and providing a platform for investigating electron flux history on the sample. Irradiation history is an important factor influencing LC-TEM results that has, to this point, been largely qualitatively and not quantitatively described. We use these devices to highlight the role of cumulative electron flux history on samples from both nanoparticle growth and biological imaging experiments and demonstrate capture of time zero, low-dose images on beam-sensitive samples. In particular, the ability to capture pristine images of biological samples, where the acquired image is the first time that the cell experiences significant electron flux, allowed us to determine that nanoparticle movement compared to the cell membrane was a function of cell damage and therefore an artifact rather than visualizing cell dynamics in action. These results highlight just a subset of the new science that is accessible with LC-TEM through the new multiwindow devices with patterned focusing aides. PMID:29725619

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

DOE PAGES

Moser, Trevor H.; Mehta, Hardeep; Park, Chiwoo; ...

2018-04-20

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

Microstructural studies of 35 degrees C copper Ni-Ti orthodontic wire and TEM confirmation of low-temperature martensite transformation.

PubMed

Brantley, William A; Guo, Wenhua; Clark, William A T; Iijima, Masahiro

2008-02-01

Previous temperature-modulated differential scanning calorimetry (TMDSC) study of nickel-titanium orthodontic wires revealed a large exothermic low-temperature peak that was attributed to transformation within martensitic NiTi. The purpose of this study was to use transmission electron microscopy (TEM) to verify this phase transformation in a clinically popular nickel-titanium wire, identify its mechanism and confirm other phase transformations found by TMDSC, and to provide detailed information about the microstructure of this wire. The 35 degrees C Copper nickel-titanium wire (Ormco) with cross-section dimensions of 0.016 in. x 0.022 in. used in the earlier TMDSC investigation was selected. Foils were prepared for TEM analyses by mechanical grinding, polishing, dimpling, ion milling and plasma cleaning. Standard bright-field and dark-field TEM images were obtained, along with convergent-beam electron diffraction patterns. A cryo-stage with the electron microscope (Phillips CM 200) permitted the specimen to be observed at -187, -45, and 50 degrees C, as well as at room temperature. Microstructures were also observed with an optical microscope and a scanning electron microscope. Room temperature microstructures had randomly oriented, elongated grains that were twinned. Electron diffraction patterns confirmed that phase transformations took place over temperature ranges previously found by TMDSC. TEM observations revealed a high dislocation density and fine-scale oxide particles, and that twinning is the mechanism for the low-temperature transformation in martensitic NiTi. TEM confirmed the low-temperature peak and other phase transformations observed by TMDSC, and revealed that twinning in martensite is the mechanism for the low-temperature peak. The high dislocation density and fine-scale oxide particles in the microstructure are the result of the wire manufacturing process.

Cryo-electron microscopy and cryo-electron tomography of nanoparticles.

PubMed

Stewart, Phoebe L

2017-03-01

Cryo-transmission electron microscopy (cryo-TEM or cryo-EM) and cryo-electron tomography (cryo-ET) offer robust and powerful ways to visualize nanoparticles. These techniques involve imaging of the sample in a frozen-hydrated state, allowing visualization of nanoparticles essentially as they exist in solution. Cryo-TEM grid preparation can be performed with the sample in aqueous solvents or in various organic and ionic solvents. Two-dimensional (2D) cryo-TEM provides a direct way to visualize the polydispersity within a nanoparticle preparation. Fourier transforms of cryo-TEM images can confirm the structural periodicity within a sample. While measurement of specimen parameters can be performed with 2D TEM images, determination of a three-dimensional (3D) structure often facilitates more spatially accurate quantization. 3D structures can be determined in one of two ways. If the nanoparticle has a homogeneous structure, then 2D projection images of different particles can be averaged using a computational process referred to as single particle reconstruction. Alternatively, if the nanoparticle has a heterogeneous structure, then a structure can be generated by cryo-ET. This involves collecting a tilt-series of 2D projection images for a defined region of the grid, which can be used to generate a 3D tomogram. Occasionally it is advantageous to calculate both a single particle reconstruction, to reveal the regular portions of a nanoparticle structure, and a cryo-electron tomogram, to reveal the irregular features. A sampling of 2D cryo-TEM images and 3D structures are presented for protein based, DNA based, lipid based, and polymer based nanoparticles. WIREs Nanomed Nanobiotechnol 2017, 9:e1417. doi: 10.1002/wnan.1417 For further resources related to this article, please visit the WIREs website. © 2016 Wiley Periodicals, Inc.

Characterization of microbially Fe(III)-reduced nontronite: Environmental cell-transmission electron microscopy study

USGS Publications Warehouse

Kim, Jin-wook; Furukawa, Yoko; Daulton, Tyrone L.; Lavoie, Dawn L.; Newell, Steven W.

2003-01-01

Microstructural changes induced by the microbial reduction of Fe(III) in nontronite by Shewanella oneidensis were studied using environmental cell (EC)-transmission electron microscopy (TEM), conventional TEM, and X-ray powder diffraction (XRD). Direct observations of clays by EC-TEM in their hydrated state allowed for the first time an accurate and unambiguous TEM measurement of basal layer spacings and the contraction of layer spacing caused by microbial effects, most likely those of Fe(III) reduction. Non-reduced and Fe(III)-reduced nontronite, observed by EC-TEM, exhibited fringes with mean d001 spacings of 1.50 nm (standard deviation, σ = 0.08 nm) and 1.26 nm (σ = 0.10 nm), respectively. In comparison, the same samples embedded with Nanoplast resin, sectioned by microtome, and observed using conventional TEM, displayed layer spacings of 1.0–1.1 nm (non-reduced) and 1.0 nm (reduced). The results from Nanoplast-embedded samples are typical of conventional TEM studies, which have measured nearly identical layer spacings regardless of Fe oxidation state. Following Fe(III) reduction, both EC- and conventional TEM showed an increase in the order of nontronite selected area electron diffraction patterns while the images exhibited fewer wavy fringes and fewer layer terminations. An increase in stacking order in reduced nontronite was also suggested by XRD measurements. In particular, the ratio of the valley to peak intensity (v/p) of the 1.7 nm basal 001 peak of ethylene glycolated nontronite was measured at 0.65 (non-reduced) and 0.85 (microbially reduced).

Transmission/Scanning Transmission Electron Microscopy | Materials Science

Science.gov Websites

imaging such as high resolution TEM. Transmission electron diffraction patterns help to determine the microstructure of a material and its defects. Phase-contrast imaging or high-resolution (HR) TEM imaging gives high scattering angle can be collected to form high-resolution, chemically sensitive, atomic number (Z

Chemical Reactions of Molecules Promoted and Simultaneously Imaged by the Electron Beam in Transmission Electron Microscopy.

PubMed

Skowron, Stephen T; Chamberlain, Thomas W; Biskupek, Johannes; Kaiser, Ute; Besley, Elena; Khlobystov, Andrei N

2017-08-15

The main objective of this Account is to assess the challenges of transmission electron microscopy (TEM) of molecules, based on over 15 years of our work in this field, and to outline the opportunities in studying chemical reactions under the electron beam (e-beam). During TEM imaging of an individual molecule adsorbed on an atomically thin substrate, such as graphene or a carbon nanotube, the e-beam transfers kinetic energy to atoms of the molecule, displacing them from equilibrium positions. Impact of the e-beam triggers bond dissociation and various chemical reactions which can be imaged concurrently with their activation by the e-beam and can be presented as stop-frame movies. This experimental approach, which we term ChemTEM, harnesses energy transferred from the e-beam to the molecule via direct interactions with the atomic nuclei, enabling accurate predictions of bond dissociation events and control of the type and rate of chemical reactions. Elemental composition and structure of the reactant molecules as well as the operating conditions of TEM (particularly the energy of the e-beam) determine the product formed in ChemTEM processes, while the e-beam dose rate controls the reaction rate. Because the e-beam of TEM acts simultaneously as a source of energy for the reaction and as an imaging tool monitoring the same reaction, ChemTEM reveals atomic-level chemical information, such as pathways of reactions imaged for individual molecules, step-by-step and in real time; structures of illusive reaction intermediates; and direct comparison of catalytic activity of different transition metals filmed with atomic resolution. Chemical transformations in ChemTEM often lead to previously unforeseen products, demonstrating the potential of this method to become not only an analytical tool for studying reactions, but also a powerful instrument for discovery of materials that can be synthesized on preparative scale.

Transmission electron microscopy of polymer blends and block copolymers

NASA Astrophysics Data System (ADS)

Gomez, Enrique Daniel

Transmission electron microscopy (TEM) of soft matter is a field that warrants further investigation. Developments in sample preparation, imaging and spectroscopic techniques could lead to novel experiments that may further our understanding of the structure and the role structure plays in the functionality of various organic materials. Unlike most hard materials, TEM of organic molecules is limited by the amount of radiation damage the material can withstand without changing its structure. Despite this limitation, TEM has been and will be a powerful tool to study polymeric materials and other soft matter. In this dissertation, an introduction of TEM for polymer scientists is presented. The fundamentals of interactions of electrons with matter are described using the Schrodinger wave equation and scattering cross-sections to fully encompass coherent and incoherent scattering. The intensity, which is the product of the wave function and its complex conjugate, shows no perceptible change due to the sample. Instead, contrast is generated through the optical system of the microscope by removing scattered electrons or by generating interference due to material-induced phase changes. Perhaps the most challenging aspect of taking TEM images, however, is sample preparation, because TEM experiments require materials with approximately 50 nm thickness. Although ultramicrotomy is a well-established powerful tool for preparing biological and polymeric sections for TEM, the development of cryogenic Focused Ion Beam may enable unprecedented cross-sectional TEM studies of polymer thin films on arbitrary substrates with nanometer precision. Two examples of TEM experiments of polymeric materials are presented. The first involves quantifying the composition profile across a lamellar phase obtained in a multicomponent blend of saturated poly(butadiene) and poly(isobutylene), stabilized by a saturated poly(butadiene) copolymer serving as a surfactant, using TEM and self-consistent field theory (SCFT). The liquid-like nature of this system at room temperature makes traditional staining methods for the enhancement of contrast ineffective. As an alternative, we take advantage of the large inelastic scattering cross-section of soft materials to generate contrast in zero-loss TEM images. Independent spatially resolved thickness measurements enable quantification of electron scattering. This enabled a comparison between the TEM data and predictions based on SCFT without any adjustable parameters. The second example involves the utilization of energy-filtered transmission electron microscopy (EFTEM) to compute elemental maps by taking advantage of ionization events. Elemental mapping of lithium is used to determine the distribution of salt in nanostructured poly(styrene-block-ethylene oxide) (SEO) copolymer/lithium salt electrolytes. Surprisingly, the concentration of lithium within a poly(ethylene oxide) (PEO) domain is found to be inhomogeneous; the salt is localized to the middle of the channels. Self-consistent field theory simulations suggest that localization of lithium is due to chain stretching at the interface, which increases with molecular weight. EFTEM and SCFT results show that the segregation of lithium salt to the middle of the PEO lamellae is greater for higher molecular weight polymers. This is correlated with the ionic conductivity of the copolymer electrolyte, which is found to show a higher conductivity for thinner lithium lamellae.

Transmission Electron Microscopy of Vacuum Sensitive, Radiation Sensitive, and Structurally Delicate Materials

NASA Astrophysics Data System (ADS)

Levin, Barnaby

The transmission electron microscope (TEM) is a powerful tool for characterizing the nanoscale and atomic structure of materials, offering insights into their fundamental physical properties. However, TEM characterization requires very thin samples of material to be placed in a high vacuum environment, and exposed to electron radiation. The high vacuum will induce some materials to evaporate or sublimate, preventing them from being accurately characterized, radiation may damage the sample, causing mass loss, or altering its structure, and structurally delicate samples may collapse and break apart when they are thinned for TEM imaging. This dissertation discusses three different projects in which each of these three difficulties pose challenges to TEM characterization of samples. Firstly, we outline strategies for minimizing radiation damage when characterizing materials in TEM at atomic resolution. We consider types of radiation damage, such as vacancy enhanced displacement, that are not included in some previous discussions of beam damage, and we consider how to minimize damage when using new imaging techniques such as annular bright-field scanning TEM. Our methodology emphasizes the general principle that variation of both signal strength and damage cross section must be considered when choosing an experimental electron beam voltage to minimize damage. Secondly, we consider samples containing sulfur, which is prone to sublimation in high vacuum. TEM is routinely used to attempt to characterize the sulfur distribution in lithium-sulfur battery electrodes, but sublimation artifacts can give misleading results. We demonstrate that sulfur sublimation can be suppressed by using cryogenic TEM to characterize sulfur at very low temperatures, or by using the recently developed airSEM to characterize sulfur without exposing it to vacuum. Finally, we discuss the characterization of aging cadmium yellow paint from early 20th century art masterpieces. The binding medium holding paint particles together bends and curls as sample thickness is reduced to 100 nm, making high resolution characterization challenging. We acquire lattice resolution images of the pigment particles through the binder using high voltage zero-loss energy filtered TEM, allowing us to measure the pigment particle size and determine the pigment crystal structure, providing insight into why the paint is aging and how it was synthesized.

Retrofit implementation of Zernike phase plate imaging for cryo-TEM

PubMed Central

Marko, Michael; Leith, ArDean; Hsieh, Chyongere; Danev, Radostin

2011-01-01

In-focus phase-plate imaging is particularly beneficial for cryo-TEM because it offers a substantial overall increase in image contrast, without an electron dose penalty, and it simplifies image interpretation. We show how phase-plate cryo-TEM can be implemented with an appropriate existing TEM, and provide a basic practical introduction to use of thin-film (carbon) phase plates. We point out potential pitfalls of phase-plate operation, and discuss solutions. We provide information on evaluating a particular TEM for its suitability. PMID:21272647

An electron energy loss spectrometer based streak camera for time resolved TEM measurements.

PubMed

Ali, Hasan; Eriksson, Johan; Li, Hu; Jafri, S Hassan M; Kumar, M S Sharath; Ögren, Jim; Ziemann, Volker; Leifer, Klaus

2017-05-01

We propose an experimental setup based on a streak camera approach inside an energy filter to measure time resolved properties of materials in the transmission electron microscope (TEM). In order to put in place the streak camera, a beam sweeper was built inside an energy filter. After exciting the TEM sample, the beam is swept across the CCD camera of the filter. We describe different parts of the setup at the example of a magnetic measurement. This setup is capable to acquire time resolved diffraction patterns, electron energy loss spectra (EELS) and images with total streaking times in the range between 100ns and 10μs. Copyright © 2016 Elsevier B.V. All rights reserved.

Amorphization induced by focused ion beam milling in metallic and electronic materials.

PubMed

Huh, Yoon; Hong, Ki Jung; Shin, Kwang Soo

2013-08-01

Focused ion beam (FIB) milling using high-energy gallium ions is widely used in the preparation of specimens for transmission electron microscopy (TEM). However, the energetic ion beam induces amorphization on the edge of specimens during milling, resulting in a mischievous influence on the clearness of high-quality transmission electron micrographs. In this work, the amorphization induced by the FIB milling was investigated by TEM for three kinds of materials, metallic materials in bulk shape, and semiconductive and electronic ceramic materials as a substrate for the deposition of thin films.

Using transmission electron microscopy and 3View® to determine collagen fibril size and three-dimensional organization

PubMed Central

Mironov, Aleksandr; Cootes, Timothy F.; Holmes, David F.; Kadler, Karl E.

2017-01-01

Collagen fibrils are the major tensile element in vertebrate tissues where they occur as ordered bundles in the extracellular matrix. Abnormal fibril assembly and organization results in scarring, fibrosis, poor wound healing and connective tissue diseases. Transmission electron microscopy (TEM) is used to assess formation of the fibrils, predominantly by measuring fibril diameter. Here we describe an enhanced protocol for measuring fibril diameter as well as fibril-volume-fraction, mean fibril length, fibril cross-sectional shape, and fibril 3D organization that are also major determinants of tissue function. Serial section TEM (ssTEM) has been used to visualize fibril 3D-organization in vivo. However, serial block face-scanning electron microscopy (SBF-SEM) has emerged as a time-efficient alternative to ssTEM. The protocol described below is suitable for preparing tissues for TEM and SBF-SEM (by 3View®). We demonstrate the power of 3View® for studying collagen fibril organization in vivo and show how to find and track individual fibrils. Time scale: ~8 days from isolating the tissue to having a 3D image stack. PMID:23807286

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

PubMed

Chen, Xin; Li, Chang; Cao, Hongling

2015-03-21

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

Properties of ion temperature gradient and trapped electron modes in tokamak plasmas with inverted density profiles

NASA Astrophysics Data System (ADS)

Du, Huarong; Jhang, Hogun; Hahm, T. S.; Dong, J. Q.; Wang, Z. X.

2017-12-01

We perform a numerical study of linear stability of the ion temperature gradient (ITG) mode and the trapped electron mode (TEM) in tokamak plasmas with inverted density profiles. A local gyrokinetic integral equation is applied for this study. From comprehensive parametric scans, we obtain stability diagrams for ITG modes and TEMs in terms of density and temperature gradient scale lengths. The results show that, for the inverted density profile, there exists a normalized threshold temperature gradient above which the ITG mode and the TEM are either separately or simultaneously unstable. The instability threshold of the TEM for the inverted density profile is substantially different from that for normal and flat density profiles. In addition, deviations are found on the ITG threshold from an early analytic theory in sheared slab geometry with the adiabatic electron response [T. S. Hahm and W. M. Tang, Phys. Fluids B 1, 1185 (1989)]. A possible implication of this work on particle transport in pellet fueled tokamak plasmas is discussed.

Demonstration of correlative atomic force and transmission electron microscopy using actin cytoskeleton

PubMed Central

Yamada, Yutaro; Konno, Hiroki; Shimabukuro, Katsuya

2017-01-01

In this study, we present a new technique called correlative atomic force and transmission electron microscopy (correlative AFM/TEM) in which a targeted region of a sample can be observed under AFM and TEM. The ultimate goal of developing this new technique is to provide a technical platform to expand the fields of AFM application to complex biological systems such as cell extracts. Recent advances in the time resolution of AFM have enabled detailed observation of the dynamic nature of biomolecules. However, specifying molecular species, by AFM alone, remains a challenge. Here, we demonstrate correlative AFM/TEM, using actin filaments as a test sample, and further show that immuno-electron microscopy (immuno-EM), to specify molecules, can be integrated into this technique. Therefore, it is now possible to specify molecules, captured under AFM, by subsequent observation using immuno-EM. In conclusion, correlative AFM/TEM can be a versatile method to investigate complex biological systems at the molecular level. PMID:28828286

Nano Electronics on Atomically Controlled van der Waals Quantum Heterostructures

DTIC Science & Technology

2015-03-30

for the structural of the atomically sharp interface between hBN and Bi2Te3. Finally, we have developed unprecedentedly clean graphene supercoductor...crystals by MBE method. We also use transmission electron microscopy (TEM) analysis for the structural of the atomically sharp interface between hBN and...by MBE method. We also use transmission electron microscopy (TEM) analysis for the structural of the atomically sharp interface between hBN and Bi2Te3

Imaging plasmodesmata with high-resolution scanning electron microscopy.

PubMed

Barton, Deborah A; Overall, Robyn L

2015-01-01

High-resolution scanning electron microscopy (HRSEM) is an effective tool to investigate the distribution of plasmodesmata within plant cell walls as well as to probe their complex, three-dimensional architecture. It is a useful alternative to traditional transmission electron microscopy (TEM) in which plasmodesmata are sectioned to reveal their internal substructures. Benefits of adopting an HRSEM approach to studies of plasmodesmata are that the specimen preparation methods are less complex and time consuming than for TEM, many plasmodesmata within a large region of tissue can be imaged in a single session, and three-dimensional information is readily available without the need for reconstructing TEM serial sections or employing transmission electron tomography, both of which are lengthy processes. Here we describe methods to prepare plant samples for HRSEM using pre- or postfixation extraction of cellular material in order to visualize plasmodesmata embedded within plant cell walls.

Unravelling surface and interfacial structures of a metal-organic framework by transmission electron microscopy.

PubMed

Zhu, Yihan; Ciston, Jim; Zheng, Bin; Miao, Xiaohe; Czarnik, Cory; Pan, Yichang; Sougrat, Rachid; Lai, Zhiping; Hsiung, Chia-En; Yao, Kexin; Pinnau, Ingo; Pan, Ming; Han, Yu

2017-05-01

Metal-organic frameworks (MOFs) are crystalline porous materials with designable topology, porosity and functionality, having promising applications in gas storage and separation, ion conduction and catalysis. It is challenging to observe MOFs with transmission electron microscopy (TEM) due to the extreme instability of MOFs upon electron beam irradiation. Here, we use a direct-detection electron-counting camera to acquire TEM images of the MOF ZIF-8 with an ultralow dose of 4.1 electrons per square ångström to retain the structural integrity. The obtained image involves structural information transferred up to 2.1 Å, allowing the resolution of individual atomic columns of Zn and organic linkers in the framework. Furthermore, TEM reveals important local structural features of ZIF-8 crystals that cannot be identified by diffraction techniques, including armchair-type surface terminations and coherent interfaces between assembled crystals. These observations allow us to understand how ZIF-8 crystals self-assemble and the subsequent influence of interfacial cavities on mass transport of guest molecules.

Unravelling surface and interfacial structures of a metal-organic framework by transmission electron microscopy

NASA Astrophysics Data System (ADS)

Zhu, Yihan; Ciston, Jim; Zheng, Bin; Miao, Xiaohe; Czarnik, Cory; Pan, Yichang; Sougrat, Rachid; Lai, Zhiping; Hsiung, Chia-En; Yao, Kexin; Pinnau, Ingo; Pan, Ming; Han, Yu

2017-05-01

Metal-organic frameworks (MOFs) are crystalline porous materials with designable topology, porosity and functionality, having promising applications in gas storage and separation, ion conduction and catalysis. It is challenging to observe MOFs with transmission electron microscopy (TEM) due to the extreme instability of MOFs upon electron beam irradiation. Here, we use a direct-detection electron-counting camera to acquire TEM images of the MOF ZIF-8 with an ultralow dose of 4.1 electrons per square ångström to retain the structural integrity. The obtained image involves structural information transferred up to 2.1 Å, allowing the resolution of individual atomic columns of Zn and organic linkers in the framework. Furthermore, TEM reveals important local structural features of ZIF-8 crystals that cannot be identified by diffraction techniques, including armchair-type surface terminations and coherent interfaces between assembled crystals. These observations allow us to understand how ZIF-8 crystals self-assemble and the subsequent influence of interfacial cavities on mass transport of guest molecules.

A simple approach to characterizing block copolymer assemblies: graphene oxide supports for high contrast multi-technique imaging†

PubMed Central

Patterson, Joseph P.; Sanchez, Ana M.; Petzetakis, Nikos; Smart, Thomas P.; Epps, Thomas H.; Portman, Ian

2013-01-01

Block copolymers are well-known to self-assemble into a range of 3-dimensional morphologies. However, due to their nanoscale dimensions, resolving their exact structure can be a challenge. Transmission electron microscopy (TEM) is a powerful technique for achieving this, but for polymeric assemblies chemical fixing/staining techniques are usually required to increase image contrast and protect specimens from electron beam damage. Graphene oxide (GO) is a robust, water-dispersable, and nearly electron transparent membrane: an ideal support for TEM. We show that when using GO supports no stains are required to acquire high contrast TEM images and that the specimens remain stable under the electron beam for long periods, allowing sample analysis by a range of electron microscopy techniques. GO supports are also used for further characterization of assemblies by atomic force microscopy. The simplicity of sample preparation and analysis, as well as the potential for significantly increased contrast background, make GO supports an attractive alternative for the analysis of block copolymer assemblies. PMID:24049544

Recent advances in electron tomography: TEM and HAADF-STEM tomography for materials science and semiconductor applications.

PubMed

Kübel, Christian; Voigt, Andreas; Schoenmakers, Remco; Otten, Max; Su, David; Lee, Tan-Chen; Carlsson, Anna; Bradley, John

2005-10-01

Electron tomography is a well-established technique for three-dimensional structure determination of (almost) amorphous specimens in life sciences applications. With the recent advances in nanotechnology and the semiconductor industry, there is also an increasing need for high-resolution three-dimensional (3D) structural information in physical sciences. In this article, we evaluate the capabilities and limitations of transmission electron microscopy (TEM) and high-angle-annular-dark-field scanning transmission electron microscopy (HAADF-STEM) tomography for the 3D structural characterization of partially crystalline to highly crystalline materials. Our analysis of catalysts, a hydrogen storage material, and different semiconductor devices shows that features with a diameter as small as 1-2 nm can be resolved in three dimensions by electron tomography. For partially crystalline materials with small single crystalline domains, bright-field TEM tomography provides reliable 3D structural information. HAADF-STEM tomography is more versatile and can also be used for high-resolution 3D imaging of highly crystalline materials such as semiconductor devices.

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

PubMed

Massover, William H

2011-02-01

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

Theory of the spatial resolution of (scanning) transmission electron microscopy in liquid water or ice layers.

PubMed

de Jonge, Niels

2018-04-01

The sample dependent spatial resolution was calculated for transmission electron microscopy (TEM) and scanning TEM (STEM) of objects (e.g., nanoparticles, proteins) embedded in a layer of liquid water or amorphous ice. The theoretical model includes elastic- and inelastic scattering, beam broadening, and chromatic aberration. Different contrast mechanisms were evaluated as function of the electron dose, the detection angle, and the sample configuration. It was found that the spatial resolution scales with the electron dose to the -1/4th power. Gold- and carbon nanoparticles were examined in the middle of water layers ranging from 0.01--10 µm thickness representing relevant classes of experiments in both materials science and biology. The optimal microscope settings differ between experimental configurations. STEM performs the best for gold nanoparticles for all layer thicknesses, while carbon is best imaged with phase-contrast TEM for thin layers but bright field STEM is preferred for thicker layers. The resolution was also calculated for a water layer enclosed between thin membranes. The influence of chromatic aberration correction for TEM was examined as well. The theory is broadly applicable to other types of materials and sample configurations. Copyright © 2018 Elsevier B.V. All rights reserved.

Retrofit implementation of Zernike phase plate imaging for cryo-TEM.

PubMed

Marko, Michael; Leith, Ardean; Hsieh, Chyongere; Danev, Radostin

2011-05-01

In-focus phase-plate imaging is particularly beneficial for cryo-TEM because it offers a substantial overall increase in image contrast, without an electron dose penalty, and it simplifies image interpretation. We show how phase-plate cryo-TEM can be implemented with an appropriate existing TEM, and provide a basic practical introduction to use of thin-film (carbon) phase plates. We point out potential pitfalls of phase-plate operation, and discuss solutions. We provide information on evaluating a particular TEM for its suitability. Copyright © 2011 Elsevier Inc. All rights reserved.

Electron energy loss spectroscopy techniques for the study of microbial chromium(VI) reduction

NASA Technical Reports Server (NTRS)

Daulton, Tyrone L.; Little, Brenda J.; Lowe, Kristine; Jones-Meehan, Joanne

2002-01-01

Electron energy loss spectroscopy (EELS) techniques were used to determine oxidation state, at high spatial resolution, of chromium associated with the metal-reducing bacteria, Shewanella oneidensis, in anaerobic cultures containing Cr(VI)O4(2-). These techniques were applied to fixed cells examined in thin section by conventional transmission electron microscopy (TEM) as well as unfixed, hydrated bacteria examined by environmental cell (EC)-TEM. Two distinct populations of bacteria were observed by TEM: bacteria exhibiting low image contrast and bacteria exhibiting high contrast in their cell membrane (or boundary) structure which was often encrusted with high-contrast precipitates. Measurements by EELS demonstrated that cell boundaries became saturated with low concentrations of Cr and the precipitates encrusting bacterial cells contained a reduced form of Cr in oxidation state + 3 or lower.

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

PubMed

Sakalli, Y; Trettin, R

2017-07-01

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

Using Graphene Liquid Cell Transmission Electron Microscopy to Study in Situ Nanocrystal Etching.

PubMed

Hauwiller, Matthew R; Ondry, Justin C; Alivisatos, A Paul

2018-05-17

Graphene liquid cell electron microscopy provides the ability to observe nanoscale chemical transformations and dynamics as the reactions are occurring in liquid environments. This manuscript describes the process for making graphene liquid cells through the example of graphene liquid cell transmission electron microscopy (TEM) experiments of gold nanocrystal etching. The protocol for making graphene liquid cells involves coating gold, holey-carbon TEM grids with chemical vapor deposition graphene and then using those graphene-coated grids to encapsulate liquid between two graphene surfaces. These pockets of liquid, with the nanomaterial of interest, are imaged in the electron microscope to see the dynamics of the nanoscale process, in this case the oxidative etching of gold nanorods. By controlling the electron beam dose rate, which modulates the etching species in the liquid cell, the underlying mechanisms of how atoms are removed from nanocrystals to form different facets and shapes can be better understood. Graphene liquid cell TEM has the advantages of high spatial resolution, compatibility with traditional TEM holders, and low start-up costs for research groups. Current limitations include delicate sample preparation, lack of flow capability, and reliance on electron beam-generated radiolysis products to induce reactions. With further development and control, graphene liquid cell may become a ubiquitous technique in nanomaterials and biology, and is already being used to study mechanisms governing growth, etching, and self-assembly processes of nanomaterials in liquid on the single particle level.

TEM-nanoindentation studies of semiconducting structures.

PubMed

Le Bourhis, E; Patriarche, G

2007-01-01

This paper reviews the application of nanoindentation coupled with transmission electron microscopy (TEM) to investigations of the plastic behaviour of semiconducting structures and its implication for device design. Instrumented nanoindentation has been developed to extract the mechanical behaviour of small volumes scaled to those encountered in semiconductor heterostructures. We illustrate that TEM is a powerful complementary tool for the study of local plasticity induced by nanoindentation. TEM-nanoindentation allows for detailed understanding of the plastic deformation in semiconducting structures and opens practical routes for improvement of devices. Performances of heterostructures are deteriously affected by dislocations that relax the lattice mismatched layers. Different ways to obtain compliant substructures are being developed in order to concentrate the plastic relaxation underneath the heterostructure. Such approaches allow for mechanical design of micro- and opto-electronic devices to be considered throughout the fabrication process.

TEM Analysis of Diffusion-Bonded Silicon Carbide Ceramics Joined Using Metallic Interlayers

NASA Technical Reports Server (NTRS)

Ozaki, T.; Hasegawa, Y.; Tsuda, H.; Mori, S.; Halbig, M. C.; Asthana, R.; Singh, M.

2017-01-01

SiC fiber-bonded ceramics (SA-Tyrannohex: SA-THX) diffusion-bonded with TiCu metallic interlayers were investigated. Thin samples of the ceramics were prepared with a focused ion beam (FIB) and the interfacial microstructure of the prepared samples was studied by transmission electron microscopy (TEM) and scanning TEM (STEM). In addition to conventional microstructure observation, for detailed analysis of reaction compounds in diffusion-bonded area, we performed STEM-EDS measurements and selected area electron diffraction (SAD) experiments. The TEM and STEM experiments revealed the diffusion-bonded area was composed of only one reaction layer, which was characterized by TiC precipitates in Cu-Si compound matrix. This reaction layer was in good contact with the SA-THX substrates, and it is concluded that the joint structure led to the excellent bonding strength.

Atom-counting in High Resolution Electron Microscopy:TEM or STEM - That's the question.

PubMed

Gonnissen, J; De Backer, A; den Dekker, A J; Sijbers, J; Van Aert, S

2017-03-01

In this work, a recently developed quantitative approach based on the principles of detection theory is used in order to determine the possibilities and limitations of High Resolution Scanning Transmission Electron Microscopy (HR STEM) and HR TEM for atom-counting. So far, HR STEM has been shown to be an appropriate imaging mode to count the number of atoms in a projected atomic column. Recently, it has been demonstrated that HR TEM, when using negative spherical aberration imaging, is suitable for atom-counting as well. The capabilities of both imaging techniques are investigated and compared using the probability of error as a criterion. It is shown that for the same incoming electron dose, HR STEM outperforms HR TEM under common practice standards, i.e. when the decision is based on the probability function of the peak intensities in HR TEM and of the scattering cross-sections in HR STEM. If the atom-counting decision is based on the joint probability function of the image pixel values, the dependence of all image pixel intensities as a function of thickness should be known accurately. Under this assumption, the probability of error may decrease significantly for atom-counting in HR TEM and may, in theory, become lower as compared to HR STEM under the predicted optimal experimental settings. However, the commonly used standard for atom-counting in HR STEM leads to a high performance and has been shown to work in practice. Copyright © 2017 Elsevier B.V. All rights reserved.

Scanning EM of non-heavy metal stained biosamples: Large-field of view, high contrast and highly efficient immunolabeling

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kuipers, Jeroen; Boer, Pascal de; Giepmans, Ben N.G., E-mail: b.n.g.giepmans@umcg.nl

Scanning electron microscopy (SEM) is increasing its application in life sciences for electron density measurements of ultrathin sections. These are traditionally analyzed with transmission electron microscopy (TEM); by most labs, SEM analysis still is associated with surface imaging only. Here we report several advantages of SEM for thin sections over TEM, both for structural inspection, as well as analyzing immuno-targeted labels such as quantum dots (QDs) and gold, where we find that QD-labeling is ten times more efficient than gold-labeling. Furthermore, we find that omitting post-staining with uranyl and lead leads to QDs readily detectable over the ultrastructure, but undermore » these conditions ultrastructural contrast was even almost invisible in TEM examination. Importantly, imaging in SEM with STEM detection leads to both outstanding QDs and ultrastructural contrast. STEM imaging is superior over back-scattered electron imaging of these non-contrasted samples, whereas secondary electron detection cannot be used at all. We conclude that examination of ultrathin sections by SEM, which may be immunolabeled with QDs, will allow rapid and straightforward analysis of large fields with more efficient labeling than can be achieved with immunogold. The large fields of view routinely achieved with SEM, but not with TEM, allows straightforward raw data sharing using virtual microscopy, also known as nanotomy when this concerns EM data in the life sciences. - Highlights: • High resolution and large fields of view via nanotomy or virtual microscopy. • Highly relevant for EM‐datasets where information density is high. • Sample preparation with low contrast good for STEM, not TEM. • Quantum dots now stand out in STEM‐based detection. • 10 Times more efficient labeling with quantum dots compared to gold.« less

Electric shielding films for biased TEM samples and their application to in situ electron holography.

PubMed

Nomura, Yuki; Yamamoto, Kazuo; Hirayama, Tsukasa; Saitoh, Koh

2018-06-01

We developed a novel sample preparation method for transmission electron microscopy (TEM) to suppress superfluous electric fields leaked from biased TEM samples. In this method, a thin TEM sample is first coated with an insulating amorphous aluminum oxide (AlOx) film with a thickness of about 20 nm. Then, the sample is coated with a conductive amorphous carbon film with a thickness of about 10 nm, and the film is grounded. This technique was applied to a model sample of a metal electrode/Li-ion-conductive-solid-electrolyte/metal electrode for biasing electron holography. We found that AlOx film with a thickness of 10 nm has a large withstand voltage of about 8 V and that double layers of AlOx and carbon act as a 'nano-shield' to suppress 99% of the electric fields outside of the sample. We also found an asymmetry potential distribution between high and low potential electrodes in biased solid-electrolyte, indicating different accumulation behaviors of lithium-ions (Li+) and lithium-ion vacancies (VLi-) in the biased solid-electrolyte.

Dopant mapping in thin FIB prepared silicon samples by Off-Axis Electron Holography.

PubMed

Pantzer, Adi; Vakahy, Atsmon; Eliyahou, Zohar; Levi, George; Horvitz, Dror; Kohn, Amit

2014-03-01

Modern semiconductor devices function due to accurate dopant distribution. Off-Axis Electron Holography (OAEH) in the transmission electron microscope (TEM) can map quantitatively the electrostatic potential in semiconductors with high spatial resolution. For the microelectronics industry, ongoing reduction of device dimensions, 3D device geometry, and failure analysis of specific devices require preparation of thin TEM samples, under 70 nm thick, by focused ion beam (FIB). Such thicknesses, which are considerably thinner than the values reported to date in the literature, are challenging due to FIB induced damage and surface depletion effects. Here, we report on preparation of TEM samples of silicon PN junctions in the FIB completed by low-energy (5 keV) ion milling, which reduced amorphization of the silicon to 10nm thick. Additional perpendicular FIB sectioning enabled a direct measurement of the TEM sample thickness in order to determine accurately the crystalline thickness of the sample. Consequently, we find that the low-energy milling also resulted in a negligible thickness of electrically inactive regions, approximately 4nm thick. The influence of TEM sample thickness, FIB induced damage and doping concentrations on the accuracy of the OAEH measurements were examined by comparison to secondary ion mass spectrometry measurements as well as to 1D and 3D simulations of the electrostatic potentials. We conclude that for TEM samples down to 100 nm thick, OAEH measurements of Si-based PN junctions, for the doping levels examined here, resulted in quantitative mapping of potential variations, within ~0.1 V. For thinner TEM samples, down to 20 nm thick, mapping of potential variations is qualitative, due to a reduced accuracy of ~0.3 V. This article is dedicated to the memory of Zohar Eliyahou. Copyright © 2014 Elsevier B.V. All rights reserved.

Transmission electron microscopy of unstained hybrid Au nanoparticles capped with PPAA (plasma-poly-allylamine): structure and electron irradiation effects.

PubMed

Gontard, Lionel C; Fernández, Asunción; Dunin-Borkowski, Rafal E; Kasama, Takeshi; Lozano-Pérez, Sergio; Lucas, Stéphane

2014-12-01

Hybrid (organic shell-inorganic core) nanoparticles have important applications in nanomedicine. Although the inorganic components of hybrid nanoparticles can be characterized readily using conventional transmission electron microscopy (TEM) techniques, the structural and chemical arrangement of the organic molecular components remains largely unknown. Here, we apply TEM to the physico-chemical characterization of Au nanoparticles that are coated with plasma-polymerized-allylamine, an organic compound with the formula C3H5NH2. We discuss the use of energy-filtered TEM in the low-energy-loss range as a contrast enhancement mechanism for imaging the organic shells of such particles. We also study electron-beam-induced crystallization and amorphization of the shells and the formation of graphitic-like layers that contain both C and N. The resistance of the samples to irradiation by high-energy electrons, which is relevant for optical tuning and for understanding the degree to which such hybrid nanostructures are stable in the presence of biomedical radiation, is also discussed. Copyright © 2014 Elsevier Ltd. All rights reserved.

Transmission Electron Microscopy of Minerals and Rocks

NASA Astrophysics Data System (ADS)

McLaren, Alex C.

1991-04-01

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

Strain mapping in TEM using precession electron diffraction

DOEpatents

Taheri, Mitra Lenore; Leff, Asher Calvin

2017-02-14

A sample material is scanned with a transmission electron microscope (TEM) over multiple steps having a predetermined size at a predetermined angle. Each scan at a predetermined step and angle is compared to a template, wherein the template is generated from parameters of the material and the scanning. The data is then analyzed using local mis-orientation mapping and/or Nye's tensor analysis to provide information about local strain states.

Rational design of Ag/TiO2 nanosystems by a combined RF-sputtering/sol-gel approach.

PubMed

Armelao, Lidia; Barreca, Davide; Bottaro, Gregorio; Gasparotto, Alberto; Maccato, Chiara; Tondello, Eugenio; Lebedev, Oleg I; Turner, Stuart; Van Tendeloo, Gustaaf; Sada, Cinzia; Stangar, Urska Lavrencic

2009-12-21

The present work is devoted to the preparation of Ag/TiO(2) nanosystems by an original synthetic strategy, based on the radio-frequency (RF) sputtering of silver particles on titania-based xerogels prepared by the sol-gel (SG) route. This approach takes advantage of the synergy between the microporous xerogel structure and the infiltration power characterizing RF-sputtering, whose combination enables the obtainment of a tailored dispersion of Ag-containing particles into the titania matrix. In addition, the system's chemico-physical features can be tuned further through proper ex situ thermal treatments in air at 400 and 600 degrees C. The synthesized composites are extensively characterized by the joint use of complementary techniques, that is, X-ray photoelectron and X-ray excited Auger electron spectroscopies (XPS, XE-AES), secondary ion mass spectrometry (SIMS), glancing incidence X-ray diffraction (GIXRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), electron diffraction (ED), high-angle annular dark field scanning TEM (HAADF-STEM), energy-filtered TEM (EF-TEM) and optical absorption spectroscopy. Finally, the photocatalytic performances of selected samples in the decomposition of the azo-dye Plasmocorinth B are preliminarily investigated. The obtained results highlight the possibility of tailoring the system characteristics over a broad range, directly influencing their eventual functional properties.

Room temperature chemical synthesis of lead selenide thin films with preferred orientation

NASA Astrophysics Data System (ADS)

Kale, R. B.; Sartale, S. D.; Ganesan, V.; Lokhande, C. D.; Lin, Yi-Feng; Lu, Shih-Yuan

2006-11-01

Room temperature chemical synthesis of PbSe thin films was carried out from aqueous ammoniacal solution using Pb(CH3COO)2 as Pb2+ and Na2SeSO3 as Se2- ion sources. The films were characterized by a various techniques including, X-ray diffraction (XRD), energy dispersive X-ray analysis (EDAX), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HR-TEM), selected area electron diffraction (SAED), Fast Fourier transform (FFT) and UV-vis-NIR techniques. The study revealed that the PbSe thin film consists of preferentially oriented nanocubes with energy band gap of 0.5 eV.

Virus templated plasmonic nanoclusters with icosahedral symmetry via directed assembly

NASA Astrophysics Data System (ADS)

Ratna, Banahalli; Fontana, Jake; Dressick, Walter; Phelps, Jamie; Johnson, John; Sampson, Travian; Rendell, Ronald; Soto, Carissa

2015-03-01

Controlling the spatial and orientational order of plasmonic nanoparticles may lead to structures with novel electromagnetic properties and applications such as sub-wavelength imaging and ultra-sensitive chemical sensors. Here we report the directed assembly of three-dimensional, icosahedral plasmonic nanoclusters with resonances at visible wavelengths. We show using transmission electron microcopy and in situ dynamic light scattering the nanoclusters consist of twelve gold nanospheres attached to thiol groups at predefined locations on the surface of a genetically engineered cowpea mosaic virus with icosahedral symmetry. We measured the bulk absorbance from aqueous suspensions of nanoclusters and reproduced the major features of the spectrum using finite-element simulations. Furthermore, because the viruses are easily produced in gram quantities the directed assembly approach is capable of high-throughput, providing a strategy to realize large quantities for applications. NRL summer intern under the HBCU/MI Summer Research Program.

Correlation between Ti source/drain contact and performance of InGaZnO-based thin film transistors

NASA Astrophysics Data System (ADS)

Choi, Kwang-Hyuk; Kim, Han-Ki

2013-02-01

Ti contact properties and their electrical contribution to an amorphous InGaZnO (a-IGZO) semiconductor-based thin film transistor (TFT) were investigated in terms of chemical, structural, and electrical considerations. TFT device parameters were quantitatively studied by a transmission line method. By comparing various a-IGZO TFT parameters with those of different Ag and Ti source/drain electrodes, Ti S/D contact with an a-IGZO channel was found to lead to a negative shift in VT (-Δ 0.52 V). This resulted in higher saturation mobility (8.48 cm2/Vs) of a-IGZO TFTs due to effective interfacial reaction between Ti and an a-IGZO semiconducting layer. Based on transmission electron microcopy, x-ray photoelectron depth profile analyses, and numerical calculation of TFT parameters, we suggest a possible Ti contact mechanism on semiconducting a-IGZO channel layers for TFTs.

Characterization of TEM Moiré Patterns Originating from Two Monolayer Graphenes Grown on the Front and Back Sides of a Copper Substrate by CVD Method

NASA Astrophysics Data System (ADS)

Yamazaki, Kenji; Maehara, Yosuke; Gohara, Kazutoshi

2018-06-01

The number of layers affects the electronic properties of graphene owing to its unique band structure, called the Dirac corn. Raman spectroscopy is a key diagnostic tool for identifying the number of graphene layers and for determining their physical properties. Here, we observed moiré structures in transmission electron microscopy (TEM) observations; these are signature patterns in multilayer, although Raman spectra showed the typical intensity of the 2D/G peak in the monolayer. We also performed a multi-slice TEM image simulation to compare the 3D atomic structures of the two graphene membranes with experimental TEM images. We found that the experimental moiré image was constructed with a 9-12 Å interlayer distance between graphene membranes. This structure was constructed by transferring CVD-grown graphene films that formed on both sides of the Cu substrate at once.

Preparation of herpes simplex virus-infected primary neurons for transmission electron microscopy.

PubMed

Miranda-Saksena, Monica; Boadle, Ross; Cunningham, Anthony L

2014-01-01

Transmission electron microscopy (TEM) provides the resolution necessary to identify both viruses and subcellular components of cells infected with many types of viruses, including herpes simplex virus. Recognized as a powerful tool in both diagnostic and research-based virology laboratories, TEM has made possible the identification of new viruses and has contributed to the elucidation of virus life cycle and virus-host cell interaction. Whilst there are many sample preparation techniques for TEM, conventional processing using chemical fixation and resin embedding remains a useful technique, available in virtually all EM laboratories, for studying virus/cell ultrastructure. In this chapter, we describe the preparation of herpes simplex virus-infected primary neurons, grown on plastic cover slips, to allow sectioning of neurons and axons in their growth plane. This technique allows TEM examination of cell bodies, axons, growth cones, and varicosities, providing powerful insights into virus-cell interaction.

Quantitative Transmission Electron Microscopy of Nanoparticles and Thin-Film Formation in Electroless Metallization of Polymeric Surfaces

NASA Astrophysics Data System (ADS)

Dutta, Aniruddha; Heinrich, Helge; Kuebler, Stephen; Grabill, Chris; Bhattacharya, Aniket

2011-03-01

Gold nanoparticles(Au-NPs) act as nucleation sites for electroless deposition of silver on functionalized SU8 polymeric surfaces. Here we report the nanoscale morphology of Au and Ag nanoparticles as studied by Transmission Electron Microscopy (TEM). Scanning TEM with a high-angle annular dark-field detector is used to obtain atomic number contrast. From the intensity-calibrated plan-view scanning TEM images we determine the mean thickness and the volume distribution of the Au-NPs on the surface of the functionalized polymer. We also report the height and the radius distribution of the gold nanoparticles obtained from STEM images taking into consideration the experimental errors. The cross sectional TEM images yield the density and the average distance of the Au and Ag nanoparticles on the surface of the polymer. Supported by grant NSF, Chemistry Division.

Comments on ”Evidence of the hydrogen release mechanism in bulk MgH2”

NASA Astrophysics Data System (ADS)

Surrey, Alexander; Nielsch, Kornelius; Rellinghaus, Bernd

2017-04-01

The effect of an electron beam induced dehydrogenation of MgH2 in the transmission electron microscope (TEM) is largely underestimated by Nogita et al., and led the authors to a misinterpretation of their TEM observations. Firstly, the selected area diffraction (SAD) pattern is falsely interpreted. A re-evaluation of the SAD pattern reveals that no MgH2 is present in the sample, but that it rather consists of Mg and MgO only. Secondly, the transformation of the sample upon in-situ heating in the TEM cannot be ascribed to dehydrogenation, but is rather to be explained by the (nanoscale) Kirkendall effect, which leads to the formation of hollow MgO shells without any metallic Mg in their cores. Hence, the conclusions drawn from the TEM investigation are invalid, as the authors apparently have never studied MgH2.

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

NASA Astrophysics Data System (ADS)

Boyes, Edward D.; Gai, Pratibha L.

2014-02-01

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

Ultrastructural changes in tracheal epithelial cells exposed to oxygen

NASA Technical Reports Server (NTRS)

Philpott, D. E.; Harrison, G. A.; Turnbill, C.; Black, S.

1977-01-01

White albino rats were sacrificed after 24, 36, 48, 72, and 96 h of exposure to 100% O2 at 1 atm. Tissue was prepared for the scanning electron microscope (SEM) by Critical Point Drying and for the transmission electron microscope (TEM) by plastic embedding. Scanning microscopy showed a loss of microvilli after 48 h of exposure. Cilia appeared relatively normal with SEM, but TEM revealed changes in the outer membrane. In TEM, nonciliated cells appeared swollen and often encroached on the ciliated cells. A heavy mucous blanket remained even after processing. All the changes observed that are induced by oxygen exposure contribute to mucostasis, reducing and/or halting mucociliary clearance.

Nanoparticle formation of deposited Agn-clusters on free-standing graphene

NASA Astrophysics Data System (ADS)

Al-Hada, M.; Peters, S.; Gregoratti, L.; Amati, M.; Sezen, H.; Parisse, P.; Selve, S.; Niermann, T.; Berger, D.; Neeb, M.; Eberhardt, W.

2017-11-01

Size-selected Agn-clusters on unsupported graphene of a commercial Quantifoil sample have been investigated by surface and element-specific techniques such as transmission electron microscopy (TEM), spatially-resolved inner-shell X-ray photoelectron spectroscopy (XPS) and Auger electron spectroscopy (AES). An agglomeration of the highly mobile clusters into nm-sized Ag-nanodots of 2-3 nm is observed. Moreover, crystalline as well as non-periodic fivefold symmetric structures of the Ag-nanoparticles are evident by high-resolution TEM. Using a lognormal size-distribution as revealed by TEM, the measured positive binding energy shift of the air-exposed Ag-nanodots can be explained by the size-dependent dynamical liquid-drop model.

In situ TEM study of electron-beam radiation induced boron diffusion and effects on phase and microstructure evolution in nanostructured CoFeB/SiO2 thin film

NASA Astrophysics Data System (ADS)

Liu, B. H.; Teo, H. W.; Mo, Z. H.; Mai, Z. H.; Lam, J.; Xue, J. M.; Zhao, Y. Z.; Tan, P. K.

2017-01-01

Using in situ transmission electron microscopy (TEM), we studied boron diffusion and segregation in CoFeB/SiO2 nanostructured thin film stacks. We also investigated how these phenomena affected the phase and microstructure of CoFeB thin films under electron beam irradiation at 300 kV. A unique phase transformation was observed in CoFeB thin films under high-dose electron irradiation, from a polycrystalline Co3Fe to a unilateral amorphous phase of Co3Fe and nanocrystalline FexCo23-xB6. The unilateral amorphization of the Co3Fe film showed an electron-dose-rate sensitivity with a threshold dose rate. Detailed in situ TEM studies revealed that the unilateral amorphization of the Co3Fe film arose from boron segregation at the bottom of the Co3Fe thin film induced by radiation-enhanced diffusion of boron atoms that were displaced by electron knock-on effects. The radiation-induced nanocrystallization of FexCo23-xB6 was also found to be dose-rate sensitive with a higher electron beam current leading to earlier nucleation and more rapid grain growth. The nanocrystallization of FexCo23-xB6 occurred preferentially at the CoFeB/SiO2 interface. Kinetic studies by in situ TEM revealed the surface crystallization and diffusion-controlled nucleation and grain growth mechanisms. The radiation-enhanced atomic diffusivity and high-concentration of radiation-induced point defects at the Co3Fe/SiO2 interface enhanced the local short-range ordering of Fe, Co, and B atoms, favoring nucleation and grain growth of FexCo23-xB6 at the interface.

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

PubMed

Sutter, Eli A; Sutter, Peter W

2014-12-03

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

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

PubMed

Zečević, Jovana; Hermannsdörfer, Justus; Schuh, Tobias; de Jong, Krijn P; de Jonge, Niels

2017-01-01

Liquid-phase transmission electron microscopy (TEM) is used for in-situ imaging of nanoscale processes taking place in liquid, such as the evolution of nanoparticles during synthesis or structural changes of nanomaterials in liquid environment. Here, it is shown that the focused electron beam of scanning TEM (STEM) brings about the dissolution of silica nanoparticles in water by a gradual reduction of their sizes, and that silica redeposites at the sides of the nanoparticles in the scanning direction of the electron beam, such that elongated nanoparticles are formed. Nanoparticles with an elongation in a different direction are obtained simply by changing the scan direction. Material is expelled from the center of the nanoparticles at higher electron dose, leading to the formation of doughnut-shaped objects. Nanoparticles assembled in an aggregate gradually fuse, and the electron beam exposed section of the aggregate reduces in size and is elongated. Under TEM conditions with a stationary electron beam, the nanoparticles dissolve but do not elongate. The observed phenomena are important to consider when conducting liquid-phase STEM experiments on silica-based materials and may find future application for controlled anisotropic manipulation of the size and the shape of nanoparticles in liquid. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

DOE PAGES

Sutter, Eli A.; Sutter, Peter W.

2014-11-19

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

Characterization of BN rich layer on ammonia treated Nextel{trademark}312 fibers

DOE Office of Scientific and Technical Information (OSTI.GOV)

Khasgiwale, N.R.; Butler, E.P.; Tsakalakos, L.

A BN rich layer grown on Nextel{trademark}312 fibers by appropriate ammonia treatments was evaluated using various complimentary techniques including X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Scanning Electron Microscopy (SEM), and Transmission Electron Microscopy (TEM)/Parallel Electron Energy Loss Spectroscopy (PEELS in TEM). Three different ammonia treatments were studied. Ammonia treatment resulted in crystallization of the Nextel{trademark}312 fiber. The BN rich surface layer formed due to ammonia treatment was clearly detected in XPS and PEELS both before and after oxidation. The layer thickness was estimated to be between 5--10 nm. The layer was stable after oxidation treatment at 600 C formore » 100 hours. High resolution TEM observations of the fiber surface revealed a variable BN rich layer thickness. Patches of turbostratic BN were observed under certain conditions, however mostly the layer appeared to be amorphous.« less

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

PubMed

Kumar, Vineet

2011-12-01

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

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

PubMed

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.

Appendix B: Summary of TEM Particle Size Distribution Datasets

EPA Pesticide Factsheets

As discussed in the main text (see Section 5.3.2), calculation of the concentration of asbestos fibers in each of the bins of potential interest requires particle size distribution data derived using transmission electron microscopy (TEM).

Nonlinear Upshift of Trapped Electron Mode Critical Density Gradient: Simulation and Experiment

NASA Astrophysics Data System (ADS)

Ernst, D. R.

2012-10-01

A new nonlinear critical density gradient for pure trapped electron mode (TEM) turbulence increases strongly with collisionality, saturating at several times the linear threshold. The nonlinear TEM threshold appears to limit the density gradient in new experiments subjecting Alcator C-Mod internal transport barriers to modulated radio-frequency heating. Gyrokinetic simulations show the nonlinear upshift of the TEM critical density gradient is associated with long-lived zonal flow dominated states [1]. This introduces a strong temperature dependence that allows external RF heating to control TEM turbulent transport. During pulsed on-axis heating of ITB discharges, core electron temperature modulations of 50% were produced. Bursts of line-integrated density fluctuations, observed on phase contrast imaging, closely follow modulations of core electron temperature inside the ITB foot. Multiple edge fluctuation measurements show the edge response to modulated heating is out of phase with the core response. A new limit cycle stability diagram shows the density gradient appears to be clamped during on-axis heating by the nonlinear TEM critical density gradient, rather than by the much lower linear threshold. Fluctuation wavelength spectra will be quantitatively compared with nonlinear TRINITY/GS2 gyrokinetic transport simulations, using an improved synthetic diagnostic. In related work, we are implementing the first gyrokinetic exact linearized Fokker Planck collision operator [2]. Initial results show short wavelength TEMs are fully stabilized by finite-gyroradius collisional effects for realistic collisionalities. The nonlinear TEM threshold and its collisionality dependence may impact predictions of density peaking based on quasilinear theory, which excludes zonal flows.[4pt] In collaboration with M. Churchill, A. Dominguez, C. L. Fiore, Y. Podpaly, M. L. Reinke, J. Rice, J. L. Terry, N. Tsujii, M. A. Barnes, I. Bespamyatnov, R. Granetz, M. Greenwald, A. Hubbard, J. W. Hughes, M. Landreman, B. Li, Y. Ma, P. Phillips, M. Porkolab, W. Rowan, S. Wolfe, and S. Wukitch.[4pt] [1] D. R. Ernst et al., Proc. 21st IAEA Fusion Energy Conference, Chengdu, China, paper IAEA-CN-149/TH/1-3 (2006). http://www-pub.iaea.org/MTCD/Meetings/FEC200/th1-3.pdf[0pt] [2] B. Li and D.R. Ernst, Phys. Rev. Lett. 106, 195002 (2011).

Atomic-Scale Insights into the Oxidation of Aluminum.

PubMed

Nguyen, Lan; Hashimoto, Teruo; Zakharov, Dmitri N; Stach, Eric A; Rooney, Aidan P; Berkels, Benjamin; Thompson, George E; Haigh, Sarah J; Burnett, Tim L

2018-01-24

The surface oxidation of aluminum is still poorly understood despite its vital role as an insulator in electronics, in aluminum-air batteries, and in protecting the metal against corrosion. Here we use atomic resolution imaging in an environmental transmission electron microscope (TEM) to investigate the mechanism of aluminum oxide formation. Harnessing electron beam sputtering we prepare a pristine, oxide-free metal surface in the TEM. This allows us to study, as a function of crystallographic orientation and oxygen gas pressure, the full oxide growth regime from the first oxide nucleation to a complete saturated, few-nanometers-thick surface film.

Can direct electron detectors outperform phosphor-CCD systems for TEM?

NASA Astrophysics Data System (ADS)

Moldovan, G.; Li, X.; Kirkland, A.

2008-08-01

A new generation of imaging detectors is being considered for application in TEM, but which device architectures can provide the best images? Monte Carlo simulations of the electron-sensor interaction are used here to calculate the expected modulation transfer of monolithic active pixel sensors (MAPS), hybrid active pixel sensors (HAPS) and double sided Silicon strip detectors (DSSD), showing that ideal and nearly ideal transfer can be obtained using DSSD and MAPS sensors. These results highly recommend the replacement of current phosphor screen and charge coupled device imaging systems with such new directly exposed position sensitive electron detectors.

Atomic-Scale Insights into the Oxidation of Aluminum

DOE PAGES

Nguyen, Lan; Hashimoto, Teruo; Zakharov, Dmitri N.; ...

2018-01-10

Here, the surface oxidation of aluminum is still poorly understood despite its vital role as an insulator in electronics, in aluminum–air batteries, and in protecting the metal against corrosion. Here we use atomic resolution imaging in an environmental transmission electron microscope (TEM) to investigate the mechanism of aluminum oxide formation. Harnessing electron beam sputtering we prepare a pristine, oxide-free metal surface in the TEM. This allows us to study, as a function of crystallographic orientation and oxygen gas pressure, the full oxide growth regime from the first oxide nucleation to a complete anometers-thick surface film.

Fabrication and In Situ Transmission Electron Microscope Characterization of Free-Standing Graphene Nanoribbon Devices.

PubMed

Wang, Qing; Kitaura, Ryo; Suzuki, Shoji; Miyauchi, Yuhei; Matsuda, Kazunari; Yamamoto, Yuta; Arai, Shigeo; Shinohara, Hisanori

2016-01-26

Edge-dependent electronic properties of graphene nanoribbons (GNRs) have attracted intense interests. To fully understand the electronic properties of GNRs, the combination of precise structural characterization and electronic property measurement is essential. For this purpose, two experimental techniques using free-standing GNR devices have been developed, which leads to the simultaneous characterization of electronic properties and structures of GNRs. Free-standing graphene has been sculpted by a focused electron beam in transmission electron microscope (TEM) and then purified and narrowed by Joule heating down to several nanometer width. Structure-dependent electronic properties are observed in TEM, and significant increase in sheet resistance and semiconducting behavior become more salient as the width of GNR decreases. The narrowest GNR width we obtained with the present method is about 1.6 nm with a large transport gap of 400 meV.

Three-dimensional cytomorphology in fine needle aspiration biopsy of medullary thyroid carcinoma.

PubMed

Chang, T C; Lai, S M; Wen, C Y; Hsiao, Y L; Huang, S H

2001-01-01

To elucidate three-dimensional (3-D) cytomorphology in fine needle aspiration biopsy (FNAB) of medullary thyroid carcinoma (MTC). ENAB was performed on tumors from five patients with MTC. The aspirate was stained and observed under a light microscope (LM). The aspirate was also fixed, dehydrated, critical point dried, spattered with gold ions and observed with a scanning electron microscope (SEM). For transmission electron microscopy (TEM), the specimen was fixed, dehydrated, embedded in an Epon mixture, cut with an ultramicrotome, mounted on copper grids, electron doubly stained with uranium acetate and lead citrate, and observed with TEM. Findings under SEM were correlated with those under LM and TEM. Under SEM, 3-D cytomorphology of MTC displayed a disorganized cellular arrangement with indistinct cell borders in three cases. The cell surface was uneven and had granular protrusions that corresponded to secretory granules observed under TEM. In one case with multiple endocrine neoplasia type IIB, there were abundant granules on the cell surface. In one case of sporadic MTC with multinucleated tumor giant cells and small cells, granular protrusions also were noted on the cell surface. Granular protrusion was a characteristic finding in FNAB of MTC tinder SEM and might be helpful in the differential diagnosis.

Design of a 300-kV gas environmental transmission electron microscope equipped with a cold field emission gun.

PubMed

Isakozawa, Shigeto; Nagaoki, Isao; Watabe, Akira; Nagakubo, Yasuhira; Saito, Nobuhiro; Matsumoto, Hiroaki; Zhang, Xiao Feng; Taniguchi, Yoshifumi; Baba, Norio

2016-08-01

A new in situ environmental transmission electron microscope (ETEM) was developed based on a 300 kV TEM with a cold field emission gun (CFEG). Particular caution was taken in the ETEM design to assure uncompromised imaging and analytical performance of the TEM. Because of the improved pumping system between the gun and column, the vacuum of CFEG was largely improved and the probe current was sufficiently stabilized to operate without tip flashing for 2-3 h or longer. A high brightness of 2.5 × 10(9) A/cm(2) sr was measured at 300 kV, verifying the high quality of the CFEG electron beam. A specially designed gas injection-heating holder was used in the in situ TEM study at elevated temperatures with or without gas around the TEM specimen. Using this holder in a 10 Pa gas atmosphere and specimen temperatures up to 1000°C, high-resolution ETEM performance and analysis were achieved. © 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.

Cross-sectional TEM specimen preparation for W/B{sub 4}C multilayer sample using FIB

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mondal, Puspen, E-mail: puspen@rrcat.gov.in; Pradhan, P. C.; Tiwari, Pragya

2016-05-23

A recent emergence of a cross-beam scanning electron microscopy (SEM)/focused-ion-beam (FIB) system have given choice to fabricate cross-sectional transmission electron microscopy (TEM) specimen of thin film multilayer sample. A 300 layer pair thin film multilayer sample of W/B{sub 4}C was used to demonstrate the specimen lift-out technique in very short time as compared to conventional cross-sectional sample preparation technique. To get large area electron transparent sample, sample prepared by FIB is followed by Ar{sup +} ion polishing at 2 kV with grazing incident. The prepared cross-sectional sample was characterized by transmission electron microscope.

Analysis of Local Structure, Chemistry and Bonding by Electron Energy Loss Spectroscopy

NASA Astrophysics Data System (ADS)

Mayer, Joachim

In the present chapter, the reader will first be introduced briefly to the basic principles of analytical transmission electron microscopy (ATEM) with special emphasis on electron energy-loss spectroscopy (EELS) and energy-filtering TEM. The quantification of spectra to obtain chemical information and the origin and interpretation of near-edge fine structures in EELS (ELNES) are discussed. Special attention will be given to the characterization of internal interfaces and the literature in this area will be reviewed. Selected examples of the application of ATEM in the investigation of internal interfaces will be given. These examples include both EELS in the energy-filtering TEM and in the scanning transmission electron microscope (STEM).

Investigation of Thermal Stability of P2-NaxCoO2 Cathode Materials for Sodium Ion Batteries Using Real-Time Electron Microscopy.

PubMed

Hwang, Sooyeon; Lee, Yongho; Jo, Eunmi; Chung, Kyung Yoon; Choi, Wonchang; Kim, Seung Min; Chang, Wonyoung

2017-06-07

Here, we take advantage of in situ transmission electron microscopy (TEM) to investigate the thermal stability of P2-type Na x CoO 2 cathode materials for sodium ion batteries, which are promising candidates for next-generation lithium ion batteries. A double-tilt TEM heating holder was used to directly characterize the changes in the morphology and the crystallographic and electronic structures of the materials with increase in temperature. The electron diffraction patterns and the electron energy loss spectra demonstrated the presence of cobalt oxides (Co 3 O 4 , CoO) and even metallic cobalt (Co) at higher temperatures as a result of reduction of Co ions and loss of oxygen. The bright-field TEM images revealed that the surface of Na x CoO 2 becomes porous at high temperatures. Higher cutoff voltages result in degrading thermal stability of Na x CoO 2 . The observations herein provide a valuable insight that thermal stability is one of the important factors to be considered in addition to the electrochemical properties when developing new electrode materials for novel battery systems.

Investigation of Thermal Stability of P2–Na xCoO 2 Cathode Materials for Sodium Ion Batteries Using Real-Time Electron Microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hwang, Sooyeon; Lee, Yongho; Jo, Eunmi

In this paper, we take advantage of in situ transmission electron microscopy (TEM) to investigate the thermal stability of P2-type Na xCoO 2 cathode materials for sodium ion batteries, which are promising candidates for next-generation lithium ion batteries. A double-tilt TEM heating holder was used to directly characterize the changes in the morphology and the crystallographic and electronic structures of the materials with increase in temperature. The electron diffraction patterns and the electron energy loss spectra demonstrated the presence of cobalt oxides (Co 3O 4, CoO) and even metallic cobalt (Co) at higher temperatures as a result of reduction ofmore » Co ions and loss of oxygen. The bright-field TEM images revealed that the surface of Na xCoO 2 becomes porous at high temperatures. Higher cutoff voltages result in degrading thermal stability of Na xCoO 2. Finally, the observations herein provide a valuable insight that thermal stability is one of the important factors to be considered in addition to the electrochemical properties when developing new electrode materials for novel battery systems.« less

Investigation of Thermal Stability of P2–Na xCoO 2 Cathode Materials for Sodium Ion Batteries Using Real-Time Electron Microscopy

DOE PAGES

Hwang, Sooyeon; Lee, Yongho; Jo, Eunmi; ...

2017-05-11

In this paper, we take advantage of in situ transmission electron microscopy (TEM) to investigate the thermal stability of P2-type Na xCoO 2 cathode materials for sodium ion batteries, which are promising candidates for next-generation lithium ion batteries. A double-tilt TEM heating holder was used to directly characterize the changes in the morphology and the crystallographic and electronic structures of the materials with increase in temperature. The electron diffraction patterns and the electron energy loss spectra demonstrated the presence of cobalt oxides (Co 3O 4, CoO) and even metallic cobalt (Co) at higher temperatures as a result of reduction ofmore » Co ions and loss of oxygen. The bright-field TEM images revealed that the surface of Na xCoO 2 becomes porous at high temperatures. Higher cutoff voltages result in degrading thermal stability of Na xCoO 2. Finally, the observations herein provide a valuable insight that thermal stability is one of the important factors to be considered in addition to the electrochemical properties when developing new electrode materials for novel battery systems.« less

Performance of low-voltage STEM/TEM with delta corrector and cold field emission gun.

PubMed

Sasaki, Takeo; Sawada, Hidetaka; Hosokawa, Fumio; Kohno, Yuji; Tomita, Takeshi; Kaneyama, Toshikatsu; Kondo, Yukihito; Kimoto, Koji; Sato, Yuta; Suenaga, Kazu

2010-08-01

To reduce radiation damage caused by the electron beam and to obtain high-contrast images of specimens, we have developed a highly stabilized transmission electron microscope equipped with a cold field emission gun and spherical aberration correctors for image- and probe-forming systems, which operates at lower acceleration voltages than conventional transmission electron microscopes. A delta-type aberration corrector is designed to simultaneously compensate for third-order spherical aberration and fifth-order 6-fold astigmatism. Both were successfully compensated in both scanning transmission electron microscopy (STEM) and transmission electron microscopy (TEM) modes in the range 30-60 kV. The Fourier transforms of raw high-angle annular dark field (HAADF) images of a Si[110] sample revealed spots corresponding to lattice spacings of 111 and 96 pm at 30 and 60 kV, respectively, and those of raw TEM images of an amorphous Ge film with gold particles showed spots corresponding to spacings of 91 and 79 pm at 30 and 60 kV, respectively. Er@C(82)-doped single-walled carbon nanotubes, which are carbon-based samples, were successfully observed by HAADF-STEM imaging with an atomic-level resolution.

Subgrain boundary analyses in deformed orthopyroxene by TEM/STEM with EBSD-FIB sample preparation technique

NASA Astrophysics Data System (ADS)

Kogure, Toshihiro; Raimbourg, Hugues; Kumamoto, Akihito; Fujii, Eiko; Ikuhara, Yuichi

2014-12-01

High-resolution structure analyses using electron beam techniques have been performed for the investigation of subgrain boundaries (SGBs) in deformed orthopyroxene (Opx) in mylonite from Hidaka Metamorphic Belt, Hokkaido, Japan, to understand ductile deformation mechanism of silicate minerals in shear zones. Scanning electron microscopy (SEM) and electron backscatter diffraction (EBSD) analysis of Opx porphyroclasts in the mylonitic rock indicated that the crystal orientation inside the Opx crystals gradually changes by rotation about the b-axis by SGBs and crystal folding. In order to observe the SGBs along the b-axis by transmission electron microscopy (TEM) or scanning TEM (STEM), the following sample preparation protocol was adopted. First, petrographic thin sections were slightly etched with hydrofluoric acid to identify SGBs in SEM. The Opx crystals whose b-axes were oriented close to the normal of the surface were identified by EBSD, and the areas containing SGBs were picked and thinned for (S) TEM analysis with a focused ion beam instrument with micro-sampling system. High-resolution TEM imaging of the SGBs in Opx revealed various boundary structures from a periodic array of dissociated (100) [001] edge dislocations to partially or completely incoherent crystals, depending on the misorientation angle. Atomic-resolution STEM imaging clearly confirmed the formation of clinopyroxene (Cpx) structure between the dissociated partial dislocations. Moreover, X-ray microanalysis in STEM revealed that the Cpx contains a considerable amount of calcium replacing iron. Such chemical inhomogeneity may limit glide motion of the dislocation and eventually the plastic deformation of the Opx porphyroclasts at a low temperature. Chemical profiles across the high-angle incoherent SGB also showed an enrichment of the latter in calcium at the boundary, suggesting that SGBs are an efficient diffusion pathway of calcium out of host Opx grain during cooling.

Synthesis of Silver and Gold Nanoparticles Using Antioxidants from Blackberry, Blueberry, Pomegranate, and Turmeric Extracts

EPA Science Inventory

Greener synthesis of Ag and Au nanoparticles is described using antioxidants from blackberry, blueberry, pomegranate, and turmeric extracts. The synthesized particles were characterized using X-ray diffraction (XRD), transmission electron microscopy (TEM), high resolution TEM (HR...

Silver nanoparticle production by Rhizopus stolonifer and its antibacterial activity against extended spectrum {beta}-lactamase producing (ESBL) strains of Enterobacteriaceae

DOE Office of Scientific and Technical Information (OSTI.GOV)

Banu, Afreen; Rathod, Vandana, E-mail: drvandanarathod@rediffmail.com; Ranganath, E.

Highlights: {yields} Silver nanoparticle production by using Rhizopus stolonifer. {yields} Antibacterial activity of silver nanoparticles against extended spectrum {beta}-lactamase producing (ESBL) strains of Enterobacteriaceae. {yields} Synergistic effect of antibiotics with silver nanoparticles towards ESBL-strains. {yields} Characterization of silver nanoparticles made by UV-vis spectra, scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transformed infrared (FTIR) spectroscopy, atomic force microscopy (AFM). -- Abstract: This report focuses on the synthesis of silver nanoparticles using the fungus, Rhizopus stolonifer and its antimicrobial activity. Research in nanotechnology highlights the possibility of green chemistry pathways to produce technologically important nanomaterials. Characterization of newly synthesized silvermore » nanoparticles was made by UV-visible absorption spectroscopy, scanning electron microscope (SEM), transmission electron microscope (TEM), Fourier transform infrared (FTIR) spectroscopy and atomic force microscope (AFM). TEM micrograph revealed the formation of spherical nanoparticles with size ranging between 3 and 20 nm. The biosynthesized silver nanoparticles (AgNPs) showed excellent antibacterial activity against ESBL-strains which includes E. coli, Proteus. sp. and Klebsiella sp.« less

Structure and chemistry of epitaxial ceria thin films on yttria-stabilized zirconia substrates, studied by high resolution electron microscopy

DOE PAGES

Sinclair, Robert; Lee, Sang Chul; Shi, Yezhou; ...

2017-03-18

Here, we have applied aberration-corrected transmission electron microscopy (TEM) imaging and electron energy loss spectroscopy (EELS) to study the structure and chemistry of epitaxial ceria thin films, grown by pulsed laser deposition onto (001) yttria-stabilized zirconia (YSZ) substrates. There are few observable defects apart from the expected mismatch interfacial dislocations and so the films would be expected to have good potential for applications. Under high electron beam dose rate (above about 6000 e-/Å 2s) domains of an ordered structure appear and these are interpreted as being created by oxygen vacancy ordering. The ordered structure does not appear at lower losemore » rates (ca. 2600 e-/Å 2s) and can be removed by imaging under 1 mbar oxygen gas in an environmental TEM. EELS confirms that there is both oxygen deficiency and the associated increase in Ce 3+ versus Ce 4+ cations in the ordered domains. In situ high resolution TEM recordings show the formation of the ordered domains as well as atomic migration along the ceria thin film (001) surface.« less

Structure and chemistry of epitaxial ceria thin films on yttria-stabilized zirconia substrates, studied by high resolution electron microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sinclair, Robert; Lee, Sang Chul; Shi, Yezhou

Here, we have applied aberration-corrected transmission electron microscopy (TEM) imaging and electron energy loss spectroscopy (EELS) to study the structure and chemistry of epitaxial ceria thin films, grown by pulsed laser deposition onto (001) yttria-stabilized zirconia (YSZ) substrates. There are few observable defects apart from the expected mismatch interfacial dislocations and so the films would be expected to have good potential for applications. Under high electron beam dose rate (above about 6000 e-/Å 2s) domains of an ordered structure appear and these are interpreted as being created by oxygen vacancy ordering. The ordered structure does not appear at lower losemore » rates (ca. 2600 e-/Å 2s) and can be removed by imaging under 1 mbar oxygen gas in an environmental TEM. EELS confirms that there is both oxygen deficiency and the associated increase in Ce 3+ versus Ce 4+ cations in the ordered domains. In situ high resolution TEM recordings show the formation of the ordered domains as well as atomic migration along the ceria thin film (001) surface.« less

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

NASA Astrophysics Data System (ADS)

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

2018-02-01

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

Direct observation of morphological evolution of a catalyst during carbon nanotube forest growth: new insights into growth and growth termination

NASA Astrophysics Data System (ADS)

Jeong, Seojeong; Lee, Jaegeun; Kim, Hwan-Chul; Hwang, Jun Yeon; Ku, Bon-Cheol; Zakharov, Dmitri N.; Maruyama, Benji; Stach, Eric A.; Kim, Seung Min

2016-01-01

In this study, we develop a new methodology for transmission electron microscopy (TEM) analysis that enables us to directly investigate the interface between carbon nanotube (CNT) arrays and the catalyst and support layers for CNT forest growth without any damage induced by a post-growth TEM sample preparation. Using this methodology, we perform in situ and ex situ TEM investigations on the evolution of the morphology of the catalyst particles and observe the catalyst particles to climb up through CNT arrays during CNT forest growth. We speculate that the lifted catalysts significantly affect the growth and growth termination of CNT forests along with Ostwald ripening and sub-surface diffusion. Thus, we propose a modified growth termination model which better explains various phenomena related to the growth and growth termination of CNT forests.In this study, we develop a new methodology for transmission electron microscopy (TEM) analysis that enables us to directly investigate the interface between carbon nanotube (CNT) arrays and the catalyst and support layers for CNT forest growth without any damage induced by a post-growth TEM sample preparation. Using this methodology, we perform in situ and ex situ TEM investigations on the evolution of the morphology of the catalyst particles and observe the catalyst particles to climb up through CNT arrays during CNT forest growth. We speculate that the lifted catalysts significantly affect the growth and growth termination of CNT forests along with Ostwald ripening and sub-surface diffusion. Thus, we propose a modified growth termination model which better explains various phenomena related to the growth and growth termination of CNT forests. Electronic supplementary information (ESI) available. See DOI: 10.1039/c5nr05547d

Optimal Simulations by Butterfly Networks: Extended Abstract,

DTIC Science & Technology

1987-11-01

Typescript , Univ. of Massachusetts; submitted for nublication. 1_2.2 Ll, - W 12. ifliU 1.8 UI1.25 . l i I 61 MICROCOPY RESOLUTION TEST CHART NATIONAL...1987): An optimal mapping of the FFT algorithm onto the tlypercube architecture. Typescript , Univ. of Massachusetts; submitted for publication. (HR I

Dynamic Production Networks.

DTIC Science & Technology

1981-04-01

UNCLASSIFIED ORC-81-7 ta. MICROCOP ES LUON’TE MICROCOPY RE.SOLUTION’ TEST CHART -U -ORC 81-7 APRIL 1981 DYNAFIC PRODUCTIn METhORKSARI by RONALD W. SHEPHARD...final outputs may be required for the facilities (activities) of a large production network. Also a compounding of the complexity of an optimization

Legal Questions of the Application of Microfilms.

ERIC Educational Resources Information Center

Basco, Jeno; And Others

This study analyses and summarizes the statutory regulations of various countries regarding the legal validation and use of certified microcopies in place of original documents. Descriptions are provided and rules summarized for the categories of: (1) the purpose of microfilming; (2) principle uses of microfilm; (3) the making of microfilm and…

Complete Tem-Tomography: 3D Structure of Gems Cluster

NASA Technical Reports Server (NTRS)

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.

Electronic structure and fine structural features of the air-grown UNxOy on nitrogen-rich uranium nitride

NASA Astrophysics Data System (ADS)

Long, Zhong; Zeng, Rongguang; Hu, Yin; Liu, Jing; Wang, Wenyuan; Zhao, Yawen; Luo, Zhipeng; Bai, Bin; Wang, Xiaofang; Liu, Kezhao

2018-06-01

Oxide formation on surface of nitrogen-rich uranium nitride film/particles was investigated using X-ray photoelectron spectroscopy (XPS), auger electron spectroscopy (AES), aberration-corrected transmission electron microscopy (TEM), and high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) coupled with electron energy-loss spectroscopy (EELS). XPS and AES studies indicated that the oxidized layer on UN2-x film is ternary compound uranium oxynitride (UNxOy) in 5-10 nm thickness. TEM/HAADF-STEM and EELS studies revealed the UNxOy crystallizes in the FCC CaF2-type structure with the lattice parameter close to the CaF2-type UN2-x matrix. The work can provide further information to the oxidation mechanism of uranium nitride.

FIB-SEM imaging of carbon nanotubes in mouse lung tissue.

PubMed

Købler, Carsten; Saber, Anne Thoustrup; Jacobsen, Nicklas Raun; Wallin, Håkan; Vogel, Ulla; Qvortrup, Klaus; Mølhave, Kristian

2014-06-01

Ultrastructural characterisation is important for understanding carbon nanotube (CNT) toxicity and how the CNTs interact with cells and tissues. The standard method for this involves using transmission electron microscopy (TEM). However, in particular, the sample preparation, using a microtome to cut thin sample sections for TEM, can be challenging for investigation of regions with agglomerations of large and stiff CNTs because the CNTs cut with difficulty. As a consequence, the sectioning diamond knife may be damaged and the uncut CNTs are left protruding from the embedded block surface excluding them from TEM analysis. To provide an alternative to ultramicrotomy and subsequent TEM imaging, we studied focused ion beam scanning electron microscopy (FIB-SEM) of CNTs in the lungs of mice, and we evaluated the applicability of the method compared to TEM. FIB-SEM can provide serial section volume imaging not easily obtained with TEM, but it is time-consuming to locate CNTs in the tissue. We demonstrate that protruding CNTs after ultramicrotomy can be used to locate the region of interest, and we present FIB-SEM images of CNTs in lung tissue. FIB-SEM imaging was applied to lung tissue from mice which had been intratracheally instilled with two different multiwalled CNTs; one being short and thin, and the other longer and thicker. FIB-SEM was found to be most suitable for detection of the large CNTs (Ø ca. 70 nm), and to be well suited for studying CNT agglomerates in biological samples which is challenging using standard TEM techniques.

Electron microscopic diagnosis of human flavivirus encephalitis: use of confocal microscopy as an aid.

PubMed

Chu, C T; Howell, D N; Morgenlander, J C; Hulette, C M; McLendon, R E; Miller, S E

1999-10-01

The distinction between intracranial viral infections and inflammatory conditions requiring immunosuppression is important. Although specific laboratory reagents are readily available for some viruses, diagnosis of arbovirus infection is more difficult. Transmission electron microscopy (TEM) theoretically allows identification of viral particles independent of reagent availability, but it has limited sensitivity. We report two cases of human flavivirus encephalitis diagnosed by TEM. Laser scanning confocal microscopy (LSCM) was used in one case to survey unembedded tissue slices for focal abnormalities, from which fragments smaller than 1 mm2 were excised for epoxy embedding. This facilitated TEM identification of intracytoplasmic, budding, 35-40 nm spherical virus particles, confirmed by serology as St. Louis encephalitis. In contrast to mosquitoes and newborn mice, in which high viral loads are associated with minimal tissue responses, these biopsies showed florid angiodestructive inflammation and microgliosis, with rare virions in necrotic perivascular cells and astrocytes. To our knowledge, this represents the first ultrastructural study of St. Louis encephalitis in humans, indicating the potential value of LSCM-aided TEM.

Electron microscopy of the amphibian model systems Xenopus laevis and Ambystoma mexicanum.

PubMed

Kurth, Thomas; Berger, Jürgen; Wilsch-Bräuninger, Michaela; Kretschmar, Susanne; Cerny, Robert; Schwarz, Heinz; Löfberg, Jan; Piendl, Thomas; Epperlein, Hans H

2010-01-01

In this chapter we provide a set of different protocols for the ultrastructural analysis of amphibian (Xenopus, axolotl) tissues, mostly of embryonic origin. For Xenopus these methods include: (1) embedding gastrulae and tailbud embryos into Spurr's resin for TEM, (2) post-embedding labeling of methacrylate (K4M) and cryosections through adult and embryonic epithelia for correlative LM and TEM, and (3) pre-embedding labeling of embryonic tissues with silver-enhanced nanogold. For the axolotl (Ambystoma mexicanum) we present the following methods: (1) SEM of migrating neural crest (NC) cells; (2) SEM and TEM of extracellular matrix (ECM) material; (3) Cryo-SEM of extracellular matrix (ECM) material after cryoimmobilization; and (4) TEM analysis of hyaluronan using high-pressure freezing and HABP labeling. These methods provide exemplary approaches for a variety of questions in the field of amphibian development and regeneration, and focus on cell biological issues that can only be answered with fine structural imaging methods, such as electron microscopy. Copyright © 2010 Elsevier Inc. All rights reserved.

cisTEM, user-friendly software for single-particle image processing.

PubMed

Grant, Timothy; Rohou, Alexis; Grigorieff, Nikolaus

2018-03-07

We have developed new open-source software called cis TEM (computational imaging system for transmission electron microscopy) for the processing of data for high-resolution electron cryo-microscopy and single-particle averaging. cis TEM features a graphical user interface that is used to submit jobs, monitor their progress, and display results. It implements a full processing pipeline including movie processing, image defocus determination, automatic particle picking, 2D classification, ab-initio 3D map generation from random parameters, 3D classification, and high-resolution refinement and reconstruction. Some of these steps implement newly-developed algorithms; others were adapted from previously published algorithms. The software is optimized to enable processing of typical datasets (2000 micrographs, 200 k - 300 k particles) on a high-end, CPU-based workstation in half a day or less, comparable to GPU-accelerated processing. Jobs can also be scheduled on large computer clusters using flexible run profiles that can be adapted for most computing environments. cis TEM is available for download from cistem.org. © 2018, Grant et al.

cisTEM, user-friendly software for single-particle image processing

PubMed Central

2018-01-01

We have developed new open-source software called cisTEM (computational imaging system for transmission electron microscopy) for the processing of data for high-resolution electron cryo-microscopy and single-particle averaging. cisTEM features a graphical user interface that is used to submit jobs, monitor their progress, and display results. It implements a full processing pipeline including movie processing, image defocus determination, automatic particle picking, 2D classification, ab-initio 3D map generation from random parameters, 3D classification, and high-resolution refinement and reconstruction. Some of these steps implement newly-developed algorithms; others were adapted from previously published algorithms. The software is optimized to enable processing of typical datasets (2000 micrographs, 200 k – 300 k particles) on a high-end, CPU-based workstation in half a day or less, comparable to GPU-accelerated processing. Jobs can also be scheduled on large computer clusters using flexible run profiles that can be adapted for most computing environments. cisTEM is available for download from cistem.org. PMID:29513216

Targeted nanodiamonds for identification of subcellular protein assemblies in mammalian cells

PubMed Central

Lake, Michael P.; Bouchard, Louis-S.

2017-01-01

Transmission electron microscopy (TEM) can be used to successfully determine the structures of proteins. However, such studies are typically done ex situ after extraction of the protein from the cellular environment. Here we describe an application for nanodiamonds as targeted intensity contrast labels in biological TEM, using the nuclear pore complex (NPC) as a model macroassembly. We demonstrate that delivery of antibody-conjugated nanodiamonds to live mammalian cells using maltotriose-conjugated polypropylenimine dendrimers results in efficient localization of nanodiamonds to the intended cellular target. We further identify signatures of nanodiamonds under TEM that allow for unambiguous identification of individual nanodiamonds from a resin-embedded, OsO4-stained environment. This is the first demonstration of nanodiamonds as labels for nanoscale TEM-based identification of subcellular protein assemblies. These results, combined with the unique fluorescence properties and biocompatibility of nanodiamonds, represent an important step toward the use of nanodiamonds as markers for correlated optical/electron bioimaging. PMID:28636640

Antifungal mechanism of antibacterial peptide, ABP-CM4, from Bombyx mori against Aspergillus niger.

PubMed

Zhang, Jie; Wu, Xi; Zhang, Shuang-Quan

2008-12-01

Antibacterial peptide, CM4 (ABP-CM4), a 35 amino acid peptide from Chinese silkworm-Bombyx mori, displayed a strong antifungal activity against Aspergillus niger, Trichoderma viride and Gibberella saubinetii. Scanning electron microcopy showed that the morphology of conidia became more irregular and swelled when treated with ABP-CM4 at its minimal inhibitory concentration (MIC) of 8 muM. A cell wall regeneration assay indicated that the plasma membrane was the prime target of ABP-CM4 action. Confocal laser scanning microscopy showed that the cytoskeleton of A. niger was destroyed when treated with ABP-CM4 at 8 muM. Furthermore, transmission electron microscopy showed that the membrane and the cellular organelles of fungus were disrupted and there were many vacuoles in the fungal cellular space after the treatment with ABP-CM4. A gel-retardation assay showed that ABP-CM4 bound the DNA of A. niger. Our results suggest that ABP-CM4 exerts its antifungal activity by disrupting the structure of cell membranes and the cytoskeleton and interacts with the organelles, such as the mitochondrion and with the DNA in the fungal cell, subsequently resulting in cell death.

The potentials and challenges of electron microscopy in the study of atomic chains

NASA Astrophysics Data System (ADS)

Banhart, Florian; Torre, Alessandro La; Romdhane, Ferdaous Ben; Cretu, Ovidiu

2017-04-01

The article is a brief review on the potential of transmission electron microscopy (TEM) in the investigation of atom chains which are the paradigm of a strictly one-dimensional material. After the progress of TEM in the study of new two-dimensional materials, microscopy of free-standing one-dimensional structures is a new challenge with its inherent potentials and difficulties. In-situ experiments in the TEM allowed, for the first time, to generate isolated atomic chains consisting of metals, carbon or boron nitride. Besides having delivered a solid proof for the existence of atomic chains, in-situ TEM studies also enabled us to measure the electrical properties of these fundamental linear structures. While ballistic quantum conductivity is observed in chains of metal atoms, electrical transport in chains of sp1-hybridized carbon is limited by resonant states and reflections at the contacts. Although substantial progress has been made in recent TEM studies of atom chains, fundamental questions have to be answered, concerning the structural stability of the chains, bonding states at the contacts, and the suitability for applications in nanotechnology. Contribution to the topical issue "The 16th European Microscopy Congress (EMC 2016)", edited by Richard Brydson and Pascale Bayle-Guillemaud

Clay minerals in primitive meteorites and interplanetary dust 2. Smectites and micas

NASA Technical Reports Server (NTRS)

Keller, L. P.; Zolensky, M. E.

1991-01-01

The classification is briefly summarized of stony meteorites and cosmic dust, and the mineralogy and chemistry is described of serpentine group minerals. The occurrence of smectites and micas in extraterrestrial materials is examined. The characterization of fine grained minerals in meteorites and IDPs relies heavily on electron beam instruments, especially the transmission electron microscope (TEM). Typically, phyllosilicates are identified by a combination of high resolution imaging of basal spacings, electron diffraction, and chemical analysis. Smectites can be difficult to differentiate from micas because the smectites lose their interlayer water and the interlayer partly collapse in the high vacuum of the TEM.

AAO-based nanoreservoir arrays: A quick and easy support for TEM characterization

NASA Astrophysics Data System (ADS)

Mace, M.; Sahaf, H.; Moyen, E.; Bedu, F.; Masson, L.; Hanbücken, M.

2010-12-01

Large-scale arrays of calibrated, nanometer sized reservoirs are prepared by adapting the well-established electrochemical method used so far for the preparation of anodic aluminium oxide (AAO) membranes. The bottom plane of the assembly is prepared to be transparent for high-energy electrons, enabling their use as a universal sample support for transmission electron microscopy studies of nanoparticles. The nanoreservoir substrates can be cleaned under ultra-high-vacuum conditions and filled, by evaporating different materials. Filled nanoreservoirs can locally be sealed with a thin carbon layer using focused-ion-beam-induced deposition (FIBID). Nanoparticles, grow at various adsorption places on the walls and bottom planes inside the nanoreservoirs. They can be characterized by transmission electron microscopy (TEM) without further sample preparation in different crystallographic directions. Due to the dense array-arrangement of the reservoirs, very good statistics can already be obtained on one single sample. The controlled fabrication of the nanoreservoir array and first TEM results obtained on Au nanoparticles before and after sealing of the reservoirs, are presented.

Nucleation and Growth of Crystalline Grains in RF-Sputtered TiO 2 Films

DOE PAGES

Johnson, J. C.; Ahrenkiel, S. P.; Dutta, P.; ...

2009-01-01

Amore » morphous TiO 2 thin films were radio frequency sputtered onto siliconmonoxide and carbon support films on molybdenum transmission electron microscope (TEM) grids and observed during in situ annealing in a TEM heating stage at 250 ∘ C. The evolution of crystallization is consistent with a classical model of homogeneous nucleation and isotropic grain growth. The two-dimensional grain morphology of the TEM foil allowed straightforward recognition of amorphous and crystallized regions of the films, for measurement of crystalline volume fraction and grain number density. By assuming that the kinetic parameters remain constant beyond the onset of crystallization, the final average grain size was computed, using an analytical extrapolation to the fully crystallized state. Electron diffraction reveals a predominance of the anatase crystallographic phase.« less

Structural properties of GaAsN grown on (001) GaAs by metalorganic molecular beam epitaxy

NASA Astrophysics Data System (ADS)

Ok, Young-Woo; Choi, Chel-Jong; Seong, Tae-Yeon; Uesugi, K.; Suemune, I.

2001-07-01

Detailed transmission electron microscopy (TEM) and transmission electron diffraction (TED) examination has been made of metalorganic molecular beam epitaxial GaAsN layers grown on (001) GaAs substrates. TEM results show that lateral composition modulation occurs in the GaAs1-xNx layer (x 6.75%). It is shown that increasing N composition and Se (dopant) concentration leads to poor crystallinity. It is also shown that the addition of Se increases N composition. Atomic force microscopy (AFM) results show that the surfaces of the samples experience a morphological change from faceting to islanding, as the N composition and Se concentration increase. Based on the TEM and AFM results, a simple model is given to explain the formation of the lateral composition modulation.

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Colby, Robert J.; Alsem, Daan H.; Liyu, Andrey V.

2015-06-01

The development of environmental transmission electron microscopy (TEM) has enabled in situ experiments in a gaseous environment with high resolution imaging and spectroscopy. Addressing scientific challenges in areas such as catalysis, corrosion, and geochemistry can require pressures much higher than the ~20 mbar achievable with a differentially pumped, dedicated environmental TEM. Gas flow stages, in which the environment is contained between two semi-transparent thin membrane windows, have been demonstrated at pressures of several atmospheres. While this constitutes significant progress towards operando measurements, the design of many current gas flow stages is such that the pressure at the sample cannot necessarilymore » be directly inferred from the pressure differential across the system. Small differences in the setup and design of the gas flow stage can lead to very different sample pressures. We demonstrate a method for measuring the gas pressure directly, using a combination of electron energy loss spectroscopy and TEM imaging. This method requires only two energy filtered TEM images, limiting the measurement time to a few seconds and can be performed during an ongoing experiment at the region of interest. This approach provides a means to ensure reproducibility between different experiments, and even between very differently designed gas flow stages.« less

Correlative Electron and Fluorescence Microscopy of Magnetotactic Bacteria in Liquid: Toward In Vivo Imaging

PubMed Central

Woehl, Taylor J.; Kashyap, Sanjay; Firlar, Emre; Perez-Gonzalez, Teresa; Faivre, Damien; Trubitsyn, Denis; Bazylinski, Dennis A.; Prozorov, Tanya

2014-01-01

Magnetotactic bacteria biomineralize ordered chains of uniform, membrane-bound magnetite or greigite nanocrystals that exhibit nearly perfect crystal structures and species-specific morphologies. Transmission electron microscopy (TEM) is a critical technique for providing information regarding the organization of cellular and magnetite structures in these microorganisms. However, conventional TEM can only be used to image air-dried or vitrified bacteria removed from their natural environment. Here we present a correlative scanning TEM (STEM) and fluorescence microscopy technique for imaging viable cells of Magnetospirillum magneticum strain AMB-1 in liquid using an in situ fluid cell TEM holder. Fluorescently labeled cells were immobilized on microchip window surfaces and visualized in a fluid cell with STEM, followed by correlative fluorescence imaging to verify their membrane integrity. Notably, the post-STEM fluorescence imaging indicated that the bacterial cell wall membrane did not sustain radiation damage during STEM imaging at low electron dose conditions. We investigated the effects of radiation damage and sample preparation on the bacteria viability and found that approximately 50% of the bacterial membranes remained intact after an hour in the fluid cell, decreasing to ~30% after two hours. These results represent a first step toward in vivo studies of magnetite biomineralization in magnetotactic bacteria. PMID:25358460

Correlative Electron and Fluorescence Microscopy of Magnetotactic Bacteria in Liquid: Toward In Vivo Imaging

DOE PAGES

Woehl, Taylor J.; Kashyap, Sanjay; Firlar, Emre; ...

2014-10-31

Magnetotactic bacteria biomineralize ordered chains of uniform, membrane-bound magnetite or greigite nanocrystals that exhibit nearly perfect crystal structures and species-specific morphologies. Transmission electron microscopy (TEM) is a critical technique for providing information regarding the organization of cellular and magnetite structures in these microorganisms. However, conventional TEM can only be used to image air-dried or vitrified bacteria removed from their natural environment. Here we present a correlative scanning TEM (STEM) and fluorescence microscopy technique for imaging viable cells of Magnetospirillum magneticum strain AMB-1 in liquid using an in situ fluid cell TEM holder. Fluorescently labeled cells were immobilized on microchip windowmore » surfaces and visualized in a fluid cell with STEM, followed by correlative fluorescence imaging to verify their membrane integrity. Notably, the post-STEM fluorescence imaging indicated that the bacterial cell wall membrane did not sustain radiation damage during STEM imaging at low electron dose conditions. We investigated the effects of radiation damage and sample preparation on the bacteria viability and found that approximately 50% of the bacterial membranes remained intact after an hour in the fluid cell, decreasing to ~30% after two hours. These results represent a first step toward in vivo studies of magnetite biomineralization in magnetotactic bacteria.« less

The influence of hair bleach on the ultrastructure of human hair with special reference to hair damage.

PubMed

Imai, Takehito

2011-05-01

The influence of human hair bleaching agents with different bleaching strength on the ultrastructure of human hair was studied using a transmission electron microscope (TEM) and an energy dispersive X-ray spectrometer equipped with TEM (EDS-TEM). Two kinds of bleaching agents were used: a lightener agent with a weak bleaching effect and a powder-bleach with a stronger bleaching effect. From the comparison of the bleaching properties obtained by the electronic staining of black and white hair samples, it was suggested that the permeability of hair was increased by bleaching, and there was an increase of the stainability of hair subjected to electronic staining. The bleaching action provoked the decomposition of melanin granules and the flow out of granular contents into the intermacrofibrillar matrix. Some metal elements were detected in the melanin granular matrix by EDS-TEM. As a result, the diffusion of metal elements into the intermacrofibrillar matrix promoted further damage to the hair by catalytic action with the hydrogen peroxide in the bleaching agents outside the melanin granules. Further study will lead us to the edge of the development of a new bleaching agent, which reacts only with melanin granules and causes the minimum of damage to outside the melanin granules.

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

PubMed

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

2014-08-01

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

ITG-TEM turbulence simulation with bounce-averaged kinetic electrons in tokamak geometry

NASA Astrophysics Data System (ADS)

Kwon, Jae-Min; Qi, Lei; Yi, S.; Hahm, T. S.

2017-06-01

We develop a novel numerical scheme to simulate electrostatic turbulence with kinetic electron responses in magnetically confined toroidal plasmas. Focusing on ion gyro-radius scale turbulences with slower frequencies than the time scales for electron parallel motions, we employ and adapt the bounce-averaged kinetic equation to model trapped electrons for nonlinear turbulence simulation with Coulomb collisions. Ions are modeled by employing the gyrokinetic equation. The newly developed scheme is implemented on a global δf particle in cell code gKPSP. By performing linear and nonlinear simulations, it is demonstrated that the new scheme can reproduce key physical properties of Ion Temperature Gradient (ITG) and Trapped Electron Mode (TEM) instabilities, and resulting turbulent transport. The overall computational cost of kinetic electrons using this novel scheme is limited to 200%-300% of the cost for simulations with adiabatic electrons. Therefore the new scheme allows us to perform kinetic simulations with trapped electrons very efficiently in magnetized plasmas.

Quasi-parallel precession diffraction: Alignment method for scanning transmission electron microscopes.

PubMed

Plana-Ruiz, S; Portillo, J; Estradé, S; Peiró, F; Kolb, Ute; Nicolopoulos, S

2018-06-06

A general method to set illuminating conditions for selectable beam convergence and probe size is presented in this work for Transmission Electron Microscopes (TEM) fitted with µs/pixel fast beam scanning control, (S)TEM, and an annular dark field detector. The case of interest of beam convergence and probe size, which enables diffraction pattern indexation, is then used as a starting point in this work to add 100 Hz precession to the beam while imaging the specimen at a fast rate and keeping the projector system in diffraction mode. The described systematic alignment method for the adjustment of beam precession on the specimen plane while scanning at fast rates is mainly based on the sharpness of the precessed STEM image. The complete alignment method for parallel condition and precession, Quasi-Parallel PED-STEM, is presented in block diagram scheme, as it has been tested on a variety of instruments. The immediate application of this methodology is that it renders the TEM column ready for the acquisition of Precessed Electron Diffraction Tomographies (EDT) as well as for the acquisition of slow Precessed Scanning Nanometer Electron Diffraction (SNED). Examples of the quality of the Precessed Electron Diffraction (PED) patterns and PED-STEM alignment images are presented with corresponding probe sizes and convergence angles. Copyright © 2018. Published by Elsevier B.V.

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

PubMed

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.

Dissolution Behaviour of Metal Elements from Several Types of E-waste Using Leaching Test

NASA Astrophysics Data System (ADS)

Nor, Nik Hisyamudin Muhd; Amira Nordin, Nurul; Mohamad, Fariza; Jaibee, Shafizan; Ismail, Al Emran; Omar, Badrul; Fauzi Ahmad, Mohd; Rahim, Abd Khalil Abd; Kamaruddin, Muhamad Khalif Ikhwan Mohd; Turan, Faiz Mohd; Abu Bakar, Elmi; Yokoyama, Seiji

2017-08-01

Rapid development of the electrical and electronic was increasing annually due to the demand by the human being. Increasing production of electrical and electronic product led to the increasing of electric and electronic waste or can be called as the e-waste. The UN Environment Programme estimates that the world generates 20-50 million tons of the e-waste each year and the amount is raising three times faster than other forms of municipal waste. This study is focusing on the investigation of the dissolution behaviour of metal element from several types of e-waste by hydrometallurgical process. Leaching test was conducted on the e-waste by using acid as the reagent solution. Prior to the leaching test, manual dismantling, separation, and crushing process were carried out to the e-waste. The e-waste were characterized by Scanning Electron Microcopy (SEM) and the Energy Dispersive X-ray Spectroscopy (EDX) to define the elements inside the sample of e-waste. While the liquid residue from leaching test was analyzed by using Inductively Couple Plasma-Mass Spectrometer (ICP-MS) to define the dissolution behaviour of the metal element that contain in the e-waste. It was found that the longest time for dismantling process was the dismantling of laptop. The dissolution behaviour of Fe, Al, Zn and Pb elements in the e-waste has affected to the increase of pH. The increasing pH led to the reduction of the metals element during leaching process.

Medical Entomology Project.

DTIC Science & Technology

1984-01-01

Culex (Melanoconion) invocator Pazos with a redescription of adults and illustration of male genitalia (Diptera: Culicidae). Mosq. Syst. 10(2):239-245...11111_2 1 11J._- 4 MICROCOPY RESOLUTION TEST CHART NATIONAL BUR[AU OF MTANDARDS 1961 A ,o __I I I~ iI!p••n AD_ _ _ _ _ _ _ _ MEDICAL ENTOMOLOGY PROJECT...12 a . Genus Anopheles .............................................. 12 b. Genus Aedes

Computer Software for Life Cycle Cost.

DTIC Science & Technology

1987-04-01

34 111. 1111I .25 IL4 jj 16 MICROCOPY RESOLUTION TEST CHART hut FILE C AIR CoMMNAMN STFF COLLG STUJDET PORTO i COMpUTER SOFTWARE FOR LIFE CYCLE CO879...obsolete), physical life (utility before physically wearing out), or application life (utility in a given function)." (7:5) The costs are usually

Simultaneous cathodoluminescence and electron microscopy cytometry of cellular vesicles labeled with fluorescent nanodiamonds

NASA Astrophysics Data System (ADS)

Nagarajan, Sounderya; Pioche-Durieu, Catherine; Tizei, Luiz H. G.; Fang, Chia-Yi; Bertrand, Jean-Rémi; Le Cam, Eric; Chang, Huan-Cheng; Treussart, François; Kociak, Mathieu

2016-06-01

Light and Transmission Electron Microscopies (LM and TEM) hold potential in bioimaging owing to the advantages of fast imaging of multiple cells with LM and ultrastructure resolution offered by TEM. Integrated or correlated LM and TEM are the current approaches to combine the advantages of both techniques. Here we propose an alternative in which the electron beam of a scanning TEM (STEM) is used to excite concomitantly the luminescence of nanoparticle labels (a process known as cathodoluminescence, CL), and image the cell ultrastructure. This CL-STEM imaging allows obtaining luminescence spectra and imaging ultrastructure simultaneously. We present a proof of principle experiment, showing the potential of this technique in image cytometry of cell vesicular components. To label the vesicles we used fluorescent diamond nanocrystals (nanodiamonds, NDs) of size ~150 nm coated with different cationic polymers, known to trigger different internalization pathways. Each polymer was associated with a type of ND with a different emission spectrum. With CL-STEM, for each individual vesicle, we were able to measure (i) their size with nanometric resolution, (ii) their content in different ND labels, and realize intracellular component cytometry. In contrast to the recently reported organelle flow cytometry technique that requires cell sonication, CL-STEM-based image cytometry preserves the cell integrity and provides a much higher resolution in size. Although this novel approach is still limited by a low throughput, the automatization of data acquisition and image analysis, combined with improved intracellular targeting, should facilitate applications in cell biology at the subcellular level.Light and Transmission Electron Microscopies (LM and TEM) hold potential in bioimaging owing to the advantages of fast imaging of multiple cells with LM and ultrastructure resolution offered by TEM. Integrated or correlated LM and TEM are the current approaches to combine the advantages of both techniques. Here we propose an alternative in which the electron beam of a scanning TEM (STEM) is used to excite concomitantly the luminescence of nanoparticle labels (a process known as cathodoluminescence, CL), and image the cell ultrastructure. This CL-STEM imaging allows obtaining luminescence spectra and imaging ultrastructure simultaneously. We present a proof of principle experiment, showing the potential of this technique in image cytometry of cell vesicular components. To label the vesicles we used fluorescent diamond nanocrystals (nanodiamonds, NDs) of size ~150 nm coated with different cationic polymers, known to trigger different internalization pathways. Each polymer was associated with a type of ND with a different emission spectrum. With CL-STEM, for each individual vesicle, we were able to measure (i) their size with nanometric resolution, (ii) their content in different ND labels, and realize intracellular component cytometry. In contrast to the recently reported organelle flow cytometry technique that requires cell sonication, CL-STEM-based image cytometry preserves the cell integrity and provides a much higher resolution in size. Although this novel approach is still limited by a low throughput, the automatization of data acquisition and image analysis, combined with improved intracellular targeting, should facilitate applications in cell biology at the subcellular level. Electronic supplementary information (ESI) available. See DOI: 10.1039/c6nr01908k

High-resolution imaging by scanning electron microscopy of semithin sections in correlation with light microscopy.

PubMed

Koga, Daisuke; Kusumi, Satoshi; Shodo, Ryusuke; Dan, Yukari; Ushiki, Tatsuo

2015-12-01

In this study, we introduce scanning electron microscopy (SEM) of semithin resin sections. In this technique, semithin sections were adhered on glass slides, stained with both uranyl acetate and lead citrate, and observed with a backscattered electron detector at a low accelerating voltage. As the specimens are stained in the same manner as conventional transmission electron microscopy (TEM), the contrast of SEM images of semithin sections was similar to TEM images of ultrathin sections. Using this technique, wide areas of semithin sections were also observed by SEM, without the obstruction of grids, which was inevitable for traditional TEM. This study also applied semithin section SEM to correlative light and electron microscopy. Correlative immunofluorescence microscopy and immune-SEM were performed in semithin sections of LR white resin-embedded specimens using a FluoroNanogold-labeled secondary antibody. Because LR white resin is hydrophilic and electron stable, this resin is suitable for immunostaining and SEM observation. Using correlative microscopy, the precise localization of the primary antibody was demonstrated by fluorescence microscopy and SEM. This method has great potential for studies examining the precise localization of molecules, including Golgi- and ER-associated proteins, in correlation with LM and SEM. © 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.

Focused ion beam (FIB)/scanning electron microscopy (SEM) in tissue structural research.

PubMed

Leser, Vladka; Milani, Marziale; Tatti, Francesco; Tkalec, Ziva Pipan; Strus, Jasna; Drobne, Damjana

2010-10-01

The focused ion beam (FIB) and scanning electron microscope (SEM) are commonly used in material sciences for imaging and analysis of materials. Over the last decade, the combined FIB/SEM system has proven to be also applicable in the life sciences. We have examined the potential of the focused ion beam/scanning electron microscope system for the investigation of biological tissues of the model organism Porcellio scaber (Crustacea: Isopoda). Tissue from digestive glands was prepared as for conventional SEM or as for transmission electron microscopy (TEM). The samples were transferred into FIB/SEM for FIB milling and an imaging operation. FIB-milled regions were secondary electron imaged, back-scattered electron imaged, or energy dispersive X-ray (EDX) analyzed. Our results demonstrated that FIB/SEM enables simultaneous investigation of sample gross morphology, cell surface characteristics, and subsurface structures. The same FIB-exposed regions were analyzed by EDX to provide basic compositional data. When samples were prepared as for TEM, the information obtained with FIB/SEM is comparable, though at limited magnification, to that obtained from TEM. A combination of imaging, micro-manipulation, and compositional analysis appears of particular interest in the investigation of epithelial tissues, which are subjected to various endogenous and exogenous conditions affecting their structure and function. The FIB/SEM is a promising tool for an overall examination of epithelial tissue under normal, stressed, or pathological conditions.

Short-Range-Order Mineral Physical Protection On Black Carbon Stabilization

NASA Astrophysics Data System (ADS)

Liang, B.; Weng, Y. T.; Wang, C. C.; Song, Y. F.; Lehmann, J.; Wang, C. H.

2015-12-01

Soil organic matter is one of the largest reservoirs in global carbon cycle, and black carbon (BC) represents a chemical resistant component. Black C plays an important role in global climate change. Generally considered recalcitrant due to high aromaticity, the reactive surface and functional groups of BC are crucial for carbon sequestration in soils. Mineral sorption and physical protection is an important mechanism for BC long term stabilization and sequestration in environments. Previous studies on mineral protection of BC were limited to analysis techniques in two-dimensions, for example, by SEM, TEM, and NanoSIMS. Little is known about the scope of organo-mineral association, the in-situ distribution and forms of minerals, and the ultimate interplay of BC and minerals. The aim of this study is to investigate the three-dimensional interaction of organic C and minerals in submicron scale using synchrotron-based Transmission X-ray Microcopy (TXM) and Fourier-Transform Infrared Spectroscopy (FTIR). Abundant poorly-crystallined nano-minerals particles were observed. These short-range-order (SRO) minerals also aggregate into clusters and sheets, and form envelops-like structures on the surface of BC. On top of large surface contact area, the intimate interplay between BC and minerals reinforces the stability of both organic C and minerals, resulting from chemical bonding through cation bridging and ligand exchange. The mineral protection enhances BC stabilization and sequestration and lowers its bioavailability in environment. The results suggest that mineral physical protection for BC sequestration may be more important than previous understanding.

Growth mechanism of surface roughed platinum nanowires through electrodeposition current control and their electrochemical applications

NASA Astrophysics Data System (ADS)

Ruan, Dajiang

The aim of this work is to investigate the effect of current density on the grain size and surface morphology of electrodeposited platinum nanowires and their applications. Platinum (Pt) nanowires were fabricated by a galvanostatic electrodeposition method in a porous anodic alumina oxide (AAO) template with different current densities. Both direct current and pulse current electrodeposition were used to synthesize the Pt nanowires. The grain size and surface morphology of the Pt nanowires were studied by field emission scanning electron microscopy (FE-SEM), transmission electron microcopy (TEM) and X-ray diffraction (XRD). The experimental results showed that the current density was the key factor to control the surface roughness. The surface of the Pt nanowires became rougher and the grain sizes were increased by increasing the current densities. From the experimental results, a growth mechanism of Pt nanowires based on progressive nucleation and crystallization was proposed in order to find out the relationship between the surface morphology and current density. The electrochemical properties and catalytic activities of these surface roughed Pt nanowires were investigated in the detection of H20 2 and for the methanol oxidation. Cyclic voltammograms of Pt nanowire modified electrodes were obtained using a potentiostat, which showed that rougher Pt nanowires have higher response and better activity than that of smooth nanowires. For H202 detection, the effect of scan rate and H202 concentration were studied and it was found that the peak current for hydrogen peroxide reduction became larger with the increasing of either scan rate or H202 concentration. It can be inferred that the process of electrocatalytic hydrogen peroxide reduction may be controlled by diffusion of hydrogen peroxide and the Pt nanowire modified glassy carbon electrode (GCE) is well suited for the detection of H202. From the relationship between the peak current and square root of scan rates for methanol oxidation, it can be inferred that the process of electrocatalytic methanol oxidation was controlled by diffusion of methanol. To understand the effect of the morphological feature on the electrocatalytic activity of the Pt nanowire catalysts, the electrochemically active surface area (ECSA) as a function of deposited current density was investigated, which suggests that Pt nanowire catalysts deposited at highest current density had the most ECSA surface morphology of the Pt nanowires. The chronoamperometric curves and electrochemical impedance spectroscopy (EIS) results confirmed that the Pt nanowire catalyst synthesized at higher current density possessed longer durability and gave more efficient electrochemical performance.

Oxide-free aC/Zr0.65Al0.075Cu0.275/aC phase plates for transmission electron microscopy.

PubMed

Dries, M; Obermair, M; Hettler, S; Hermann, P; Seemann, K; Seifried, F; Ulrich, S; Fischer, R; Gerthsen, D

2018-06-01

Thin-film phase plates (PP) have become a valuable tool for the imaging of organic objects in transmission electron microscopy (TEM). The thin film usually consists of amorphous carbon (aC), which undergoes rapid aging under intense illumination with high-energy electrons. The limited lifetime of aC film PPs calls for alternative PP materials with improved material stability. This work presents thin-film PPs fabricated from the metallic glass alloy Zr 0.65 Al 0.075 Cu 0.275 (ZAC), which was identified as a promising PP material with beneficial properties, such as a large inelastic mean free path. An adverse effect of the ZAC alloy is the formation of a surface oxide layer in ambient air, which reduces the electrical conductivity and causes electrostatic charging in the electron beam. To avoid surface oxidation, the ZAC alloy is enclosed by thin aC layers. The resulting aC/ZAC/aC layer system is used to fabricate Zernike and Hilbert PPs. Phase-contrast TEM imaging is demonstrated for a sample of carbon nanotubes, which show strong contrast enhancement in PP TEM images. Copyright © 2018 Elsevier B.V. All rights reserved.

Recombination-related properties of a-screw dislocations in GaN: A combined CL, EBIC, TEM study

DOE Office of Scientific and Technical Information (OSTI.GOV)

Medvedev, O. S., E-mail: o.s.medvedev@spbu.ru; Mikhailovskii, V. Yu.; IRC for Nanotechnology, Research Park, St.-Petersburg State University

2016-06-17

Cathodoluminescence (CL), electron beam current (EBIC) and transmission electron microscopy (TEM) techniques have been applied to investigate recombination properties and structure of freshly introduced dislocations in low-ohmic GaN crystals. It was confirmed that the only a-screw dislocations exhibited an intense characteristic dislocation-related luminescence (DRL) which persisted up to room temperature and was red-shifted by about 0.3 eV with respect to the band gap energy not only in HVPE but also in MOCVD grown samples. EBIC contrast of the dislocations was found to be temperature independent indicating that the dislocation-related recombination level is situated below 200 meV with respect of conductionmore » band minimum. With the increasing of the magnification of the dislocation TEM cross-sectional images they were found to disappear, probably, due to the recombination enhanced dislocation glide (REDG) under electron beam exposure which was immediately observed in CL investigations on a large scale. The stacking fault ribbon in the core of dissociated a-screw dislocation which form a quantum well for electrons was proposed to play an important role both in DRL spectrum formation and in REDG.« less

Elastically frustrated rehybridization: Origin of chemical order and compositional limits in InGaN quantum wells

NASA Astrophysics Data System (ADS)

Lymperakis, L.; Schulz, T.; Freysoldt, C.; Anikeeva, M.; Chen, Z.; Zheng, X.; Shen, B.; Chèze, C.; Siekacz, M.; Wang, X. Q.; Albrecht, M.; Neugebauer, J.

2018-01-01

Nominal InN monolayers grown by molecular beam epitaxy on GaN(0001) are investigated combining in situ reflection high-energy electron diffraction (RHEED), transmission electron microscopy (TEM), and density functional theory (DFT). TEM reveals a chemical intraplane ordering never observed before. Employing DFT, we identify a novel surface stabilization mechanism elastically frustrated rehybridization, which is responsible for the observed chemical ordering. The mechanism also sets an incorporation barrier for indium concentrations above 25% and thus fundamentally limits the indium content in coherently strained layers.

In situ nanomechanical testing of twinned metals in a transmission electron microscope

DOE PAGES

Li, Nan; Wang, Jiangwei; Mao, Scott; ...

2016-04-01

This paper focuses on in situ transmission electron microscope (TEM) characterization to explore twins in face-centered-cubic and body-centered-cubic monolithic metals, and their impact on the overall mechanical performance. Taking advantage of simultaneous nanomechanical deformation and nanoscale imaging using versatile in situ TEM tools, direct correlation of these unique microscopic defects with macroscopic mechanical performance becomes possible. This article summarizes recent evidence to support the mechanisms related to strengthening and plasticity in metals, including nanotwinned Cu, Ni, Al, Au, and others in bulk, thin film, and nanowire forms.

Dispersion of Co/CNTs via strong electrostatic adsorption method: Thermal treatment effect

DOE Office of Scientific and Technical Information (OSTI.GOV)

Akbarzadeh, Omid, E-mail: omid.akbarzadeh63@gmail.com; Abdullah, Bawadi, E-mail: bawadi-abdullah@petronas.com.my; Subbarao, Duvvuri, E-mail: duvvuri-subbarao@petronas.com.my

The effect of different thermal treatment temperature on the structure of multi-walled carbon nanotubes (MWCNTs) and Co particle dispersion on CNTs support is studied using Strong electrostatic adsorption (SEA) method. The samples tested by N{sub 2}-adsorption, field emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). N{sub 2}-adsorption results showed BET surface area increased using thermal treatment and TEM images showed that increasing the thermal treatment temperature lead to flaky CNTs and defects introduced on the outer surface and Co particle dispersion increased.

In situ nanomechanical testing of twinned metals in a transmission electron microscope

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li, Nan; Wang, Jiangwei; Mao, Scott

This paper focuses on in situ transmission electron microscope (TEM) characterization to explore twins in face-centered-cubic and body-centered-cubic monolithic metals, and their impact on the overall mechanical performance. Taking advantage of simultaneous nanomechanical deformation and nanoscale imaging using versatile in situ TEM tools, direct correlation of these unique microscopic defects with macroscopic mechanical performance becomes possible. This article summarizes recent evidence to support the mechanisms related to strengthening and plasticity in metals, including nanotwinned Cu, Ni, Al, Au, and others in bulk, thin film, and nanowire forms.

Thermophysical ESEM and TEM Characterization of Carbon Fibers CTE, Spectroscopy and Roughness Studies at High Temperatures

NASA Technical Reports Server (NTRS)

Ochoa, Ozden O.

2004-01-01

Accurate determination of the transverse properties of carbon fibers is important for assessment and prediction of local material as well as global structural response of composite components. However the measurements are extremely difficult due to the very small diameters of the fibers (few microns only) and must be conducted within a microscope. In this work, environmental scanning electron microscope (ESEM) and transmission electron microscope (TEM) are used to determine the transverse coefficient of thermal expansion of different carbon fibers as a function of temperature.

Static and Dynamic Electron Microscopy Investigations at the Atomic and Ultrafast Scales

NASA Astrophysics Data System (ADS)

Suri, Pranav Kumar

Advancements in the electron microscopy capabilities - aberration-corrected imaging, monochromatic spectroscopy, direct-electron detectors - have enabled routine visualization of atomic-scale processes with millisecond temporal resolutions in this decade. This, combined with progress in the transmission electron microscopy (TEM) specimen holder technology and nanofabrication techniques, allows comprehensive experiments on a wide range of materials in various phases via in situ methods. The development of ultrafast (sub-nanosecond) time-resolved TEM with ultrafast electron microscopy (UEM) has further pushed the envelope of in situ TEM to sub-nanosecond temporal resolution while maintaining sub-nanometer spatial resolution. A plethora of materials phenomena - including electron-phonon coupling, phonon transport, first-order phase transitions, bond rotation, plasmon dynamics, melting, and dopant atoms arrangement - are not yet clearly understood and could be benefitted with the current in situ TEM capabilities having atomic-level and ultrafast precision. Better understanding of these phenomena and intrinsic material dynamics (e.g. how phonons propagate in a material, what time-scales are involved in a first-order phase transition, how fast a material melts, where dopant atoms sit in a crystal) in new-generation and technologically important materials (e.g. two-dimensional layered materials, semiconductor and magnetic devices, rare-earth-element-free permanent magnets, unconventional superconductors) could bring a paradigm shift in their electronic, structural, magnetic, thermal and optical applications. Present research efforts, employing cutting-edge static and dynamic in situ electron microscopy resources at the University of Minnesota, are directed towards understanding the atomic-scale crystallographic structural transition and phonon transport in an iron-pnictide parent compound LaFeAsO, studying the mechanical stability of fast moving hard-drive heads in heat-assisted magnetic recording (HAMR) technology, exploring the possibility of ductile ceramics in magnesium oxide (MgO) nanomaterials, and revealing the atomic-structure of newly discovered rare-earth-element-free iron nitride (FeN) magnetic materials. Via atomic-resolution imaging and electron diffraction coupled with in situ TEM cooling on LaFeAsO, it was found that additional effects not related to the structural transition, namely dynamical scattering and electron channeling, can give signatures reminiscent of those typically associated with the symmetry change. UEM studies on LaFeAsO revealed direct, real-space imaging of the emergence and evolution of acoustic phonons and resolved dispersion behavior during propagation and scattering. Via UEM bright-field imaging, megahertz vibrational frequencies were observed upon laser-illumination in TEM specimens made out of HAMR devices which could be detrimental to their long-term thermal and structural reliability. Compression testing of 100-350 nm single-crystal MgO nanocubes shows size-dependent stresses and engineering strains of 4-13.8 GPa and 0.046-0.221 respectively at the first signs of yield accompanied by an absence of brittle fracture, which is a significant increase in plasticity of a brittle ceramic material. Atomic-scale characterization of FeN phases show that it is possible to detect interstitial locations of low atomic-number nitrogen atoms in iron crystal and hints at a development of novel routes (without involving rare-earth elements) for bulk permanent magnet synthesis.

Rapid misfit dislocation characterization in heteroepitaxial III-V/Si thin films by electron channeling contrast imaging

DOE Office of Scientific and Technical Information (OSTI.GOV)

Carnevale, Santino D.; Deitz, Julia I.; Carlin, John A.

Electron channeling contrast imaging (ECCI) is used to characterize misfit dislocations in heteroepitaxial layers of GaP grown on Si(100) substrates. Electron channeling patterns serve as a guide to tilt and rotate sample orientation so that imaging can occur under specific diffraction conditions. This leads to the selective contrast of misfit dislocations depending on imaging conditions, confirmed by dynamical simulations, similar to using standard invisibility criteria in transmission electron microscopy (TEM). The onset and evolution of misfit dislocations in GaP films with varying thicknesses (30 to 250 nm) are studied. This application simultaneously reveals interesting information about misfit dislocations in GaP/Si layersmore » and demonstrates a specific measurement for which ECCI is preferable versus traditional plan-view TEM.« less

Two novel approaches to study arthropod anatomy by using dualbeam FIB/SEM.

PubMed

Di Giulio, Andrea; Muzzi, Maurizio

2018-03-01

Transmission Electron Microscopy (TEM) has always been the conventional method to study arthropod ultrastructure, while the use of Scanning Electron Microscopy (SEM) was mainly devoted to the examination of the external cuticular structures by secondary electrons. The new generation field emission SEMs are capable to generate images at sub-cellular level, comparable to TEM images employing backscattered electrons. The potential of this kind of acquisition becomes very powerful in the dual beam FIB/SEM where the SEM column is combined with a Focused Ion Beam (FIB) column. FIB uses ions as a nano-scalpel to slice samples fixed and embedded in resin, replacing traditional ultramicrotomy. We here present two novel methods, which optimize the use of FIB/SEM for studying arthropod anatomy. Copyright © 2017 Elsevier Ltd. All rights reserved.

Interlayer coupling and electronic structure of misfit-layered bismuth-based cobaltites

NASA Astrophysics Data System (ADS)

Takakura, Sho-ichi; Yamamoto, Isamu; Tanaka, Eishi; Azuma, Junpei; Maki, Makoto

2017-05-01

The [Bi2M2O4] pCoO2 materials (M =Ca , Sr, and Ba) were studied to clarify the effect of the lattice incommensurability on electronic properties using angle-resolved photoemission spectroscopy and transmission electron microscopy (TEM). Results show that the insulating behavior is characterized by a spectral weight for binding energies higher than 2.0 eV. Moreover, the spectral shape is modified as a function of the incident photon energy, demonstrating a close relationship between the electrical properties and interlayer coupling. TEM results show that the effect of the lattice mismatch differs for different misfit parameters p . We therefore conclude that the carrier concentration and the chemical environment at the misfit interface, which depend on the degree of incommensurability, mutually determine the electronic properties of the system.

Nanobelt formation of magnesium hydroxide sulfate hydrate via a soft chemistry process.

PubMed

Zhou, Zhengzhi; Sun, Qunhui; Hu, Zeshan; Deng, Yulin

2006-07-13

The nanobelt formation of magnesium hydroxide sulfate hydrate (MHSH) via a soft chemistry approach using carbonate salt and magnesium sulfate as reactants was successfully demonstrated. X-ray diffraction (XRD), energy dispersion X-ray spectra (EDS), selected area electron diffraction (SAED), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) analysis revealed that the MHSH nanobelts possessed a thin belt structure (approximately 50 nm in thickness) and a rectangular cross profile (approximately 200 nm in width). The MHSH nanobelts suffered decomposition under electron beam irradiation during TEM observation and formed MgO with the pristine nanobelt morphology preserved. The formation process of the MHSH nanobelts was studied by tracking the morphology of the MHSH nanobelts during the reaction. A possible chemical reaction mechanism is proposed.

Double-tilt in situ TEM holder with ultra-high stability.

PubMed

Xu, Mingjie; Dai, Sheng; Blum, Thomas; Li, Linze; Pan, Xiaoqing

2018-05-06

A double tilting holder with high stability is essential for acquiring atomic-scale information by transmission electron microscopy (TEM), but the availability of such holders for in situ TEM studies under various external stimuli is limited. Here, we report a unique design of seal-bearing components that provides ultra-high stability and multifunctionality (including double tilting) in an in situ TEM holder. The seal-bearing subsystem provides superior vibration damping and electrical insulation while maintaining excellent vacuum sealing and small form factor. A wide variety of in situ TEM applications including electrical measurement, STM mapping, photovoltaic studies, and CL spectroscopy can be performed on this platform with high spatial resolution imaging and electrical sensitivity at the pA scale. Copyright © 2018 Elsevier B.V. All rights reserved.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Guetaz, Laure; Lopez-Haro, M.; Escribano, S.

Investigation of membrane/electrode assembly (MEA) microstructure has become an essential step to optimize the MEA components and manufacturing processes or to study the MEA degradation. For these investigations, transmission electron microscopy (TEM) is a tool of choice as it provides direct imaging of the different components. TEM is then widely used for analyzing the catalyst nanoparticles and their carbon support. However, the ionomer inside the electrode is more difficult to be imaged. The difficulties come from the fact that the ionomer forms an ultrathin layer surrounding the carbon particles and in addition, these two components, having similar density, present nomore » difference in contrast. In this paper, we show how the recent progresses in TEM techniques as spherical aberration (Cs) corrected HRTEM, electron tomography and X-EDS elemental mapping provide new possibilities for imaging this ionomer network and consequently to study its degradation.« less

RBS, TEM and SEM Characterization of Gold Nanoclusters in TiO2(110)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shutthanandan, V; Zhang, Yanwen; Wang, Chong M.

2004-05-01

Nucleation of gold nanoclusters in TiO2(110) single crystal using ion implantation and subsequent annealing were studied by Rutherford backscattering spectrometry /channeling (RBS/C), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Approximately 1000 Au2+/nm2 was implanted at room temperature in TiO2(110) substrates. TEM and SEM measurements revel that rounded nanoclusters were formed during the implantation. In contrast subsequent annealing in air for 10 hours at 1275 K promoted the formation of faceted (rectangular shaped) Au nano structures in TiO2. RBS channeling measurements further reveled that Au atoms randomly occupied in the host TiO2 lattice during the implantation. However, some ofmore » the gold atoms were moved into the Ti lattice position after annealing.« less

Correlative Light- and Electron Microscopy Using Quantum Dot Nanoparticles.

PubMed

Killingsworth, Murray C; Bobryshev, Yuri V

2016-08-07

A method is described whereby quantum dot (QD) nanoparticles can be used for correlative immunocytochemical studies of human pathology tissue using widefield fluorescence light microscopy and transmission electron microscopy (TEM). To demonstrate the protocol we have immunolabeled ultrathin epoxy sections of human somatostatinoma tumor using a primary antibody to somatostatin, followed by a biotinylated secondary antibody and visualization with streptavidin conjugated 585 nm cadmium-selenium (CdSe) quantum dots (QDs). The sections are mounted on a TEM specimen grid then placed on a glass slide for observation by widefield fluorescence light microscopy. Light microscopy reveals 585 nm QD labeling as bright orange fluorescence forming a granular pattern within the tumor cell cytoplasm. At low to mid-range magnification by light microscopy the labeling pattern can be easily recognized and the level of non-specific or background labeling assessed. This is a critical step for subsequent interpretation of the immunolabeling pattern by TEM and evaluation of the morphological context. The same section is then blotted dry and viewed by TEM. QD probes are seen to be attached to amorphous material contained in individual secretory granules. Images are acquired from the same region of interest (ROI) seen by light microscopy for correlative analysis. Corresponding images from each modality may then be blended to overlay fluorescence data on TEM ultrastructure of the corresponding region.

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

NASA Astrophysics Data System (ADS)

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

2013-09-01

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

PROPOSED ASTM METHOD FOR THE DETERMINATION OF ASBESTOS IN AIR BY TEM AND INFORMATION ON INTERFERING FIBERS

EPA Science Inventory

The draft of the ASTM Test Method for air entitled: "Airborne Asbestos Concentration in Ambient and Indoor Atmospheres as Determined by Transmission Electron Microscopy Direct Transfer (TEM)" (ASTM Z7077Z) is an adaptation of the International Standard, ISO 10312. It is currently...

Correlative transmission electron microscopy and electrical properties study of switchable phase-change random access memory line cells

DOE Office of Scientific and Technical Information (OSTI.GOV)

Oosthoek, J. L. M.; Kooi, B. J., E-mail: B.J.Kooi@rug.nl; Voogt, F. C.

2015-02-14

Phase-change memory line cells, where the active material has a thickness of 15 nm, were prepared for transmission electron microscopy (TEM) observation such that they still could be switched and characterized electrically after the preparation. The result of these observations in comparison with detailed electrical characterization showed (i) normal behavior for relatively long amorphous marks, resulting in a hyperbolic dependence between SET resistance and SET current, indicating a switching mechanism based on initially long and thin nanoscale crystalline filaments which thicken gradually, and (ii) anomalous behavior, which holds for relatively short amorphous marks, where initially directly a massive crystalline filament ismore » formed that consumes most of the width of the amorphous mark only leaving minor residual amorphous regions at its edges. The present results demonstrate that even in (purposely) thick TEM samples, the TEM sample preparation hampers the probability to observe normal behavior and it can be debated whether it is possible to produce electrically switchable TEM specimen in which the memory cells behave the same as in their original bulk embedded state.« less

Correlative transmission electron microscopy and electrical properties study of switchable phase-change random access memory line cells

NASA Astrophysics Data System (ADS)

Oosthoek, J. L. M.; Voogt, F. C.; Attenborough, K.; Verheijen, M. A.; Hurkx, G. A. M.; Gravesteijn, D. J.; Kooi, B. J.

2015-02-01

Phase-change memory line cells, where the active material has a thickness of 15 nm, were prepared for transmission electron microscopy (TEM) observation such that they still could be switched and characterized electrically after the preparation. The result of these observations in comparison with detailed electrical characterization showed (i) normal behavior for relatively long amorphous marks, resulting in a hyperbolic dependence between SET resistance and SET current, indicating a switching mechanism based on initially long and thin nanoscale crystalline filaments which thicken gradually, and (ii) anomalous behavior, which holds for relatively short amorphous marks, where initially directly a massive crystalline filament is formed that consumes most of the width of the amorphous mark only leaving minor residual amorphous regions at its edges. The present results demonstrate that even in (purposely) thick TEM samples, the TEM sample preparation hampers the probability to observe normal behavior and it can be debated whether it is possible to produce electrically switchable TEM specimen in which the memory cells behave the same as in their original bulk embedded state.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Thangadurai, P.; Lumelsky, Yulia; Silverstein, Michael S.

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 PMMAmore » 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.« less

Distortion of DNA Origami on Graphene Imaged with Advanced TEM Techniques.

PubMed

Kabiri, Yoones; Ananth, Adithya N; van der Torre, Jaco; Katan, Allard; Hong, Jin-Yong; Malladi, Sairam; Kong, Jing; Zandbergen, Henny; Dekker, Cees

2017-08-01

While graphene may appear to be the ultimate support membrane for transmission electron microscopy (TEM) imaging of DNA nanostructures, very little is known if it poses an advantage over conventional carbon supports in terms of resolution and contrast. Microscopic investigations are carried out on DNA origami nanoplates that are supported onto freestanding graphene, using advanced TEM techniques, including a new dark-field technique that is recently developed in our lab. TEM images of stained and unstained DNA origami are presented with high contrast on both graphene and amorphous carbon membranes. On graphene, the images of the origami plates show severe unwanted distortions, where the rectangular shape of the nanoplates is significantly distorted. From a number of comparative control experiments, it is demonstrated that neither staining agents, nor screening ions, nor the level of electron-beam irradiation cause this distortion. Instead, it is suggested that origami nanoplates are distorted due to hydrophobic interaction of the DNA bases with graphene upon adsorption of the DNA origami nanoplates. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Radiation induced deposition of copper nanoparticles inside the nanochannels of poly(acrylic acid)-grafted poly(ethylene terephthalate) track-etched membranes

NASA Astrophysics Data System (ADS)

Korolkov, Ilya V.; Güven, Olgun; Mashentseva, Anastassiya A.; Atıcı, Ayse Bakar; Gorin, Yevgeniy G.; Zdorovets, Maxim V.; Taltenov, Abzal A.

2017-01-01

Poly(ethylene terephthalate) PET, track-etched membranes (TeMs) with 400 nm average pore size were UV-grafted with poly(acrylic acid) (PAA) after oxidation of inner surfaces by H2O2/UV system. Carboxylate groups of grafted PAA chains were easily complexed with Cu2+ ions in aqueous solutions. These ions were converted into metallic copper nanoparticles (NPs) by radiation-induced reduction of copper ions in aqueous-alcohol solution by gamma rays in the dose range of 46-250 kGy. Copper ions chelating with -COOH groups of PAA chains grafted on PET TeMs form polymer-metal ion complex that prevent the formation of agglomerates during reduction of copper ions to metallic nanoparticles. The detailed analysis by X-Ray diffraction technique (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDX) confirmed the deposition of copper nanoparticles with the average size of 70 nm on the inner surface of nanochannels of PET TeMs. Samples were also investigated by FTIR, ESR spectroscopies to follow copper ion reduction.

Experimental investigation of solid by-product as sensible heat storage material: Characterization and corrosion study

NASA Astrophysics Data System (ADS)

Ortega-Fernández, Iñigo; Faik, Abdessamad; Mani, Karthik; Rodriguez-Aseguinolaza, Javier; D'Aguanno, Bruno

2016-05-01

The experimental investigation of water cooled electrical arc furnace (EAF) slag used as filler material in the storage tank for sensible heat storage application was demonstrated in this study. The physicochemical and thermal properties of the tested slags were characterized by using X-ray diffraction, scanning electron microcopy, Fourier transform infrared spectroscopy, Raman spectroscopy and laser flash analysis, respectively. In addition, the chemical compatibility between slags and molten nitrate salt (60 wt. % NaNO3 and 40 wt. % KNO3) was investigated at 565 °C for 500 hrs. The obtained results were clearly demonstrated that the slags showed a good corrosion resistance in direct contact with molten salt at elevated temperature. The present study was clearly indicated that a low-cost filler material used in the storage tank can significantly reduce the overall required quantities of the relatively higher cost molten salt and consequently reduce the overall cost of the electricity production.

Electrochemical performance of La2O3/Li2O/TiO2 nano-particle coated cathode material LiFePO4.

PubMed

Wang, Hong; Yang, Chi; Liu, Shu-Xin

2014-09-01

Cathode material, LiFePO4 was modified by coating with a thin layer of La2O3/Li2O/TiO2 nano-particles for improving its performance for lithium ion batteries. The morphology and structure of the modified cathode material were characterized by powder X-ray diffraction, scanning electron microcopy and AES. The performance of the battery with the modified cathode material, including cycling stability, C-rate discharge was examined. The results show that the battery composed of the coated cathode materials can discharge at a large current density and show stable cycling performance in the range from 2.5 to 4.0 V. The rate of Li ion diffusion increases in the battery with the La2O3/Li2O/TiO2-coated LiFePO4 as a cathode and the coating layer may acts as a faster ion conductor (La(2/3-x)Li(3x)TiO3).

Structural and magnetic properties of Fe and carbon nanotubes derived from coconut shells

NASA Astrophysics Data System (ADS)

Qadri, S. B.; Gorzkowski, E. P.; Bussmann, K.; Rath, B. B.; Feng, J.

2018-05-01

Ferric oxide (Fe2O3) was directly reduced to metallic Fe using the carbon source from the coconut shells at temperatures above 1400 °C in argon gas atmospheres. X-ray diffraction analysis showed the presence of α-, γ- phases of Fe in addition to the presence of carbon nanotubes (CNTs). By selecting the appropriate ratios of coconut shell powder to Fe2O3, it is demonstrated that pure Fe is produced without any residual ferric oxide. The quantitative analysis of each of the Fe phases and carbon nanotubes was dependent on the temperature and the duration of processing at high temperature. Transmission electron microcopy results showed copious amount of carbon nanotubes in the samples. Magnetic property measurements suggested that, the average magnetic moment is consistent with presence of α-phase and the ferromagnetic γ-phase of Fe. This novel method of producing pure α- and γ-Fe in the presence of carbon nanotubes using coconut shells has potential applications as nanocomposites.

Electron holography—basics and applications

NASA Astrophysics Data System (ADS)

Lichte, Hannes; Lehmann, Michael

2008-01-01

Despite the huge progress achieved recently by means of the corrector for aberrations, allowing now a true atomic resolution of 0.1 nm, hence making it an unrivalled tool for nanoscience, transmission electron microscopy (TEM) suffers from a severe drawback: in a conventional electron micrograph only a poor phase contrast can be achieved, i.e. phase structures are virtually invisible. Therefore, conventional TEM is nearly blind for electric and magnetic fields, which are pure phase objects. Since such fields provoked by the atomic structure, e.g. of semiconductors and ferroelectrics, largely determine the solid state properties, hence the importance for high technology applications, substantial object information is missing. Electron holography in TEM offers the solution: by superposition with a coherent reference wave, a hologram is recorded, from which the image wave can be completely reconstructed by amplitude and phase. Now the object is displayed quantitatively in two separate images: one representing the amplitude, the other the phase. From the phase image, electric and magnetic fields can be determined quantitatively in the range from micrometre down to atomic dimensions by all wave optical methods that one can think of, both in real space and in Fourier space. Electron holography is pure wave optics. Therefore, we discuss the basics of coherence and interference, the implementation into a TEM, the path of rays for recording holograms as well as the limits in lateral and signal resolution. We outline the methods of reconstructing the wave by numerical image processing and procedures for extracting the object properties of interest. Furthermore, we present a broad spectrum of applications both at mesoscopic and atomic dimensions. This paper gives an overview of the state of the art pointing at the needs for further development. It is also meant as encouragement for those who refrain from holography, thinking that it can only be performed by specialists in highly specialized laboratories. In fact, a modern TEM built for atomic resolution and equipped with a field emitter or a Schottky emitter, well aligned by a skilled operator, can deliver good holograms. Running commercially available image processing software and mathematics programs on a laptop-computer is sufficient for reconstruction of the amplitude and phase images and extracting desirable object information.

Resolution Quality and Atom Positions in Sub-?ngstr?m Electron Microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

O'Keefe, Michael A.; Allard Jr, Lawrence Frederick; Blom, Douglas Allen

2005-01-01

John Cowley pioneered use of transmission electron microscopy (TEM) for high-resolution imaging and helped spur improvements in resolution that enabled researchers to pinpoint the positions of all but the lightest atoms within a crystal structure. Sub-{angstrom} capabilities allow imaging of even the lightest atoms. Initially achieved with software aberration correction (focal-series reconstruction of the specimen exit-surface wave), sub-{angstrom} imaging will become commonplace for next-generation electron microscopes with hardware-corrected lenses and monochromated electron beams. Currently, advanced HR-TEMs can image columns of light atoms (carbon, oxygen, nitrogen) in complex structures, including the lithium atoms present in battery materials. The ability to determinemore » whether an image peak represents one single atom (or atom column) instead of several depends on the resolution of the HR-(S)TEM. Rayleigh's resolution criterion, an accepted standard in optics, was derived as a means for judging when two image intensity peaks from two sources of light (stars) are distinguishable from a single source. Atom spacings closer than the Rayleigh limit have been resolved in HR-TEM, suggesting that it may be useful to consider other limits, such as the Sparrow resolution criterion. From the viewpoint of the materials scientist, it is important to be able to use the image to determine whether an image feature represents one or more atoms (resolution), and where the atoms (or atom columns) are positioned relative to one another (resolution quality). When atoms and the corresponding image peaks are separated by more than the Rayleigh limit of the HR-(S)TEM, it is possible to adjust imaging parameters so that relative peak positions in the image correspond to relative atom positions in the specimen. When atoms are closer than the Rayleigh limit, we must find the relationship of the peak position to the atom position by peak fitting or, if we have a suitable model, by image simulation.« less

Stop-Frame Filming and Discovery of Reactions at the Single-Molecule Level by Transmission Electron Microscopy

PubMed Central

2017-01-01

We report an approach, named chemTEM, to follow chemical transformations at the single-molecule level with the electron beam of a transmission electron microscope (TEM) applied as both a tunable source of energy and a sub-angstrom imaging probe. Deposited on graphene, disk-shaped perchlorocoronene molecules are precluded from intermolecular interactions. This allows monomolecular transformations to be studied at the single-molecule level in real time and reveals chlorine elimination and reactive aryne formation as a key initial stage of multistep reactions initiated by the 80 keV e-beam. Under the same conditions, perchlorocoronene confined within a nanotube cavity, where the molecules are situated in very close proximity to each other, enables imaging of intermolecular reactions, starting with the Diels–Alder cycloaddition of a generated aryne, followed by rearrangement of the angular adduct to a planar polyaromatic structure and the formation of a perchlorinated zigzag nanoribbon of graphene as the final product. ChemTEM enables the entire process of polycondensation, including the formation of metastable intermediates, to be captured in a one-shot “movie”. A molecule with a similar size and shape but with a different chemical composition, octathio[8]circulene, under the same conditions undergoes another type of polycondensation via thiyl biradical generation and subsequent reaction leading to polythiophene nanoribbons with irregular edges incorporating bridging sulfur atoms. Graphene or carbon nanotubes supporting the individual molecules during chemTEM studies ensure that the elastic interactions of the molecules with the e-beam are the dominant forces that initiate and drive the reactions we image. Our ab initio DFT calculations explicitly incorporating the e-beam in the theoretical model correlate with the chemTEM observations and give a mechanism for direct control not only of the type of the reaction but also of the reaction rate. Selection of the appropriate e-beam energy and control of the dose rate in chemTEM enabled imaging of reactions on a time frame commensurate with TEM image capture rates, revealing atomistic mechanisms of previously unknown processes. PMID:28191929

Structural, magnetic and electronic structure properties of Co doped ZnO nanoparticles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kumar, Shalendra, E-mail: shailuphy@gmail.com; School of Materials Science and Engineering, Changwon National University, Changwon, Gyeongnam 641-773; Song, T.K., E-mail: tksong@changwon.ac.kr

Highlights: • XRD and HR-TEM results show the single phase nature of Co doped ZnO nanoparticles. • XMCD and dc magnetization results indicate the RT-FM in Co doped ZnO nanoparticles. • Co L{sub 3,2} NEXAFS spectra infer that Co ions are in 2+ valence state. • O K edge NEXAFS spectra show that O vacancy increases with Co doping in ZnO. - Abstract: We reported structural, magnetic and electronic structure studies of Co doped ZnO nanoparticles. Doping of Co ions in ZnO host matrix has been studied and confirmed using various methods; such as X-ray diffraction (XRD), field emission scanningmore » electron microscopy (FE-SEM), energy dispersed X-ray (EDX), high resolution transmission electron microscopy (HR-TEM), Fourier transform infrared spectroscopy (FT-IR), near edge X-ray absorption fine structure (NEXAFS) spectroscopy, magnetic hysteresis loop measurements and X-ray magnetic circular dichroism (XMCD). From the XRD and HR-TEM results, it is observed that Co doped ZnO nanoparticles have single phase nature with wurtzite structure and exclude the possibility of secondary phase formation. FE-SEM and TEM micrographs show that pure and Co doped nanoparticles are nearly spherical in shape. O K edge NEXAFS spectra indicate that O vacancies increase with Co doping. The Co L{sub 3,2} edge NEXAFS spectra revealed that Co ions are in 2+ valence state. DC magnetization hysteresis loops and XMCD results clearly showed the intrinsic origin of temperature ferromagnetism in Co doped ZnO nanoparticles.« less

Development and Application of Operando TEM to a Ruthenium Catalyst for CO Oxidation

NASA Astrophysics Data System (ADS)

Miller, Benjamin Kyle

Operando transmission electron microscopy (TEM) is an extension of in-situ TEM in which the performance of the material being observed is measured simultaneously. This is of great value, since structure-performance relationships lie at the heart of materials science. For catalyst materials, like the SiO2-supported Ru nanoparticles studied, the important performance metric, catalyst activity, is measured inside the microscope by determining the gas composition during imaging. This is accomplished by acquisition of electron energy loss spectra (EELS) of the gas in the environmental TEM while catalysis is taking place. In this work, automated methods for rapidly quantifying low-loss and core-loss EELS of gases were developed. A new sample preparation method was also established to increase catalytic conversion inside a differentially-pumped environmental TEM, and the maximum CO conversion observed was about 80%. A system for mixing gases and delivering them to the environmental TEM was designed and built, and a method for locating and imaging nanoparticles in zone axis orientations while minimizing electron dose rate was determined. After atomic resolution images of Ru nanoparticles observed during CO oxidation were obtained, the shape and surface structures of these particles was investigated. A Wulff model structure for Ru particles was compared to experimental images both by manually rotating the model, and by automatically determining a matching orientation using cross-correlation of shape signatures. From this analysis, it was determined that most Ru particles are close to Wulff-shaped during CO oxidation. While thick oxide layers were not observed to form on Ru during CO oxidation, thin RuO2 layers on the surface of Ru nanoparticles were imaged with atomic resolution for the first time. The activity of these layers is discussed in the context of the literature on the subject, which has thus far been inconclusive. We conclude that disordered oxidized ruthenium, rather than crystalline RuO2 is the most active species.

Inducing fluorescence of uranyl acetate as a dual-purpose contrast agent for correlative light-electron microscopy with nanometre precision.

PubMed

Tuijtel, Maarten W; Mulder, Aat A; Posthuma, Clara C; van der Hoeven, Barbara; Koster, Abraham J; Bárcena, Montserrat; Faas, Frank G A; Sharp, Thomas H

2017-09-05

Correlative light-electron microscopy (CLEM) combines the high spatial resolution of transmission electron microscopy (TEM) with the capability of fluorescence light microscopy (FLM) to locate rare or transient cellular events within a large field of view. CLEM is therefore a powerful technique to study cellular processes. Aligning images derived from both imaging modalities is a prerequisite to correlate the two microscopy data sets, and poor alignment can limit interpretability of the data. Here, we describe how uranyl acetate, a commonly-used contrast agent for TEM, can be induced to fluoresce brightly at cryogenic temperatures (-195 °C) and imaged by cryoFLM using standard filter sets. This dual-purpose contrast agent can be used as a general tool for CLEM, whereby the equivalent staining allows direct correlation between fluorescence and TEM images. We demonstrate the potential of this approach by performing multi-colour CLEM of cells containing equine arteritis virus proteins tagged with either green- or red-fluorescent protein, and achieve high-precision localization of virus-induced intracellular membrane modifications. Using uranyl acetate as a dual-purpose contrast agent, we achieve an image alignment precision of ~30 nm, twice as accurate as when using fiducial beads, which will be essential for combining TEM with the evolving field of super-resolution light microscopy.

Evolution of the substructure of a novel 12% Cr steel under creep conditions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yadav, Surya Deo, E-mail: surya.yadav@tugraz.at; Kalácska, Szilvia, E-mail: kalacska@metal.elte.hu; Dománková, Mária, E-mail: maria.domankova@stuba.sk

2016-05-15

In this work we study the microstruture evolution of a newly developed 12% Cr martensitic/ferritic steel in as-received condition and after creep at 650 °C under 130 MPa and 80 MPa. The microstructure is described as consisting of mobile dislocations, dipole dislocations, boundary dislocations, precipitates, lath boundaries, block boundaries, packet boundaries and prior austenitic grain boundaries. The material is characterized employing light optical microscopy (LOM), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and electron backscatter diffraction (EBSD). TEM is used to characterize the dislocations (mobile + dipole) inside the subgrains and XRD measurements are used tomore » the characterize mobile dislocations. Based on the subgrain boundary misorientations obtained from EBSD measurements, the boundary dislocation density is estimated. The total dislocation density is estimated for the as-received and crept conditions adding the mobile, boundary and dipole dislocation densities. Additionally, the subgrain size is estimated from the EBSD measurements. In this publication we propose the use of three characterization techniques TEM, XRD and EBSD as necessary to characterize all type of dislocations and quantify the total dislocation densty in martensitic/ferritic steels. - Highlights: • Creep properties of a novel 12% Cr steel alloyed with Ta • Experimental characterization of different types of dislocations: mobile, dipole and boundary • Characterization and interpretation of the substructure evolution using unique combination of TEM, XRD and EBSD.« less

Homocores, Cores and Operational Inefficiency in Superadditive N-Person Games.

DTIC Science & Technology

1983-02-01

MICROCOPY RESOLUTION TEST CHART NATIONAL BUREAU OF STANDARDS -963-A ’I .. . Re,, arch Report CCS 456 HOMOCO.S S, WOkLS AND OPLP AI [OW \\l INEFFICIENCY...modifications were made in L. Johanssen’s working papers at The Econometric Institute of The University of Oslo in 1981 and in Aumann [1981]. Yet we know

Microcopying wildland maps for distribution and scanner digitizing

Treesearch

Elliot L Amidon; Joyce E. Dye

1976-01-01

Maps for wildland resource inventory and managament purposes typically show vegetation types, soils, and other areal information. For field work, maps must be large-scale. For safekeeping and compact storage, however, they can be reduced onto film, ready to be enlarged on demand by office viewers. By meeting certain simple requirements, film images are potential input...

Radar Backscatter Study of Sea Ice.

DTIC Science & Technology

1980-02-01

CRINC/RS-TR-331-14 N END 11111 .0 W 2.0 =il I.0 i IIIB ii 2 IIIII Bill IlIIIl 8 [(25 I 4 Bi l 1.6 MICROCOPY RE SOL UTIION TEIST CHART 177 slopes...Research, 1978. 51. Continentai Shelf Data Systems, Beaufort Sea-Arctic Coast: Oceano - graphic and Climatologic Data, Vol. 1, Continental Shelf Data Systems

Electron Microscopist | Center for Cancer Research

Cancer.gov

PROGRAM DESCRIPTION The Cancer Research Technology Program (CRTP) develops and implements emerging technology, cancer biology expertise and research capabilities to accomplish NCI research objectives. The CRTP is an outward-facing, multi-disciplinary hub purposed to enable the external cancer research community and provides dedicated support to NCI’s intramural Center for Cancer Research (CCR). The dedicated units provide electron microscopy, protein characterization, protein expression, optical microscopy and genetics. These research efforts are an integral part of CCR at the Frederick National Laboratory for Cancer Research (FNLCR). CRTP scientists also work collaboratively with intramural NCI investigators to provide research technologies and expertise. KEY ROLES/RESPONSIBILITIES - THIS POSITION IS CONTINGENT UPON FUNDING APPROVAL The Electron Microscopist will: Operate ultramicrotomes (Leica) and other instrumentation related to the preparation of embedded samples for EM (TEM and SEM) Operate TEM microscopes, (specifically Hitachi, FEI T20 and FEI T12) as well as SEM microscopes (Hitachi); task will include loading samples, screening, and performing data collection for a variety of samples: from cells to proteins Manage maintenance for the TEM and SEM microscopes Provide technical advice to investigators on sample preparation and data collection

Multiple double cross-section transmission electron microscope sample preparation of specific sub-10 nm diameter Si nanowire devices.

PubMed

Gignac, Lynne M; Mittal, Surbhi; Bangsaruntip, Sarunya; Cohen, Guy M; Sleight, Jeffrey W

2011-12-01

The ability to prepare multiple cross-section transmission electron microscope (XTEM) samples from one XTEM sample of specific sub-10 nm features was demonstrated. Sub-10 nm diameter Si nanowire (NW) devices were initially cross-sectioned using a dual-beam focused ion beam system in a direction running parallel to the device channel. From this XTEM sample, both low- and high-resolution transmission electron microscope (TEM) images were obtained from six separate, specific site Si NW devices. The XTEM sample was then re-sectioned in four separate locations in a direction perpendicular to the device channel: 90° from the original XTEM sample direction. Three of the four XTEM samples were successfully sectioned in the gate region of the device. From these three samples, low- and high-resolution TEM images of the Si NW were taken and measurements of the NW diameters were obtained. This technique demonstrated the ability to obtain high-resolution TEM images in directions 90° from one another of multiple, specific sub-10 nm features that were spaced 1.1 μm apart.

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

NASA Technical Reports Server (NTRS)

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.

The importance of transmission electron microscopy analysis of spermatozoa: Diagnostic applications and basic research.

PubMed

Moretti, Elena; Sutera, Gaetano; Collodel, Giulia

2016-06-01

This review is aimed at discussing the role of ultrastructural studies on human spermatozoa and evaluating transmission electron microscopy as a diagnostic tool that can complete andrology protocols. It is clear that morphological sperm defects may explain decreased fertilizing potential and acquire particular value in the field of male infertility. Electron microscopy is the best method to identify systematic or monomorphic and non-systematic or polymorphic sperm defects. The systematic defects are characterized by a particular anomaly that affects the vast majority of spermatozoa in a semen sample, whereas a heterogeneous combination of head and tail defects found in variable percentages are typically non-systematic or polymorphic sperm defects. A correct diagnosis of these specific sperm alterations is important for choosing the male infertility's therapy and for deciding to turn to assisted reproduction techniques. Transmission electron microscopy (TEM) also represents a valuable method to explore the in vitro effects of different compounds (for example drugs with potential spermicidal activity) on the morphology of human spermatozoa. Finally, TEM used in combination with immunohistochemical techniques, integrates structural and functional aspects that provide a wide horizon in the understanding of sperm physiology and pathology. transmission electron microscopy: TEM; World Health Organization: WHO; light microscopy: LM; motile sperm organelle morphology examination: MSOME; intracytoplasmic morphologically selected sperm injection: IMSI; intracytoplasmic sperm injection: ICSI; dysplasia of fibrous sheath: DFS; primary ciliary dyskinesia: PCD; outer dense fibers: ODF; assisted reproduction technologies: ART; scanning electron microscopy: SEM; polyvinylpirrolidone: PVP; tert-butylhydroperoxide: TBHP.

Electronic and crystal structure changes induced by in-plane oxygen vacancies in multiferroic YMnO 3

DOE PAGES

Cheng, Shaobo; Meng, Qingping; Li, Mengli; ...

2016-02-08

Here, the widely spread oxygen vacancies (V O) in multiferroic materials can strongly affect their physical properties. However, their exact influence has rarely been identified in hexagonal manganites. Here, with the combined use of transmission electron microscopy (TEM) and first-principles calculations, we have systematically studied the electronic and crystal structure modifications induced by V O located at the same Mn atomic plane (in-plane V O). Our TEM experiments reveal that the easily formed in-plane V O not only influence the electronic structure of YMnO 3 but alter the in-plane Wyckoff positions of Mn ions, which may subsequently affect the intraplanemore » and interplane exchange interaction of Mn ions. The ferroelectricity is also impaired due to the introduction of V O. Further calculations confirm these electronic and structural changes and modifications. Our results indicate that the electronic and crystal structure of YMnO 3 can be manipulated by the creation of V O.« less

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

PubMed

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

2018-04-01

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

Tissue and cellular localization of tannins in Tunisian dates (Phoenix dactylifera L.) by light and transmission electron microscopy.

PubMed

Hammouda, Hédi; Alvarado, Camille; Bouchet, Brigitte; Kalthoum-Chérif, Jamila; Trabelsi-Ayadi, Malika; Guyot, Sylvain

2014-07-16

A histological approach including light microscopy and transmission electron microscopy (TEM) was used to provide accurate information on the localization of condensed tannins in the edible tissues and in the stone of date fruits (Phoenix dactylifera L.). Light microscopy was carried out on fresh tissues after staining by 4-dimethylaminocinnamaldehyde (DMACA) for a specific detection of condensed tannins. Thus, whether under light microscopy or transmission electron microscopy (TEM), results showed that tannins are not located in the epidermis but more deeply in the mesocarp in the vacuole of very large cells. Regarding the stones, tannins are found in a specific cell layer located at 50 μm from the sclereid cells of the testa.

The experimental electron mean-free-path in Si under typical (S)TEM conditions.

PubMed

Potapov, P L

2014-12-01

The electron mean-free-path in Si was measured by EELS using the test structure with the certified dimensions as a calibration standard. In a good agreement with the previous CBED measurements, the mean-free-path is 150nm for 200keV and 179nm for 300keV energy of primary electrons at large collection angles. These values are accurately predicted by the model of Iakoubovskii et al. while the model of Malis et al. incorporated in common microscopy software underestimates the mean-free-path by 15% at least. Correspondingly, the thickness of TEM samples reported in many studies of the Si-based materials last decades might be noticeably underestimated. Copyright © 2014 Elsevier B.V. All rights reserved.

Catalyst-layer ionomer imaging of fuel cells

DOE PAGES

Guetaz, Laure; Lopez-Haro, M.; Escribano, S.; ...

2015-09-14

Investigation of membrane/electrode assembly (MEA) microstructure has become an essential step to optimize the MEA components and manufacturing processes or to study the MEA degradation. For these investigations, transmission electron microscopy (TEM) is a tool of choice as it provides direct imaging of the different components. TEM is then widely used for analyzing the catalyst nanoparticles and their carbon support. However, the ionomer inside the electrode is more difficult to be imaged. The difficulties come from the fact that the ionomer forms an ultrathin layer surrounding the carbon particles and in addition, these two components, having similar density, present nomore » difference in contrast. In this paper, we show how the recent progresses in TEM techniques as spherical aberration (Cs) corrected HRTEM, electron tomography and X-EDS elemental mapping provide new possibilities for imaging this ionomer network and consequently to study its degradation.« less

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhang, C.; Golberg, D., E-mail: xuzhi@iphy.ac.cn, E-mail: golberg.dmitri@nims.go.jp; Graduate School of Pure and Applied Sciences, University of Tsukuba, Tennodai 1, Tsukuba, Ibaraki 3058577

2015-08-31

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

A transmission Kikuchi diffraction study of cementite in a quenched and tempered steel

DOE Office of Scientific and Technical Information (OSTI.GOV)

Saleh, Ahmed A., E-mail: asaleh@uow.edu.au; Casillas, Gilberto; Pereloma, Elena V.

2016-04-15

This is the first transmission Kikuchi diffraction (TKD) study to report the indexing of nano-sized cementite as distinct structures and its orientation relationship with the body-centered cubic matrix in a quenched and tempered steel. Crystallographic analysis via TKD and selected area diffraction returned the well-known Bagaryatskii and Isaichev orientation relationships. However, the indexing of nano-sized cementite via TKD was sensitive to the thickness of the electron transparent region such that TEM remains the most precise method to characterise such precipitates. - Highlights: • Nano-sized cementite in a QT steel has been investigated by TKD and TEM. • Cementite has beenmore » indexed as distinct structures via TKD. • Crystallographic analysis returned the Bagaryatskii and Isaichev ORs. • Success of TKD is sensitive to the thickness of the electron transparent region. • TEM remains the most precise technique to characterise nano-sized precipitates.« less

The study of 'microsurfaces' using thermal desorption spectroscopy

NASA Technical Reports Server (NTRS)

Thomas, M. E.; Poppa, H.; Pound, G. M.

1979-01-01

The use of a newly combined ultrahigh vacuum technique for studying continuous and particulate evaporated thin films using thermal desorption spectroscopy (TDS), transmission electron microscopy (TEM), and transmission electron diffraction (TED) is discussed. It is shown that (1) CO thermal desorption energies of epitaxially deposited (111) Ni and (111) Pd surfaces agree perfectly with previously published data on bulk (111) single crystal, (2) contamination and surface structural differences can be detected using TDS as a surface probe and TEM as a complementary technique, and (3) CO desorption signals from deposited metal coverages of one-thousandth of a monolayer should be detectable. These results indicate that the chemisorption properties of supported 'microsurfaces' of metals can now be investigated with very high sensitivity. The combined use of TDS and TEM-TED experimental methods is a very powerful technique for fundamental studies in basic thin film physics and in catalysis.

Cryo-FIB specimen preparation for use in a cartridge-type cryo-TEM.

PubMed

He, Jie; Hsieh, Chyongere; Wu, Yongping; Schmelzer, Thomas; Wang, Pan; Lin, Ying; Marko, Michael; Sui, Haixin

2017-08-01

Cryo-electron tomography (cryo-ET) is a well-established technique for studying 3D structural details of subcellular macromolecular complexes and organelles in their nearly native context in the cell. A primary limitation of the application of cryo-ET is the accessible specimen thickness, which is less than the diameters of almost all eukaryotic cells. It has been shown that focused ion beam (FIB) milling can be used to prepare thin, distortion-free lamellae of frozen biological material for high-resolution cryo-ET. Commercial cryosystems are available for cryo-FIB specimen preparation, however re-engineering and additional fixtures are often essential for reliable results with a particular cryo-FIB and cryo-transmission electron microscope (cryo-TEM). Here, we describe our optimized protocol and modified instrumentation for cryo-FIB milling to produce thin lamellae and subsequent damage-free cryotransfer of the lamellae into our cartridge-type cryo-TEM. Published by Elsevier Inc.

Making the practically impossible "Merely difficult"--Cryogenic FIB lift-out for "Damage free" soft matter imaging.

PubMed

Parmenter, Christopher D J; Fay, Michael W; Hartfield, Cheryl; Eltaher, Hoda M

2016-04-01

The preparation of thinned lamellae from bulk samples for transmission electron microscopy (TEM) analysis has been possible in the focussed ion beam scanning electron microscope (FIB-SEM) for over 20 years via the in situ lift-out method. Lift-out offers a fast and site specific preparation method for TEM analysis, typically in the field of materials science. More recently it has been applied to a low-water content biological sample (Rubino 2012). This work presents the successful lift-out of high-water content lamellae, under cryogenic conditions (cryo-FIB lift-out) and using a nanomanipulator retaining its full range of motion, which are advances on the work previously done by Rubino (2012). Strategies are explored for maintaining cryogenic conditions, grid attachment using cryo-condensation of water and protection of the lamella when transferring to the TEM. © 2016 Wiley Periodicals, Inc.

Microstructural characterization of Ti-6Al-4V metal chips by focused ion beam (FIB) and transmission electron microscopy (TEM)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Schneider, Judy; Dong, Lei; Howe, Jane Y

2011-01-01

The microstructure of the secondary deformation zone (SDZ) near the cutting surface in metal chips of Ti-6Al-4V formed during machining was investigated using focused ion beam (FIB) specimen preparation and transmission electron microscopy (TEM) imaging. Use of the FIB allowed precise extraction of the specimen across this region to reveal its inhomogeneous microstructure resulting from the non-uniform distribution of strain, strain rate, and temperature generated during the cutting process. Initial imaging from conventional TEM foil preparation revealed microstructures ranging from heavily textured to regions of fine grains. Using FIB preparation, the transverse microstructure could be interpreted as fine grains nearmore » the cutting surface which transitioned to coarse grains toward the free surface. At the cutting surface a 10 nm thick recrystallized layer was observed capping a 20 nm thick amorphous layer.« less

STEM-HAADF electron microscopy analysis of the central dark line defect of human tooth enamel crystallites.

PubMed

Gasga, Jose Reyes; Carbajal-de-la-Torre, Georgina; Bres, Etienne; Gil-Chavarria, Ivet M; Rodríguez-Hernández, Ana G; Garcia-Garcia, Ramiro

2008-02-01

When human tooth enamel is observed with the Transmission Electron Microscope (TEM), a structural defect is registered in the central region of their nanometric grains or crystallites. This defect has been named as Central Dark Line (CDL) and its structure and function in the enamel structure have been unknown yet. In this work we present the TEM analysis to these crystallites using the High Angle Annular Dark Field (HAADF) technique. Our results suggest that the CDL region is the calcium richest part of the human tooth enamel crystallites.

The core contribution of transmission electron microscopy to functional nanomaterials engineering

NASA Astrophysics Data System (ADS)

Carenco, Sophie; Moldovan, Simona; Roiban, Lucian; Florea, Ileana; Portehault, David; Vallé, Karine; Belleville, Philippe; Boissière, Cédric; Rozes, Laurence; Mézailles, Nicolas; Drillon, Marc; Sanchez, Clément; Ersen, Ovidiu

2016-01-01

Research on nanomaterials and nanostructured materials is burgeoning because their numerous and versatile applications contribute to solve societal needs in the domain of medicine, energy, environment and STICs. Optimizing their properties requires in-depth analysis of their structural, morphological and chemical features at the nanoscale. In a transmission electron microscope (TEM), combining tomography with electron energy loss spectroscopy and high-magnification imaging in high-angle annular dark-field mode provides access to all features of the same object. Today, TEM experiments in three dimensions are paramount to solve tough structural problems associated with nanoscale matter. This approach allowed a thorough morphological description of silica fibers. Moreover, quantitative analysis of the mesoporous network of binary metal oxide prepared by template-assisted spray-drying was performed, and the homogeneity of amino functionalized metal-organic frameworks was assessed. Besides, the morphology and internal structure of metal phosphide nanoparticles was deciphered, providing a milestone for understanding phase segregation at the nanoscale. By extrapolating to larger classes of materials, from soft matter to hard metals and/or ceramics, this approach allows probing small volumes and uncovering materials characteristics and properties at two or three dimensions. Altogether, this feature article aims at providing (nano)materials scientists with a representative set of examples that illustrates the capabilities of modern TEM and tomography, which can be transposed to their own research.Research on nanomaterials and nanostructured materials is burgeoning because their numerous and versatile applications contribute to solve societal needs in the domain of medicine, energy, environment and STICs. Optimizing their properties requires in-depth analysis of their structural, morphological and chemical features at the nanoscale. In a transmission electron microscope (TEM), combining tomography with electron energy loss spectroscopy and high-magnification imaging in high-angle annular dark-field mode provides access to all features of the same object. Today, TEM experiments in three dimensions are paramount to solve tough structural problems associated with nanoscale matter. This approach allowed a thorough morphological description of silica fibers. Moreover, quantitative analysis of the mesoporous network of binary metal oxide prepared by template-assisted spray-drying was performed, and the homogeneity of amino functionalized metal-organic frameworks was assessed. Besides, the morphology and internal structure of metal phosphide nanoparticles was deciphered, providing a milestone for understanding phase segregation at the nanoscale. By extrapolating to larger classes of materials, from soft matter to hard metals and/or ceramics, this approach allows probing small volumes and uncovering materials characteristics and properties at two or three dimensions. Altogether, this feature article aims at providing (nano)materials scientists with a representative set of examples that illustrates the capabilities of modern TEM and tomography, which can be transposed to their own research. Electronic supplementary information (ESI) available. See DOI: 10.1039/c5nr05460e

The Use of Backscattered Electron Imaging and Transmission Electron Microscopy to Assess Bone Architecture and Mineral Loci: Effect of Intermittent Slow-Release Sodium Fluoride Therapy

NASA Astrophysics Data System (ADS)

Zerwekh, Joseph E.; Bellotto, Dennis; Prostak, Kenneth S.; Hagler, Herbert K.; Pak, Charles Y. C.

1996-04-01

Backscattered electron imaging (BEI) and transmission electron microscopy (TEM) were used to examine the effects of treatment with intermittent slow-release sodium fluoride (SRNaF) and continuous calcium citrate on bone architecture and crystallinity. Examination was performed in nondecalcified biopsies obtained from patients following up to four years of therapy (placebo or SRNaF) and compared to pretreatment biopsies from each patient, as well as to bone from young, normal subjects. BEI images disclosed increased areas of recent bone formation following fluoride administration. There was no evidence of a mineralization defect in any biopsy and both cortical and trabecular architecture remained normal. TEM analysis demonstrated intrafibrillar platelike crystals and extrafibrillar needlelike crystals for both the pre- and post-treatment biopsies as well as for the bone from young normal subjects. There was no evidence of increased crystal size or of an increase in extrafibrillar mineral deposition. These observations suggest that intermittent SRNaF and continuous calcium therapy exerts an anabolic action on the skeleton not accompanied by a mineralization defect or an alteration of bone mineral deposition. The use of BEI and TEM holds promise for the study of the pathophysiology and treatment of metabolic bone diseases.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kawasaki, Tadahiro; PRESTO-JST, 4-1-8 Honcho, Kawaguchi, Saitama 332-0012; Ueda, Kouta

We have developed an improved, windowed type environmental-cell (E-cell) transmission electron microscope (TEM) for in situ observation of gas-solid interactions, such as catalytic reactions at atmospheric pressure. Our E-cell TEM includes a compact E-cell specimen holder with mechanical stability, resulting in smoother introduction of the desired gases compared with previous E-cell TEMs. In addition, the gas control unit was simplified by omitting the pressure control function of the TEM pre-evacuation chamber. This simplification was due to the successful development of remarkably tough thin carbon films as the window material. These films, with a thickness of <10 nm, were found tomore » withstand pressure differences >2 atm. Appropriate arrangement of the specimen position inside the E-cell provided quantitatively analyzable TEM images, with no disturbances caused by the windowed films. As an application, we used this E-cell TEM to observe the dynamic shape change in a catalytic gold nanoparticle supported on TiO{sub 2} during the oxidation of CO gas.« less

Direct observation of a stacking fault in Si(1 - x)Ge(x) semiconductors by spherical aberration-corrected TEM and conventional ADF-STEM.

PubMed

Yamasaki, Jun; Kawai, Tomoyuki; Tanaka, Nobuo

2004-01-01

Spherical aberration (C(S))-corrected transmission electron microscopy (TEM) and annular dark-field scanning TEM (ADF-STEM) are applied to high-resolution observation of stacking faults in Si(1 - x)Ge(x) alloy films prepared on a Si(100) buffer layer by the chemical vapor deposition method. Both of the images clarify the individual nature of stacking faults from their directly interpretable image contrast and also by using image simulation in the case of the C(S)-corrected TEM. Positions of the atomic columns obtained in the ADF-STEM images almost agree with a projection of the theoretical model studied by Chou et al. (Phys. Rev. B 32(1985): 7979). Comparison between the C(S)-corrected TEM and ADF-STEM images shows that their resolution is at a similar level, but directly interpretable image contrast is obtained in ultrathin samples for C(S)-corrected TEM and in slightly thicker samples for ADF-STEM.

Synthesis of Non-uniformly Pr-doped SrTiO3 Ceramics and Their Thermoelectric Properties

PubMed Central

Mehdizadeh Dehkordi, Arash; Bhattacharya, Sriparna; Darroudi, Taghi; Zeng, Xiaoyu; Alshareef, Husam N.; Tritt, Terry M.

2015-01-01

We demonstrate a novel synthesis strategy for the preparation of Pr-doped SrTiO3 ceramics via a combination of solid state reaction and spark plasma sintering techniques. Polycrystalline ceramics possessing a unique morphology can be achieved by optimizing the process parameters, particularly spark plasma sintering heating rate. The phase and morphology of the synthesized ceramics were investigated in detail using X-ray diffraction, scanning electron microcopy and energy-dispersive X-ray spectroscopy. It was observed that the grains of these bulk Pr-doped SrTiO3 ceramics were enhanced with Pr-rich grain boundaries. Electronic and thermal transport properties were also investigated as a function of temperature and doping concentration. Such a microstructure was found to give rise to improved thermoelectric properties. Specifically, it resulted in a significant improvement in carrier mobility and the thermoelectric power factor. Simultaneously, it also led to a marked reduction in the thermal conductivity. As a result, a significant improvement (> 30%) in the thermoelectric figure of merit was achieved for the whole temperature range over all previously reported maximum values for SrTiO3-based ceramics. This synthesis demonstrates the steps for the preparation of bulk polycrystalline ceramics of non-uniformly Pr-doped SrTiO3. PMID:26327483

Comparison of the structure, crystallography and composition of eggshells of the guinea fowl and graylag goose.

PubMed

Pérez-Huerta, Alberto; Dauphin, Yannicke

2016-02-01

The structure and composition of the eggshells of two commercial species (guinea fowl and greylag goose) have been studied. Thin sections and scanning electron microcopy show the similarity of the overall structure, but the relative thickness of the layers differs in these two taxa. Atomic force microscopy shows that the different layers are composed of rounded, heterogeneous granules, the diameter of which is between 50 and 100 nm, with a thin cortex. Infrared data and thermogravimetric analyses show that both eggshells are made of calcite, but differing on the quality and quantity when the organic component is considered. Chemical maps show that chemical element distribution is not uniform within a sample, and differs between the species, but with low magnesium content. Electron back scattered diffraction confirms the eggshells are calcite, but the microtexture strongly differs between the two species. Based on the chemical-structural differences, a species-specific biological control on the biomineralization is found, despite the rapid formation of an eggshell. Overall results indicate that to estimate the quality of eggshells, such as resistance to breakage, is not a straightforward process because of the high complexity of avian eggshell biomineralization. Copyright © 2015 Elsevier GmbH. All rights reserved.

Synthesis of Non-uniformly Pr-doped SrTiO3 Ceramics and Their Thermoelectric Properties.

PubMed

Mehdizadeh Dehkordi, Arash; Bhattacharya, Sriparna; Darroudi, Taghi; Zeng, Xiaoyu; Alshareef, Husam N; Tritt, Terry M

2015-08-15

We demonstrate a novel synthesis strategy for the preparation of Pr-doped SrTiO3 ceramics via a combination of solid state reaction and spark plasma sintering techniques. Polycrystalline ceramics possessing a unique morphology can be achieved by optimizing the process parameters, particularly spark plasma sintering heating rate. The phase and morphology of the synthesized ceramics were investigated in detail using X-ray diffraction, scanning electron microcopy and energy-dispersive X-ray spectroscopy. It was observed that the grains of these bulk Pr-doped SrTiO3 ceramics were enhanced with Pr-rich grain boundaries. Electronic and thermal transport properties were also investigated as a function of temperature and doping concentration. Such a microstructure was found to give rise to improved thermoelectric properties. Specifically, it resulted in a significant improvement in carrier mobility and the thermoelectric power factor. Simultaneously, it also led to a marked reduction in the thermal conductivity. As a result, a significant improvement (> 30%) in the thermoelectric figure of merit was achieved for the whole temperature range over all previously reported maximum values for SrTiO3-based ceramics. This synthesis demonstrates the steps for the preparation of bulk polycrystalline ceramics of non-uniformly Pr-doped SrTiO3.

Structural, Optical and Electrical Properties of ITO Thin Films

NASA Astrophysics Data System (ADS)

Sofi, A. H.; Shah, M. A.; Asokan, K.

2018-02-01

Transparent and conductive thin films of indium tin oxide were fabricated on glass substrates by the thermal evaporation technique. Tin doped indium ingots with low tin content were evaporated in vacuum (1.33 × 10-7 kpa) followed by an oxidation for 15 min in the atmosphere in the temperature range of 600-700°C. The structure and phase purity, surface morphology, optical and electrical properties of thin films were studied by x-ray diffractometry and Raman spectroscopy, scanning electron microcopy and atomic force microscopy, UV-visible spectrometry and Hall measurements in the van der Pauw configuration. The x-ray diffraction study showed the formation of the cubical phase of polycrystalline thin films. The morphological analysis showed the formation of ginger like structures and the energy dispersive x-ray spectrum confirmed the presence of indium (In), tin (Sn) and oxygen (O) elements. Hall measurements confirmed n-type conductivity of films with low electrical resistivity ( ρ) ˜ 10-3 Ω cm and high carrier concentration ( n) ˜ 1020 cm-3. For prevalent scattering mechanisms in the films, experimental data was analyzed by calculating a mean free path ( L) using a highly degenerate electron gas model. Furthermore, to investigate the performance of the deposited films as a transparent conductive material, the optical figure of merit was obtained for all the samples.

[Architectural ultrastructure of the human urinary transitional epithelium].

PubMed

Takayama, H; Konishi, T

1984-07-01

Human urinary bladder mucosa, confirmed to be normal by cystoscopic, histologic and bacteriologic examination, were obtained from four patients at prostatectomy and from two patients at an anti-VUR procedure. The luminal surface and the three dimensional architecture of the bladder mucosa were observed by scanning electron microscopy (SEM) after cryofracture of specimen and by transmission electron microscopy (TEM). The epithelium consists of superficial, intermediate and basal cells, and SEM and TEM showed that it was stratified. Intermediate cells reached the basal lamina by slender cytoplasmic processes but superficial cells were not directly in contact with the basal lamina. No pleomorphic or long microvilli were observed but short microvilli or granular protrusions were sparsely seen on the luminal surface of superficial cells. SEM of cryofractured surfaces revealed that cells from each cell layer were in contact with cellular junctions such as ridges, plicated projections and septum-like walls. Their junctions were more complicated with increasing depth of the cell layer. No pleomorphic or long microvilli were observed on any cell surface of the intermediate or basal cell layer. Under TEM, however, these junctional structures of ridges, plicated projections and septal walls appeared to be microvilli under TEM. Microvilli-like structures on TEM, therefore, have to be carefully distinguished from real microvilli. Careful observation is required when the presence of cells covered with microvilli is described as a sign of malignancy.

Multi-class segmentation of neuronal electron microscopy images using deep learning

NASA Astrophysics Data System (ADS)

Khobragade, Nivedita; Agarwal, Chirag

2018-03-01

Study of connectivity of neural circuits is an essential step towards a better understanding of functioning of the nervous system. With the recent improvement in imaging techniques, high-resolution and high-volume images are being generated requiring automated segmentation techniques. We present a pixel-wise classification method based on Bayesian SegNet architecture. We carried out multi-class segmentation on serial section Transmission Electron Microscopy (ssTEM) images of Drosophila third instar larva ventral nerve cord, labeling the four classes of neuron membranes, neuron intracellular space, mitochondria and glia / extracellular space. Bayesian SegNet was trained using 256 ssTEM images of 256 x 256 pixels and tested on 64 different ssTEM images of the same size, from the same serial stack. Due to high class imbalance, we used a class-balanced version of Bayesian SegNet by re-weighting each class based on their relative frequency. We achieved an overall accuracy of 93% and a mean class accuracy of 88% for pixel-wise segmentation using this encoder-decoder approach. On evaluating the segmentation results using similarity metrics like SSIM and Dice Coefficient, we obtained scores of 0.994 and 0.886 respectively. Additionally, we used the network trained using the 256 ssTEM images of Drosophila third instar larva for multi-class labeling of ISBI 2012 challenge ssTEM dataset.

Transmission Electron Microscopy (TEM) Sample Preparation of Si(1-x)Gex in c-Plane Sapphire Substrate

NASA Technical Reports Server (NTRS)

Kim, Hyun Jung; Choi, Sang H.; Bae, Hyung-Bin; Lee, Tae Woo

2012-01-01

The National Aeronautics and Space Administration-invented X-ray diffraction (XRD) methods, including the total defect density measurement method and the spatial wafer mapping method, have confirmed super hetero epitaxy growth for rhombohedral single crystalline silicon germanium (Si1-xGex) on a c-plane sapphire substrate. However, the XRD method cannot observe the surface morphology or roughness because of the method s limited resolution. Therefore the authors used transmission electron microscopy (TEM) with samples prepared in two ways, the focused ion beam (FIB) method and the tripod method to study the structure between Si1-xGex and sapphire substrate and Si1?xGex itself. The sample preparation for TEM should be as fast as possible so that the sample should contain few or no artifacts induced by the preparation. The standard sample preparation method of mechanical polishing often requires a relatively long ion milling time (several hours), which increases the probability of inducing defects into the sample. The TEM sampling of the Si1-xGex on sapphire is also difficult because of the sapphire s high hardness and mechanical instability. The FIB method and the tripod method eliminate both problems when performing a cross-section TEM sampling of Si1-xGex on c-plane sapphire, which shows the surface morphology, the interface between film and substrate, and the crystal structure of the film. This paper explains the FIB sampling method and the tripod sampling method, and why sampling Si1-xGex, on a sapphire substrate with TEM, is necessary.

Nanoscale chromatin structure characterization for optical applications: a transmission electron microscopy study (Conference Presentation)

NASA Astrophysics Data System (ADS)

Li, Yue; Cherkezyan, Lusik; Zhang, Di; Almassalha, Luay; Roth, Eric; Chandler, John; Bleher, Reiner; Subramanian, Hariharan; Dravid, Vinayak P.; Backman, Vadim

2017-02-01

Structural and biological origins of light scattering in cells and tissue are still poorly understood. We demonstrate how this problem might be addressed through the use of transmission electron microscopy (TEM). For biological samples, TEM image intensity is proportional to mass-density, and thus proportional to refractive index (RI). By calculating the autocorrelation function (ACF) of TEM image intensity of a thin-section of cells, we essentially maintain the nanoscale ACF of the 3D cellular RI distribution, given that the RI distribution is statistically isotropic. Using this nanoscale 3D RI ACF, we can simulate light scattering through biological samples, and thus guiding many optical techniques to quantify specific structures. In this work, we chose to use Partial Wave Spectroscopy (PWS) microscopy as a one of the nanoscale-sensitive optical techniques. Hela cells were prepared using standard protocol to preserve nanoscale ultrastructure, and a 50-nm slice was sectioned for TEM imaging at 6 nm resolution. The ACF was calculated for chromatin, and the PWS mean sigma was calculated by summing over the power spectral density in the visible light frequency of a random medium generated to match the ACF. A 1-µm slice adjacent to the 50-nm slice was sectioned for PWS measurement to guarantee identical chromatin structure. For 33 cells, we compared the calculated PWS mean sigma from TEM and the value measured directly, and obtained a strong correlation of 0.69. This example indicates the great potential of using TEM measured RI distribution to better understand the quantification of cellular nanostructure by optical methods.

Thinking about Non-Linear Smoothers.

DTIC Science & Technology

1986-05-01

ALI6-87 F/G 12/1 UL EhhhhhhhhhhhhEl EhhhhohhhhhhhE EhhhhhmhhhhhhE 1111 101112.0 1111.25 111111. 111 . MICROCOPY RESOLUTION TEST CH -ART NATIONAL BUREAU OF...605 1053 (3467) 5794 7532 196 -3 -5 -1 195 500 608 1080 3384 5638 7653 183 45 58 14 (183) 515 614 1092 3332 5483 7845 228 27 -18 -4 224 537 617 192

Synthesis of Textures Using Simultaneous Autoregressive Models.

DTIC Science & Technology

1981-07-01

CHELLAPPA AFOSR-77-3271 UNCLASSIFIED TR- 1082 AFOSR-TR-81-0795 NL 110~2.8 .113:’I0 111.02. 1111I25 II.4~* 1.6 MICROCOPY R[ SOLUTION ILS1 CHARI ,.TR- 81...NUMBER TR- 1082 . 7. AUTHOR(*) S. CONTRACT OR GRANT NUMBER(&) R. Chella-)pa AFOSR-77-3271 9. PERFORMING ORGANIZATION NAME AND ADDRESS 10. PROGRAM ELEMENT

New Cadets and other College Freshmen: Class of 1984,

DTIC Science & Technology

1981-03-01

V HOUSTON UNCLASSIFID 81-009 5Lm H40 1 .0 IIIJILI15 MICROCOPY RISOtUTION IfLST CHART ~z~LV~LUNITED K STATES 00 1AMILITARY ACADEMY I -~ WEST POINT...INTRODUCTION, METHOD and RESULTS ............................................ 1 -3 SECTION I. BIOGRAPHICAL AND SOCIOECONOMIC CHARACTERISTICS 1 . Age...6 8. Year Graduated from High School ................................ 6 , 1 9. Distance from Home to College

Minigrant Program. A Differential Geometric Approach to Electromagnetic Lens Design.

DTIC Science & Technology

1984-06-01

34,___" ,. --. 5 %’’ %, ;_-- - .-.- -. ...’ .¢ MICROCOPY RESOLUTION TEST CHART NATIONAL BUREAU OF STANDARDS-1963-A _"O i ’,... • . , w .T..rm,..p,. .. , .e W...ORGANIZATION REPORT NU,/dEHj) AD"A144 239 AFOSRTR- 3 4 - 0 5 9 6 aNIAME OF PERFORMING ORGANIZATION 6b OFFICE SYMBOL 74. NAME OF MONITORING ORGANIZATION

Compressive Classification for TEM-EELS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hao, Weituo; Stevens, Andrew; Yang, Hao

Electron energy loss spectroscopy (EELS) is typically conducted in STEM mode with a spectrometer, or in TEM mode with energy selction. These methods produce a 3D data set (x, y, energy). Some compressive sensing [1,2] and inpainting [3,4,5] approaches have been proposed for recovering a full set of spectra from compressed measurements. In many cases the final form of the spectral data is an elemental map (an image with channels corresponding to elements). This means that most of the collected data is unused or summarized. We propose a method to directly recover the elemental map with reduced dose and acquisitionmore » time. We have designed a new computational TEM sensor for compressive classification [6,7] of energy loss spectra called TEM-EELS.« less

Transmission Electron Microscopy of Cometary Residues from Micron-Sized Craters in the Stardust Al-Foils

NASA Technical Reports Server (NTRS)

Leroux, Hugues; Stroud, Rhonda M.; Dai, Zu Rong; Graham, Giles A.; Troadec, David; Bradley, John P.; Teslich, Nick; Borg, Janet; Kearsley, Anton T.; Horz, Friedrich

2008-01-01

We report Transmission Electron Microscopy (TEM) investigations of micro-craters that originated from hypervelocity impacts of comet 81P/Wild 2 dust particles on the aluminium foil of the Stardust collector. The craters were selected by Scanning Electron Microscopy (SEM) and then prepared by Focused Ion Beam (FIB) milling techniques in order to provide electron transparent cross-sections for TEM studies. The crater residues contain both amorphous and crystalline materials in varying proportions and compositions. The amorphous component is interpreted as resulting from shock melting during the impact and the crystalline phases as relict minerals. The latter show evidence for shock metamorphism. Based on the residue morphology and the compositional variation, the impacting particles are inferred to have been dominated by mixtures of submicron olivine, pyroxene and Fe-sulfide grains, in agreement with prior results of relatively coarse-grained mineral assemblages in the aerogel collector.

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

PubMed

Malladi, Sairam; Shen, Chenggang; Xu, Qiang; de Kruijff, Tom; Yücelen, Emrah; Tichelaar, Frans; Zandbergen, Henny

2013-11-28

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 platinum tubing permits the usage of aggressive chemicals like hydrochloric acid (HCl).

Characterization of CuCl quantum dots grown in NaCl single crystals via optical measurements, X-ray diffraction, and transmission electron microscopy

NASA Astrophysics Data System (ADS)

Miyajima, Kensuke; Akatsu, Tatsuro; Itoh, Ken

2018-05-01

We evaluated the crystal size, shape, and alignment of the lattice planes of CuCl quantum dots (QDs) embedded in NaCl single crystals by optical measurements, X-ray diffraction (XRD) patterns, and transmission electron microscopy (TEM). We obtained, for the first time, an XRD pattern and TEM images for CuCl QDs in NaCl crystals. The XRD pattern showed that the lattice planes of the CuCl QDs were parallel to those of the NaCl crystals. In addition, the size of the QDs was estimated from the diffraction width. It was apparent from the TEM images that almost all CuCl QDs were polygonal, although some cubic QDs were present. The mean size and size distribution of the QDs were also obtained. The dot size obtained from optical measurements, XRD, and TEM image were almost consistent. Our new findings can help to reveal the growth mechanism of semiconductor QDs embedded in a crystallite matrix. In addition, this work will play an important role in progressing the study of optical phenomena originating from assembled semiconductor QDs.

A 57GHz overmoded coaxial relativistic backward wave oscillator with high conversion efficiency and pure TM01 mode output

NASA Astrophysics Data System (ADS)

Chen, Siyao; Zhang, Jun; Bai, Zhen

2017-10-01

A 57GHz overmoded relativistic backward wave oscillator (RBWO) operating on the quasi-TEM mode with pure TM01 mode output is presented in this paper, by using outer trapezoidal slow wave structure (SWS) with large distance between inner and outer conductors. The large overmoded ratio can be obtained in coaxial devices to improve power handling capacity, while the large distance between inner and outer conductors can guarantee the electron beam transmit effectively. The 8π/9 mode of quasi-TEM synchronously interacts with the electron beam, while the TM01 mode diffracted by the quasi-TEM mode outputs. The existence of TM01 6π/9 mode in SWS can extract energy from the quasi-TEM mode (which has a high value of Qe) thus increasing the power handling capacity. Particle-in-cell simulation shows that generation with high power 560 MW and efficiency 43.5% is obtained under the diode voltage 520 kV and current 2.47 kA. And the microwave has the pure frequency spectrum of 56.8 GHz radiates in the pure TM01 mode (about 98%).

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Edmondson, Philip D.

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-qualitymore » in situ experiments to be conducted on irradiated materials.« less

Correlative scanning-transmission electron microscopy reveals that a chimeric flavivirus is released as individual particles in secretory vesicles.

PubMed

Burlaud-Gaillard, Julien; Sellin, Caroline; Georgeault, Sonia; Uzbekov, Rustem; Lebos, Claude; Guillaume, Jean-Marc; Roingeard, Philippe

2014-01-01

The intracellular morphogenesis of flaviviruses has been well described, but flavivirus release from the host cell remains poorly documented. We took advantage of the optimized production of an attenuated chimeric yellow fever/dengue virus for vaccine purposes to study this phenomenon by microscopic approaches. Scanning electron microscopy (SEM) showed the release of numerous viral particles at the cell surface through a short-lived process. For transmission electron microscopy (TEM) studies of the intracellular ultrastructure of the small number of cells releasing viral particles at a given time, we developed a new correlative microscopy method: CSEMTEM (for correlative scanning electron microscopy - transmission electron microscopy). CSEMTEM analysis suggested that chimeric flavivirus particles were released as individual particles, in small exocytosis vesicles, via a regulated secretory pathway. Our morphological findings provide new insight into interactions between flaviviruses and cells and demonstrate that CSEMTEM is a useful new method, complementary to SEM observations of biological events by intracellular TEM investigations.

The effect of defects produced by electron irradiation on the electrical properties of graphene and MoS2

NASA Astrophysics Data System (ADS)

Rodriguez-Manzo, Julio Alejandro; Balan, Adrian; Nayor, Carl; Parkin, Will; Puster, Matthew; Johnson, A. T. Charlie; Drndic, Marija

2015-03-01

We present a study of the effects of the defects produced by electron irradiation on the electrical and crystalline properties of graphene and MoS2 monolayers. We realized back or side gated electrical devices from monolayer MoS2 or graphene crystals (triangles respectively hexagons) suspended on a 50nm SiNx m. The devices are exposed to electron irradiation inside a 200kV transmission electron microscope (TEM) and we perform in situ conductance measurements. The number of defects and the quality of the crystalline lattice obtained by diffraction are correlated with the observed decrease in mobility and conductivity of the devices. We observe a different behavior between MoS2 and graphene, and try to associate this with different models for conduction with defects. Finally, we use the TEM electron beam to tailor the macroscopic layers into ribbons to be used as the sensing element in MoS2 nanoribbon - nanopore devices for DNA detection and sequencing.

Correlative Scanning-Transmission Electron Microscopy Reveals that a Chimeric Flavivirus Is Released as Individual Particles in Secretory Vesicles

PubMed Central

Burlaud-Gaillard, Julien; Sellin, Caroline; Georgeault, Sonia; Uzbekov, Rustem; Lebos, Claude; Guillaume, Jean-Marc; Roingeard, Philippe

2014-01-01

The intracellular morphogenesis of flaviviruses has been well described, but flavivirus release from the host cell remains poorly documented. We took advantage of the optimized production of an attenuated chimeric yellow fever/dengue virus for vaccine purposes to study this phenomenon by microscopic approaches. Scanning electron microscopy (SEM) showed the release of numerous viral particles at the cell surface through a short-lived process. For transmission electron microscopy (TEM) studies of the intracellular ultrastructure of the small number of cells releasing viral particles at a given time, we developed a new correlative microscopy method: CSEMTEM (for correlative scanning electron microscopy - transmission electron microscopy). CSEMTEM analysis suggested that chimeric flavivirus particles were released as individual particles, in small exocytosis vesicles, via a regulated secretory pathway. Our morphological findings provide new insight into interactions between flaviviruses and cells and demonstrate that CSEMTEM is a useful new method, complementary to SEM observations of biological events by intracellular TEM investigations. PMID:24681578

Structural analysis of the PSD-95 cluster by electron tomography and CEMOVIS: a proposal for the application of the genetically encoded metallothionein tag.

PubMed

Hirabayashi, Ai; Fukunaga, Yuko; Miyazawa, Atsuo

2014-06-01

Postsynaptic density-95 (PSD-95) accumulates at excitatory postsynapses and plays important roles in the clustering and anchoring of numerous proteins at the PSD. However, a detailed ultrastructural analysis of clusters exclusively consisting of PSD-95 has never been performed. Here, we employed a genetically encoded tag, three tandem repeats of metallothionein (3MT), to study the structure of PSD-95 clusters in cells by electron tomography and cryo-electron microscopy of vitreous sections. We also performed conventional transmission electron microscopy (TEM). Cultured hippocampal neurons expressing a fusion protein of PSD-95 coupled to 3MT (PDS-95-3MT) were incubated with CdCl2 to result in the formation of Cd-bound PSD-95-3MT. Two types of electron-dense deposits composed of Cd-bound PSD-95-3MT were observed in these cells by TEM, as reported previously. Electron tomography revealed the presence of membrane-shaped structures representing PSD-95 clusters at the PSD and an ellipsoidal structure located in the non-synaptic cytoplasm. By TEM, the PSD-95 clusters appeared to be composed of a number of dense cores. In frozen hydrated sections, these dense cores were also found beneath the postsynaptic membrane. Taken together, our findings suggest that dense cores of PSD-95 aggregate to form the larger clusters present in the PSD and the non-synaptic cytoplasm. © 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.

Synthesis of Lead Sulfide Nanoparticles by Chemical Precipitation Method

NASA Astrophysics Data System (ADS)

Chongad, L. S.; Sharma, A.; Banerjee, M.; Jain, A.

2016-10-01

Lead sulfide (PbS) nanoparticles were prepared by chemical precipitation method (CPM) with the assistance of H2S gas. The microstructure and morphology of the synthesized nanoparticles have been investigated using X-ray diffraction (XRD) and transmission electron microscopy (TEM). The XRD patterns of the PbS nanoparticles reveal formation of cubic phase. To investigate the quality of prepared nanoparticles, the particles size, lattice constant, strain, dislocation density etc. have been determined using XRD. TEM images reveal formation of cubic nanoparticles and the particle size determined from TEM images agree well with those from XRD.

Serial Section Scanning Electron Microscopy (S3EM) on Silicon Wafers for Ultra-Structural Volume Imaging of Cells and Tissues

PubMed Central

Horstmann, Heinz; Körber, Christoph; Sätzler, Kurt; Aydin, Daniel; Kuner, Thomas

2012-01-01

High resolution, three-dimensional (3D) representations of cellular ultrastructure are essential for structure function studies in all areas of cell biology. While limited subcellular volumes have been routinely examined using serial section transmission electron microscopy (ssTEM), complete ultrastructural reconstructions of large volumes, entire cells or even tissue are difficult to achieve using ssTEM. Here, we introduce a novel approach combining serial sectioning of tissue with scanning electron microscopy (SEM) using a conductive silicon wafer as a support. Ribbons containing hundreds of 35 nm thick sections can be generated and imaged on the wafer at a lateral pixel resolution of 3.7 nm by recording the backscattered electrons with the in-lens detector of the SEM. The resulting electron micrographs are qualitatively comparable to those obtained by conventional TEM. S3EM images of the same region of interest in consecutive sections can be used for 3D reconstructions of large structures. We demonstrate the potential of this approach by reconstructing a 31.7 µm3 volume of a calyx of Held presynaptic terminal. The approach introduced here, Serial Section SEM (S3EM), for the first time provides the possibility to obtain 3D ultrastructure of large volumes with high resolution and to selectively and repetitively home in on structures of interest. S3EM accelerates process duration, is amenable to full automation and can be implemented with standard instrumentation. PMID:22523574

Serial section scanning electron microscopy (S3EM) on silicon wafers for ultra-structural volume imaging of cells and tissues.

PubMed

Horstmann, Heinz; Körber, Christoph; Sätzler, Kurt; Aydin, Daniel; Kuner, Thomas

2012-01-01

High resolution, three-dimensional (3D) representations of cellular ultrastructure are essential for structure function studies in all areas of cell biology. While limited subcellular volumes have been routinely examined using serial section transmission electron microscopy (ssTEM), complete ultrastructural reconstructions of large volumes, entire cells or even tissue are difficult to achieve using ssTEM. Here, we introduce a novel approach combining serial sectioning of tissue with scanning electron microscopy (SEM) using a conductive silicon wafer as a support. Ribbons containing hundreds of 35 nm thick sections can be generated and imaged on the wafer at a lateral pixel resolution of 3.7 nm by recording the backscattered electrons with the in-lens detector of the SEM. The resulting electron micrographs are qualitatively comparable to those obtained by conventional TEM. S(3)EM images of the same region of interest in consecutive sections can be used for 3D reconstructions of large structures. We demonstrate the potential of this approach by reconstructing a 31.7 µm(3) volume of a calyx of Held presynaptic terminal. The approach introduced here, Serial Section SEM (S(3)EM), for the first time provides the possibility to obtain 3D ultrastructure of large volumes with high resolution and to selectively and repetitively home in on structures of interest. S(3)EM accelerates process duration, is amenable to full automation and can be implemented with standard instrumentation.

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zieliński, W., E-mail: wiziel@inmat.pw.edu.pl; Płociński, T.; Kurzydłowski, K.J.

2015-06-15

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

Size determination of Acipenser ruthenus spermatozoa in different types of electron microscopy.

PubMed

Psenicka, Martin; Tesarová, Martina; Tesitel, Jakub; Nebesárová, Jana

2010-07-01

In this study three types of scanning electron microscopes were used for the size determination of spermatozoa of sterlet Acipenser ruthenus - high vacuum scanning electron microscope (SEM, JEOL 6300), environmental scanning electron microscope (ESEM, Quanta 200 FEG), field emission scanning electron microscope (FESEM, JEOL 7401F) with cryoattachment Alto 2500 (Gatan) and transmission electron microscope (TEM, JEOL 1010). The use of particular microscopes was tied with different specimen preparation techniques. The aim of this study was to evaluate to what degree the type of used electron microscope can influence the size of different parts of spermatozoa. For high vacuum SEM the specimen was prepared using two slightly different procedures. After chemical fixation with 2.5% glutaraldehyde in 0.1M phosphate buffer and post-fixation by 1% osmium tetroxide, the specimen was dehydrated by acetone series and dried either by critical point method or by means of t-butylalcohol. For ESEM fresh, unfixed material was used, which was dropped on microscopic copper grids. In FESEM working in cryo-mode the specimen was observed in a frozen state. Ultrathin sections from chemically fixed and Epon embedded specimens were prepared for TEM observation. Distinct parts of sterlet spermatozoa were measured in each microscope and the data obtained was statistically processed. Results confirmed that the classical chemical procedure of specimen preparation for SEM including critical point drying method led to a significant contraction of all measured values, which could deviate up to 30% in comparison with values measured on the fresh chemically untreated specimen in ESEM. Surprisingly sperm dimensions determinated on ultrathin sections by TEM are comparable with values obtained in ESEM or FESEM. Copyright 2010 Elsevier Ltd. All rights reserved.

Probing Structural and Electronic Dynamics with Ultrafast Electron Microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Plemmons, DA; Suri, PK; Flannigan, DJ

In this Perspective, we provide an overview,of the field of ultrafast electron microscopy (UEM). We begin by briefly discussing the emergence of methods for probing ultrafast structural dynamics and the information that can be obtained. Distinctions are drawn between the two main types a probes for femtosecond (fs) dynamics fast electrons and X-ray photons and emphasis is placed on hour the nature of charged particles is exploited in ultrafast electron-based' experiments:. Following this, we describe the versatility enabled by the ease with which electron trajectories and velocities can be manipulated with transmission electron microscopy (TEM): hardware configurations, and we emphasizemore » how this is translated to the ability to measure scattering intensities in real, reciprocal, and energy space from presurveyed and selected rianoscale volumes. Owing to decades of ongoing research and development into TEM instrumentation combined with advances in specimen holder technology, comprehensive experiments can be conducted on a wide range of materials in various phases via in situ methods. Next, we describe the basic operating concepts, of UEM, and we emphasize that its development has led to extension of several of the formidable capabilities of TEM into the fs domain, dins increasing the accessible temporal parameter spade by several orders of magnitude. We then divide UEM studies into those conducted in real (imaging), reciprocal (diffraction), and energy (spectroscopy) spate. We begin each of these sections by providing a brief description of the basic operating principles and the types of information that can be gathered followed by descriptions of how these approaches are applied in UM, the type of specimen parameter space that can be probed, and an example of the types of dynamics that can be resolved. We conclude with an Outlook section, wherein we share our perspective on some future directions of the field pertaining to continued instrument development and application of the technique to solving seemingly intractable materials problems in addition to discovery-based research. Our goal with this Perspective is to bring the capabilities of TIEM to the-attention of materials scientists, chemists, physicists, and engineers in hopes that new,avenues of research emerge and to make clear the large parameter space that is opened by extending TEM, and the ability to readily manipulate electron trajectories and energies, into the ultrafast domain.« less

Influences of surfactants on the preparation of copper nanoparticles by electron beam irradiation

NASA Astrophysics Data System (ADS)

Zhou, Ruimin; Wu, Xinfeng; Hao, Xufeng; Zhou, Fei; Li, Hongbin; Rao, Weihong

2008-02-01

Electron beam radiation was applied to prepare nano-size copper in water system using polyvinyl alcohol, sodium dodecyl benzene sulfonate, gluten and polyethylene glycol as the surfactants, respectively. The irradiated products were characterized by XRD, TEM and LSPSDA. The XRD and TEM showed that relative pure copper products with an average size of 20 nm, 40 nm and 20 nm can be obtained by using gluten, PEG and SDBS as surfactant, respectively. An admixture of copper and cuprous oxide was obtained in PVA system. The LSPSDA showed that the size of the Cu nanoparticles decreased with increasing the glutin concentration.

Post-ion beam induced degradation of copper layers in transmission electron microscopy specimens

NASA Astrophysics Data System (ADS)

Seidel, F.; Richard, O.; Bender, H.; Vandervorst, W.

2015-11-01

Copper containing transmission electron microscopy (TEM) specimens frequently show corrosion after focused ion beam (FIB) preparation. This paper reveals that the corrosion product is a Cu-S phase growing over the specimen surface. The layer is identified by energy-dispersive x-ray spectroscopy, and lattice spacing indexing of power spectra patterns. The corrosion process is further studied by TEM on cone-shaped specimens, which are intentionally stored after FIB preparation with S flakes for short time. Furthermore, a protective method against corrosion is developed by varying the time in the FIB vacuum and the duration of a subsequent plasma cleaning.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Janeoo, Shashi; Sharma, Mamta, E-mail: mamta.phy85@gmail.com; Goswamy, J.

Polyaniline-indium oxide (In{sub 2}O{sub 3}/PANI) nanocomposite have been prepared by in-situ polymerization of aniline and as-synthesized In{sub 2}O{sub 3} nanoparticles. X-ray diffraction (XRD), Transmission electron microscopy (TEM), Fourier transformation infrared (FTIR) and UV/Vis spectroscopy techniques are used to investigate the structural and optical properties of In{sub 2}O{sub 3}/PANI nanocomposite. TEM analysis shows In{sub 2}O{sub 3} nanoparticles are embedded in PANI nanofibers. FTIR spectra show the good interactions between PANI nanofibers and In{sub 2}O{sub 3} nanoparticles. The band gap and electronic transitions in In{sub 2}O{sub 3}/PANI nanocomposite is determined by using UV/Vis spectra.

Synthesis and characterization of nanocrystalline graphite from coconut shell with heating process

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wachid, Frischa M., E-mail: frischamw@yahoo.com, E-mail: adhiyudhaperkasa@yahoo.com, E-mail: afandisar@yahoo.com, E-mail: nurulrosyidah92@gmail.com, E-mail: darminto@physics.its.ac.id; Perkasa, Adhi Y., E-mail: frischamw@yahoo.com, E-mail: adhiyudhaperkasa@yahoo.com, E-mail: afandisar@yahoo.com, E-mail: nurulrosyidah92@gmail.com, E-mail: darminto@physics.its.ac.id; Prasetya, Fandi A., E-mail: frischamw@yahoo.com, E-mail: adhiyudhaperkasa@yahoo.com, E-mail: afandisar@yahoo.com, E-mail: nurulrosyidah92@gmail.com, E-mail: darminto@physics.its.ac.id

Graphite were synthesized and characterized by heating process of coconut shell with varying temperature (400, 800 and 1000°C) and holding time (3 and 5 hours). After heating process, the samples were characterized by X-ray diffraction (XRD) and analyzed by X'pert HighScore Plus Software, Scanning Electron Microcope-Energy Dispersive X-Ray (SEM-EDX) and Transmission Electron Microscope-Energy Dispersive X-Ray (TEM-EDX). Graphite and londsdaelite phase were analyzed by XRD. According to EDX analysis, the sample was heated in 1000°C got the highest content of carbon. The amorphous carbon and nanocrystalline graphite were observed by SEM-EDX and TEM-EDX.

Clean Transfer of Large Graphene Single Crystals for High-Intactness Suspended Membranes and Liquid Cells.

PubMed

Zhang, Jincan; Lin, Li; Sun, Luzhao; Huang, Yucheng; Koh, Ai Leen; Dang, Wenhui; Yin, Jianbo; Wang, Mingzhan; Tan, Congwei; Li, Tianran; Tan, Zhenjun; Liu, Zhongfan; Peng, Hailin

2017-07-01

The atomically thin 2D nature of suspended graphene membranes holds promising in numerous technological applications. In particular, the outstanding transparency to electron beam endows graphene membranes great potential as a candidate for specimen support of transmission electron microscopy (TEM). However, major hurdles remain to be addressed to acquire an ultraclean, high-intactness, and defect-free suspended graphene membrane. Here, a polymer-free clean transfer of sub-centimeter-sized graphene single crystals onto TEM grids to fabricate large-area and high-quality suspended graphene membranes has been achieved. Through the control of interfacial force during the transfer, the intactness of large-area graphene membranes can be as high as 95%, prominently larger than reported values in previous works. Graphene liquid cells are readily prepared by π-π stacking two clean single-crystal graphene TEM grids, in which atomic-scale resolution imaging and temporal evolution of colloid Au nanoparticles are recorded. This facile and scalable production of clean and high-quality suspended graphene membrane is promising toward their wide applications for electron and optical microscopy. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Micro-structural characterization of precipitation-synthesized fluorapatite nano-material by transmission electron microscopy using different sample preparation techniques.

PubMed

Chinthaka Silva, G W; Ma, Longzhou; Hemmers, Oliver; Lindle, Dennis

2008-01-01

Fluorapatite is a naturally occurring mineral of the apatite group and it is well known for its high physical and chemical stability. There is a recent interest in this ceramic to be used as a radioactive waste form material due to its intriguing chemical and physical properties. In this study, the nano-sized fluorapatite particles were synthesized using a precipitation method and the material was characterized using X-ray diffraction (XRD) and transmission electron microscopy (TEM). Two well-known methods, called solution-drop and the microtome cutting, were used to prepare the sample for TEM analysis. It was found that the microtome cutting technique is advantageous for examining the particle shape and cross-sectional morphology as well as for obtaining ultra-thin samples. However, this method introduces artifacts and strong background contrast for high-resolution transmission electron microscopy (HRTEM) observation. On the other hand, phase image simulations showed that the solution-drop method is reliable and stable for HRTEM analysis. Therefore, in order to comprehensively analyze the microstructure and morphology of the nano-material, it is necessary to combine both solution-drop and microtome cutting techniques for TEM sample preparation.

EBSD and TEM characterization of high burn-up mixed oxide fuel

NASA Astrophysics Data System (ADS)

Teague, Melissa; Gorman, Brian; Miller, Brandon; King, Jeffrey

2014-01-01

Understanding and studying the irradiation behavior of high burn-up oxide fuel is critical to licensing of future fast breeder reactors. Advancements in experimental techniques and equipment are allowing for new insights into previously irradiated samples. In this work dual column focused ion beam (FIB)/scanning electron microscope (SEM) was utilized to prepared transmission electron microscope samples from mixed oxide fuel with a burn-up of 6.7% FIMA. Utilizing the FIB/SEM for preparation resulted in samples with a dose rate of <0.5 mRem/h compared to ∼1.1 R/h for a traditionally prepared TEM sample. The TEM analysis showed that the sample taken from the cooler rim region of the fuel pellet had ∼2.5× higher dislocation density than that of the sample taken from the mid-radius due to the lower irradiation temperature of the rim. The dual column FIB/SEM was additionally used to prepared and serially slice ∼25 μm cubes. High quality electron back scatter diffraction (EBSD) were collected from the face at each step, showing, for the first time, the ability to obtain EBSD data from high activity irradiated fuel.

Microstructural characterization of Ti-6Al-4V alloy subjected to the duplex SMAT/plasma nitriding.

PubMed

Pi, Y; Faure, J; Agoda-Tandjawa, G; Andreazza, C; Potiron, S; Levesque, A; Demangel, C; Retraint, D; Benhayoune, H

2013-09-01

In this study, microstructural characterization of Ti-6Al-4V alloy, subjected to the duplex surface mechanical attrition treatment (SMAT)/nitriding treatment, leading to improve its mechanical properties, was carried out through novel and original samples preparation methods. Instead of acid etching which is limited for morphological characterization by scanning electron microscopy (SEM), an original ion polishing method was developed. Moreover, for structural characterization by transmission electron microscopy (TEM), an ion milling method based with the use of two ions guns was also carried out for cross-section preparation. To demonstrate the efficiency of the two developed methods, morphological investigations were done by traditional SEM and field emission gun SEM. This was followed by structural investigations through selected area electron diffraction (SAED) coupled with TEM and X-ray diffraction techniques. The results demonstrated that ionic polishing allowed to reveal a variation of the microstructure according to the surface treatment that could not be observed by acid etching preparation. TEM associated to SAED and X-ray diffraction provided information regarding the nanostructure compositional changes induced by the duplex SMAT/nitriding process. Copyright © 2013 Wiley Periodicals, Inc.

Radiation sensitivity of quartz crystal oscillators experiment for the Long Duration Exposure Facility (LDEF)

NASA Technical Reports Server (NTRS)

Ahearn, J. S.; Venables, J. D.

1992-01-01

Factors determining the radiation sensitivity of quartz crystal oscillators were studied on NASA's LDEF. Quartz materials were examined in the transmission electron microscope (TEM) and classified as to their sensitivity to radiation damage by establishing the rate of damage caused by the electron beam in the microscope. Two types of materials, i.e., swept premium Q quartz and natural quartz were chosen because clear differences were observed in their response to the electron beam in the TEM studies. Quartz resonators were then fabricated from them, tested for frequency stability over a greater than 6 mo. period and flown on the LDEF satellite. After retrieval (more than 7 yrs in space) the stability of the resonators was again determined. All of the space exposed resonators fabricated with swept premium Q material exhibited a frequency shift above that of the control resonators: none of the resonators fabricated from the natural quartz materials exhibited such a shift. The significant differences observed between the two types of materials in both the ground-based TEM studies and the space radiation induced frequency changes suggest that there may be a correlation between the two observations.

TEM and STEM Studies on the Cross-sectional Morphologies of Dual-/Tri-layer Broadband SiO2 Antireflective Films

NASA Astrophysics Data System (ADS)

Wang, Shuangyue; Yan, Hongwei; Li, Dengji; Qiao, Liang; Han, Shaobo; Yuan, Xiaodong; Liu, Wei; Xiang, Xia; Zu, Xiaotao

2018-02-01

Dual-layer and tri-layer broadband antireflective (AR) films with excellent transmittance were successfully fabricated using base-/acid-catalyzed mixed sols and propylene oxide (PO) modified silica sols. The sols and films were characterized by scanning electron microscope (SEM), Fourier transform infrared spectroscopy (FTIR), nuclear magnetic resonance (NMR), transmission electron microscope (TEM), and scanning transmission electron microscope (STEM). FTIR and TEM results suggest that the PO molecules were covalently bonded to the silica particles and the bridge structure existing in PO modified silica sol is responsible for the low density of the top layer. The density ratio between different layers was measured by cross-sectional STEM, and the results are 1.69:1 and 2.1:1.7:1 from bottom-layer to top-layer for dual-layer and tri-layer films, respectively. The dual-layer film demonstrates good stability with 99.8% at the central wavelength of 351 nm and nearly 99.5% at the central wavelength of 1053 nm in laser system, and for the tri-layer AR film, the maximum transmittance reached nearly 100% at both the central wavelengths of 527 and 1053 nm.

TEM Studies: The Key for Understanding the Origin of the 3.3 V and 4.5 V Steps Observed in LiMn 2O 4-based Spinels

NASA Astrophysics Data System (ADS)

Dupont, L.; Hervieu, M.; Rousse, G.; Masquelier, C.; Palacín, M. R.; Chabre, Y.; Tarascon, J. M.

2000-12-01

Transmission electron microscopy (TEM) measurements were performed on electrochemically partially delithiated prepared spinel Li1-xMn2O4 samples. The potential-composition profile of LiMn2O4 exhibits (besides the two plateaus at 4.05 and 4.1 V) two additional redox steps of identical capacity at 4.5 and 3.3/3.95 V. We found by TEM studies that these extra steps are the signature of a reversible phase transition between LiMn2O4 spinel type structure and a new Li1-xMn2O4 double hexagonal (DH) type structure (a≈5.8 Å, c≈8.9 Å, P63mc). The latter is isotypic with DH LiFeSnO4. Selected area electron diffraction (SAED) and high-resolution transmission electron microscopy (HRTEM) made it possible to identify the mechanism by which this cubic-DH phase transition occurs within a particle. Based on the structural findings the origin as well as the similar electrochemical capacity of the 3.3/3.95 and 4.5 V anomalies are explained.

Kinetic precipitation of solution-phase polyoxomolybdate followed by transmission electron microscopy: a window to solution-phase nanostructure.

PubMed

Zhu, Yan; Cammers-Goodwin, Arthur; Zhao, Bin; Dozier, Alan; Dickey, Elizabeth C

2004-05-17

This study aimed to elucidate the structural nature of the polydisperse, nanoscopic components in the solution and the solid states of partially reduced polyoxomolybdate derived from the [Mo132] keplerate, [(Mo)Mo5]12-[Mo2 acetate]30. Designer tripodal hexamine-tris-crown ethers and nanoscopic molybdate coprecipitated from aqueous solution. These microcrystalline solids distributed particle radii between 2-30 nm as assayed by transmission electron microscopy (TEM). The solid materials and their particle size distributions were snap shots of the solution phase. The mother liquor of the preparation of the [Mo132] keplerate after three days revealed large species (r=20-30 nm) in the coprecipitate, whereas [Mo132] keplerate redissolved in water revealed small species (3-7 nm) in the coprecipitate. Nanoparticles of coprecipitate were more stable than solids derived solely from partially reduced molybdate. The TEM features of all material analyzed lacked facets on the nanometer length scale; however, the structures diffracted electrons and appeared to be defect-free as evidenced by Moiré patterns in the TEM images. Moiré patterns and size-invariant optical densities of the features in the micrographs suggested that the molybdate nanoparticles were vesicular.

The ultrastructural features of the premalignant oral lesions.

PubMed

Olinici, Doiniţa; Cotrutz, Carmen Elena; Mihali, Ciprian Valentin; Grecu, Vasile Bogdan; Botez, Emanuela Ana; Stoica, Laura; Onofrei, Pavel; Condurache, Oana; Dimitriu, Daniela Cristina

2018-01-01

Premalignant oral lesions are among the most important risk factors for the development of oral squamocellular carcinoma. Recent population studies indicate a significant rise in the prevalence of leukoplakia, erythroplakia/erythroleukoplakia, actinic cheilitis, submucous fibrosis and erosive lichen planus. Since standard histopathological examination has numerous limitations regarding the accurate appreciation of potential malignant transformation, the present study aims to aid these evaluations using the transmission electron microscopy (TEM) technique, which emphasizes ultrastructural changes pertaining to this pathology. Oral mucosa fragments collected from 43 patients that were clinically and histopathologically diagnosed with leukoplakia, erosive actinic cheilitis and erosive lichen planus have been processed through the classic technique for the examination using TEM and were examined using a Philips CM100 transmission electron microscope. The electron microscopy study has confirmed the histopathological diagnosis of the tissue samples examined using photonic microscopy and has furthermore revealed a series of ultrastructural details that on the one hand indicate the tendency for malignant transformation, and on the other reveal characteristic features of tumor development. All the details furnished by TEM complete the overall picture of morphological changes, specific to these lesions, indicating the importance of using these techniques in establishing both a correct diagnosis and prognosis.

Particle transport in low-collisionality H-mode plasmas on DIII-D

DOE PAGES

Mordijck, Saskia; Wang, Xin; Doyle, Edward J.; ...

2015-10-05

In this article we show that changing from an ion temperature gradient (ITG) to trapped electron mode (TEM) dominant turbulence regime (based on linear gyrokinetic simulations) results experimentally in a strong density pump-out (defined as a reduction in line-averaged density) in low collisionality, low power H-mode plasmas. We vary the turbulence drive by changing the heating from pre-dominantly ion heatedusing neutral beam injection to electron heated using electron cyclotron heating, which changes the T e/T i ratio and the temperature gradients. Perturbed gas puff experiments show an increase in transport outside ρ = 0.6, through a strong increase in themore » perturbed diffusion coefficient and a decrease in the inward pinch. Linear gyrokinetic simulations with TGLF show an increase in the particle flux outside the mid-radius. In conjunction an increase in intermediate-scale length density fluctuations is observed, which indicates an increase in turbulence intensity at typical TEM wavelengths. However, although the experimental changes in particle transport agree with a change from ITG to TEM turbulence regimes, we do not observe a reduction in the core rotation at mid-radius, nor a rotation reversal.« less

EBSD and TEM Characterization of High Burn-up Mixed Oxide Fuel

DOE Office of Scientific and Technical Information (OSTI.GOV)

Teague, Melissa C.; Gorman, Brian P.; Miller, Brandon D.

2014-01-01

Understanding and studying the irradiation behavior of high burn-up oxide fuel is critical to licensing of future fast breeder reactors. Advancements in experimental techniques and equipment are allowing for new insights into previously irradiated samples. In this work dual column focused ion beam (FIB)/scanning electron microscope (SEM) was utilized to prepared transmission electron microscope samples from mixed oxide fuel with a burn-up of 6.7% FIMA. Utilizing the FIB/SEM for preparation resulted in samples with a dose rate of <0.5 mRem/h compared to approximately 1.1 R/h for a traditionally prepared TEM sample. The TEM analysis showed that the sample taken frommore » the cooler rim region of the fuel pellet had approximately 2.5x higher dislocation density than that of the sample taken from the mid-radius due to the lower irradiation temperature of the rim. The dual column FIB/SEM was additionally used to prepared and serially slice approximately 25 um cubes. High quality electron back scatter diffraction (EBSD) were collected from the face at each step, showing, for the first time, the ability to obtain EBSD data from high activity irradiated fuel.« less

EELS from organic crystalline materials

NASA Astrophysics Data System (ADS)

Brydson, R.; Eddleston, M. D.; Jones, W.; Seabourne, C. R.; Hondow, N.

2014-06-01

We report the use of the electron energy loss spectroscopy (EELS) for providing light element chemical composition information from organic, crystalline pharmaceutical materials including theophylline and paracetamol and discuss how this type of data can complement transmission electron microscopy (TEM) imaging and electron diffraction when investigating polymorphism. We also discuss the potential for the extraction of bonding information using electron loss near-edge structure (ELNES).

Electron-beam irradiation induced transformation of Cu2(OH)3NO3 nanoflakes into nanocrystalline CuO

NASA Astrophysics Data System (ADS)

Padhi, S. K.; Gottapu, S. N.; Krishna, M. Ghanashyam

2016-05-01

The transmission electron microscope electron-beam (TEM e-beam) as a material modification tool has been demonstrated. The material modification is realised in the high-resolution TEM mode (largest condenser aperture, 150 μm, and 200 nm spot size) at a 200 keV beam energy. The Cu2(OH)3NO3 (CHN) nanoflakes used in this study were microwave solution processed that were layered single crystals and radiation sensitive. The single domain CHN flakes disintegrate into a large number of individual CuO crystallites within a 90 s span of time. The sequential bright-field, dark-field, and selected area electron diffraction modes were employed to record the evolved morphology, microstructural changes, and structural transformation that validate CHN modification. High-resolution transmission electron microscopy imaging of e-beam irradiated regions unambiguously supports the growth of CuO nanoparticles (11.8(3.2) nm in diameter). This study demonstrates e-beam irradiation induced CHN depletion, subsequent nucleation and growth of nanocrystalline CuO regions well embedded in the parent burnt porous matrix which can be useful for miniaturized sensing applications. NaBH4 induced room temperature reduction of CHN to elemental Cu and its printability on paper was also demonstrated.The transmission electron microscope electron-beam (TEM e-beam) as a material modification tool has been demonstrated. The material modification is realised in the high-resolution TEM mode (largest condenser aperture, 150 μm, and 200 nm spot size) at a 200 keV beam energy. The Cu2(OH)3NO3 (CHN) nanoflakes used in this study were microwave solution processed that were layered single crystals and radiation sensitive. The single domain CHN flakes disintegrate into a large number of individual CuO crystallites within a 90 s span of time. The sequential bright-field, dark-field, and selected area electron diffraction modes were employed to record the evolved morphology, microstructural changes, and structural transformation that validate CHN modification. High-resolution transmission electron microscopy imaging of e-beam irradiated regions unambiguously supports the growth of CuO nanoparticles (11.8(3.2) nm in diameter). This study demonstrates e-beam irradiation induced CHN depletion, subsequent nucleation and growth of nanocrystalline CuO regions well embedded in the parent burnt porous matrix which can be useful for miniaturized sensing applications. NaBH4 induced room temperature reduction of CHN to elemental Cu and its printability on paper was also demonstrated. Electronic supplementary information (ESI) available. See DOI: 10.1039/c6nr02572b

Comparison between measured and predicted turbulence frequency spectra in ITG and TEM regimes

NASA Astrophysics Data System (ADS)

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.

Minerals and aligned collagen fibrils in tilapia fish scales: structural analysis using dark-field and energy-filtered transmission electron microscopy and electron tomography.

PubMed

Okuda, Mitsuhiro; Ogawa, Nobuhiro; Takeguchi, Masaki; Hashimoto, Ayako; Tagaya, Motohiro; Chen, Song; Hanagata, Nobutaka; Ikoma, Toshiyuki

2011-10-01

The mineralized structure of aligned collagen fibrils in a tilapia fish scale was investigated using transmission electron microscopy (TEM) techniques after a thin sample was prepared using aqueous techniques. Electron diffraction and electron energy loss spectroscopy data indicated that a mineralized internal layer consisting of aligned collagen fibrils contains hydroxyapatite crystals. Bright-field imaging, dark-field imaging, and energy-filtered TEM showed that the hydroxyapatite was mainly distributed in the hole zones of the aligned collagen fibrils structure, while needle-like materials composed of calcium compounds including hydroxyapatite existed in the mineralized internal layer. Dark-field imaging and three-dimensional observation using electron tomography revealed that hydroxyapatite and needle-like materials were mainly found in the matrix between the collagen fibrils. It was observed that hydroxyapatite and needle-like materials were preferentially distributed on the surface of the hole zones in the aligned collagen fibrils structure and in the matrix between the collagen fibrils in the mineralized internal layer of the scale.

Characterization of Sulfur and Nanostructured Sulfur Battery Cathodes in Electron Microscopy Without Sublimation Artifacts

DOE Office of Scientific and Technical Information (OSTI.GOV)

Levin, Barnaby D. A.; Zachman, Michael J.; Werner, Jörg G.

Abstract Lithium sulfur (Li–S) batteries have the potential to provide higher energy storage density at lower cost than conventional lithium ion batteries. A key challenge for Li–S batteries is the loss of sulfur to the electrolyte during cycling. This loss can be mitigated by sequestering the sulfur in nanostructured carbon–sulfur composites. The nanoscale characterization of the sulfur distribution within these complex nanostructured electrodes is normally performed by electron microscopy, but sulfur sublimates and redistributes in the high-vacuum conditions of conventional electron microscopes. The resulting sublimation artifacts render characterization of sulfur in conventional electron microscopes problematic and unreliable. Here, we demonstratemore » two techniques, cryogenic transmission electron microscopy (cryo-TEM) and scanning electron microscopy in air (airSEM), that enable the reliable characterization of sulfur across multiple length scales by suppressing sulfur sublimation. We use cryo-TEM and airSEM to examine carbon–sulfur composites synthesized for use as Li–S battery cathodes, noting several cases where the commonly employed sulfur melt infusion method is highly inefficient at infiltrating sulfur into porous carbon hosts.« less

Correlative Magnetic Imaging of Heat-Assisted Magnetic Recording Media in Cross Section Using Lorentz TEM and MFM

DOE PAGES

Kim, Taeho Roy; Phatak, Charudatta; Petford-Long, Amanda K.; ...

2017-10-23

In order to increase the storage density of hard disk drives, a detailed understanding of the magnetic structure of the granular magnetic layer is essential. Here, we demonstrate an experimental procedure of imaging recorded bits on heat-assisted magnetic recording (HAMR) media in cross section using Lorentz transmission electron microscopy (TEM). With magnetic force microscopy and focused ion beam (FIB), we successfully targeted a single track to prepare cross-sectional TEM specimens. Then, we characterized the magnetic structure of bits with their precise location and orientation using Fresnel mode of Lorentz TEM. Here, this method can promote understanding of the correlation betweenmore » bits and their material structure in HAMR media to design better the magnetic layer.« less

Correlative Magnetic Imaging of Heat-Assisted Magnetic Recording Media in Cross Section Using Lorentz TEM and MFM

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kim, Taeho Roy; Phatak, Charudatta; Petford-Long, Amanda K.

In order to increase the storage density of hard disk drives, a detailed understanding of the magnetic structure of the granular magnetic layer is essential. Here, we demonstrate an experimental procedure of imaging recorded bits on heat-assisted magnetic recording (HAMR) media in cross section using Lorentz transmission electron microscopy (TEM). With magnetic force microscopy and focused ion beam (FIB), we successfully targeted a single track to prepare cross-sectional TEM specimens. Then, we characterized the magnetic structure of bits with their precise location and orientation using Fresnel mode of Lorentz TEM. Here, this method can promote understanding of the correlation betweenmore » bits and their material structure in HAMR media to design better the magnetic layer.« less

Species Profiles: Life Histories and Environmental Requirements of Coastal Fishes and Invertebrates (Pacific Southwest). Chinook Salmon.

DTIC Science & Technology

1986-04-01

LAS UN SFED M AALLE NET A 6 F iS-82- 49 F/G /3 U INLA E NEhhIhLson1hsohhIN I flflflfl.... 1.0 ~2𔃻’l lim MICROCOPY RESOLUTION TESI CHART NATIONAL...22 II it released from Coleman National Fish Nordstrom, D. 1977. Hydrogeochemical Hatchery, on naturally produced and microbiological factors affect

An Integrated Micro- and Macroarchitectural Analysis of the Drosophila Brain by Computer-Assisted Serial Section Electron Microscopy

PubMed Central

Cardona, Albert; Saalfeld, Stephan; Preibisch, Stephan; Schmid, Benjamin; Cheng, Anchi; Pulokas, Jim; Tomancak, Pavel; Hartenstein, Volker

2010-01-01

The analysis of microcircuitry (the connectivity at the level of individual neuronal processes and synapses), which is indispensable for our understanding of brain function, is based on serial transmission electron microscopy (TEM) or one of its modern variants. Due to technical limitations, most previous studies that used serial TEM recorded relatively small stacks of individual neurons. As a result, our knowledge of microcircuitry in any nervous system is very limited. We applied the software package TrakEM2 to reconstruct neuronal microcircuitry from TEM sections of a small brain, the early larval brain of Drosophila melanogaster. TrakEM2 enables us to embed the analysis of the TEM image volumes at the microcircuit level into a light microscopically derived neuro-anatomical framework, by registering confocal stacks containing sparsely labeled neural structures with the TEM image volume. We imaged two sets of serial TEM sections of the Drosophila first instar larval brain neuropile and one ventral nerve cord segment, and here report our first results pertaining to Drosophila brain microcircuitry. Terminal neurites fall into a small number of generic classes termed globular, varicose, axiform, and dendritiform. Globular and varicose neurites have large diameter segments that carry almost exclusively presynaptic sites. Dendritiform neurites are thin, highly branched processes that are almost exclusively postsynaptic. Due to the high branching density of dendritiform fibers and the fact that synapses are polyadic, neurites are highly interconnected even within small neuropile volumes. We describe the network motifs most frequently encountered in the Drosophila neuropile. Our study introduces an approach towards a comprehensive anatomical reconstruction of neuronal microcircuitry and delivers microcircuitry comparisons between vertebrate and insect neuropile. PMID:20957184

Comprehensive analysis of TEM methods for LiFePO4/FePO4 phase mapping: spectroscopic techniques (EFTEM, STEM-EELS) and STEM diffraction techniques (ACOM-TEM).

PubMed

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.

Pulsed Laser Ablation-Induced Green Synthesis of TiO2 Nanoparticles and Application of Novel Small Angle X-Ray Scattering Technique for Nanoparticle Size and Size Distribution Analysis.

PubMed

Singh, Amandeep; Vihinen, Jorma; Frankberg, Erkka; Hyvärinen, Leo; Honkanen, Mari; Levänen, Erkki

2016-12-01

This paper aims to introduce small angle X-ray scattering (SAXS) as a promising technique for measuring size and size distribution of TiO 2 nanoparticles. In this manuscript, pulsed laser ablation in liquids (PLAL) has been demonstrated as a quick and simple technique for synthesizing TiO 2 nanoparticles directly into deionized water as a suspension from titanium targets. Spherical TiO 2 nanoparticles with diameters in the range 4-35 nm were observed with transmission electron microscopy (TEM). X-ray diffraction (XRD) showed highly crystalline nanoparticles that comprised of two main photoactive phases of TiO 2 : anatase and rutile. However, presence of minor amounts of brookite was also reported. The traditional methods for nanoparticle size and size distribution analysis such as electron microscopy-based methods are time-consuming. In this study, we have proposed and validated SAXS as a promising method for characterization of laser-ablated TiO 2 nanoparticles for their size and size distribution by comparing SAXS- and TEM-measured nanoparticle size and size distribution. SAXS- and TEM-measured size distributions closely followed each other for each sample, and size distributions in both showed maxima at the same nanoparticle size. The SAXS-measured nanoparticle diameters were slightly larger than the respective diameters measured by TEM. This was because SAXS measures an agglomerate consisting of several particles as one big particle which slightly increased the mean diameter. TEM- and SAXS-measured mean diameters when plotted together showed similar trend in the variation in the size as the laser power was changed which along with extremely similar size distributions for TEM and SAXS validated the application of SAXS for size distribution measurement of the synthesized TiO 2 nanoparticles.

TEM Analysis of Interfaces in Diffusion-Bonded Silicon Carbide Ceramics Joined Using Metallic Interlayers

NASA Technical Reports Server (NTRS)

Ozaki, T.; Tsuda, H.; Halbig, M. C.; Singh, M.; Hasegawa, Y.; Mori, S.; Asthana R.

2016-01-01

Silicon Carbide (SiC) is a promising material for thermo-structural applications due to its excellent high-temperature mechanical properties, oxidation resistance, and thermal stability. However, joining and integration technologies are indispensable for this material in order to fabricate large size and complex shape components with desired functionalities. Although diffusion bonding techniques using metallic interlayers have been commonly utilized to bond various SiC ceramics, detailed microstructural observation by Transmission Electron Microscopy (TEM) of the bonded area has not been carried out due to difficulty in preparing TEM samples. In this study, we tried to prepare TEM samples from joints of diffusion bonded SiC ceramics by Focused Ion Beam (FIB) system and carefully investigated the interfacial microstructure by TEM analysis. The samples used in this study were SiC fiber bonded ceramics (SA-Tyrannohex: SA-THX) diffusion bonded with metallic interlayers such as Ti, TiMo, and Mo-B. In this presentation, the result of microstructural analysis obtained by TEM observations and the influence of metallic interlayers and fiber orientation of SA-THX on the joint microstructure will be discussed.

TEM Analysis of Diffusion-Bonded Silicon Carbide Ceramics Joined Using Metallic Interlayers

NASA Technical Reports Server (NTRS)

Ozaki, T.; Tsuda, H.; Halbig, M. C.; Singh, M.; Hasegawa, Y; Mori, S.; Asthana, R.

2017-01-01

Silicon Carbide (SiC) is a promising material for thermostructural applications due to its excellent high-temperature mechanical properties, oxidation resistance, and thermal stability. However, joining and integration technologies are indispensable for this material in order to fabricate large size and complex shape components with desired functionalities. Although diffusion bonding techniques using metallic interlayers have been commonly utilized to bond various SiC ceramics, detailed microstructural observation by Transmission Electron Microscopy (TEM) of the bonded area has not been carried out due to difficulty in preparing TEM samples. In this study, we tried to prepare TEM samples from joints of diffusion bonded SiC ceramics by Focused Ion Beam (FIB) system and carefully investigated the interfacial microstructure by TEM analysis. The samples used in this study were SiC fiber bonded ceramics (SA-Tyrannohex: SA-THX) diffusion bonded with metallic interlayers such as Ti, TiMo, Mo-B and TiCu. In this presentation, we report the microstructure of diffusion bonded SA-THX mainly with TiCu interlayers obtained by TEM observations, and the influence of metallic interlayers on the joint microstructure and microhardness will be discussed.

One-dimensional nanoferroic rods; synthesis and characterization

NASA Astrophysics Data System (ADS)

Ahmed, M. A.; Seddik, U.; Okasha, N.; Imam, N. G.

2015-11-01

One-dimensional nanoferroic rods of BaTiO3 were synthesized by improved citrate auto-combustion technology using tetrabutyl titanate. X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray (EDX), transmission electron microscopy (TEM), atomic force microscopy (AFM) and Fourier transform infrared spectroscopy (FTIR) have been used to characterize the prepared sample. The results indicated that the crystal structure of BaTiO3 is tetragonal phase with an average crystallite size of 47 nm. SEM image gives a cauliflower-like morphology of the agglomerated nanorods. The stoichiometry of the chemical composition of the BaTiO3 ceramic was confirmed by EDX. TEM micrograph exhibited that BaTiO3 nanoparticles have rod-like shape with an average length of 120 nm and width of 43 nm. AFM was used to investigate the surface topography and its roughness. The topography image in 3D showed that the BaTiO3 particles have a rod shape with an average particle size of 116 nm which in agreement with 3D TEM result.

Selective Capture of Histidine-tagged Proteins from Cell Lysates Using TEM grids Modified with NTA-Graphene Oxide

NASA Astrophysics Data System (ADS)

Benjamin, Christopher J.; Wright, Kyle J.; Bolton, Scott C.; Hyun, Seok-Hee; Krynski, Kyle; Grover, Mahima; Yu, Guimei; Guo, Fei; Kinzer-Ursem, Tamara L.; Jiang, Wen; Thompson, David H.

2016-10-01

We report the fabrication of transmission electron microscopy (TEM) grids bearing graphene oxide (GO) sheets that have been modified with Nα, Nα-dicarboxymethyllysine (NTA) and deactivating agents to block non-selective binding between GO-NTA sheets and non-target proteins. The resulting GO-NTA-coated grids with these improved antifouling properties were then used to isolate His6-T7 bacteriophage and His6-GroEL directly from cell lysates. To demonstrate the utility and simplified workflow enabled by these grids, we performed cryo-electron microscopy (cryo-EM) of His6-GroEL obtained from clarified E. coli lysates. Single particle analysis produced a 3D map with a gold standard resolution of 8.1 Å. We infer from these findings that TEM grids modified with GO-NTA are a useful tool that reduces background and improves both the speed and simplicity of biological sample preparation for high-resolution structure elucidation by cryo-EM.

Preparation and analysis of particulate metal deposits

NASA Technical Reports Server (NTRS)

Poppa, H.; Moorhead, D.; Heinemann, K.

1985-01-01

Small particles and clusters of palladium were grown by deposition from the vapor phase under ultrahigh vacuum conditions. Amorphous and crystalline support films of Al2O3 and ultrathin amorphous carbon films were used as substrate materials. The growth of the metal deposit was monitored in situ by scanning transmission diffraction of energy-filtered 100 kV electrons and high resolution transmission electron microscopy (TEM) analysis was performed in a separate instrument. It was established by in situ TEM, however, that the transfer of specimens in this case did not unduly affect the size and distribution of deposit particles. It was found that the cleanness, stoichiometry, crystallinity and structural perfection of the support surface play an essential role in determining the crystalline perfection and structure of the particles. The smallest palladium clusters reproducibly prepared contained not more than six atoms but size determinations below 1 nm average particle diameter are very problematic with conventional TEM. Palladium particles grown on carbon supports feature an impurity-stabilized mosaic structure.

ERDA, RBS, TEM and SEM characterization of microstructural evolution in helium-implanted Hastelloy N alloy

NASA Astrophysics Data System (ADS)

Gao, Jie; Bao, Liangman; Huang, Hefei; Li, Yan; Lei, Qiantao; Deng, Qi; Liu, Zhe; Yang, Guo; Shi, Liqun

2017-05-01

Hastelloy N alloy was implanted with 30 keV, 5 × 1016 ions/cm2 helium ions at room temperature, and subsequent annealed at 600 °C for 1 h and further annealed at 850 °C for 5 h in vacuum. Using elastic recoil detection analysis (ERDA) and transmission electron microscopy (TEM), the depth profiles of helium concentration and helium bubbles in helium-implanted Hastelloy N alloy were investigated, respectively. The diffusion of helium and molybdenum elements to surface occurred during the vacuum annealing at 850 °C (5 h). It was also observed that bubbles in molybdenum-enriched region were much larger in size than those in deeper region. In addition, it is worth noting that plenty of nano-holes can be observed on the surface of helium-implanted sample after high temperature annealing by scanning electron microscope (SEM). This observation provides the evidence for the occurrence of helium release, which can be also inferred from the results of ERDA and TEM analysis.

Selective Capture of Histidine-tagged Proteins from Cell Lysates Using TEM grids Modified with NTA-Graphene Oxide.

PubMed

Benjamin, Christopher J; Wright, Kyle J; Bolton, Scott C; Hyun, Seok-Hee; Krynski, Kyle; Grover, Mahima; Yu, Guimei; Guo, Fei; Kinzer-Ursem, Tamara L; Jiang, Wen; Thompson, David H

2016-10-17

We report the fabrication of transmission electron microscopy (TEM) grids bearing graphene oxide (GO) sheets that have been modified with N α , N α -dicarboxymethyllysine (NTA) and deactivating agents to block non-selective binding between GO-NTA sheets and non-target proteins. The resulting GO-NTA-coated grids with these improved antifouling properties were then used to isolate His 6 -T7 bacteriophage and His 6 -GroEL directly from cell lysates. To demonstrate the utility and simplified workflow enabled by these grids, we performed cryo-electron microscopy (cryo-EM) of His 6 -GroEL obtained from clarified E. coli lysates. Single particle analysis produced a 3D map with a gold standard resolution of 8.1 Å. We infer from these findings that TEM grids modified with GO-NTA are a useful tool that reduces background and improves both the speed and simplicity of biological sample preparation for high-resolution structure elucidation by cryo-EM.

Calcium copper-titanate thin film growth: tailoring of the operational conditions through nanocharacterization and substrate nature effects.

PubMed

Lo Nigro, Raffaella; Toro, Roberta G; Malandrino, Graziella; Fragalà, Ignazio L; Losurdo, Maria; Giangregorio, Michelaria M; Bruno, Giovanni; Raineri, Vito; Fiorenza, Patrick

2006-09-07

A novel approach based on a molten multicomponent precursor source has been applied for the MOCVD fabrication of high-quality CaCu(3)Ti(4)O(12) (CCTO) thin films on various substrates. The adopted in situ strategy involves a molten mixture consisting of Ca(hfa)(2).tetraglyme, Ti(tmhd)(2)(O-iPr)(2), and Cu(tmhd)(2) [Hhfa = 1,1,1,5,5,5-hexafluoro-2,4-pentanedione; tetraglyme = 2,5,8,11,14-pentaoxapentadecane; Htmhd = 2,2,6,6-tetramethyl-3,5-heptandione; O-iPr = isopropoxide] precursors. Film structural and morphological characterizations have been carried out by several techniques [X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM)], and in particular the energy filtered TEM mapping and X-ray energy dispersive (EDX) analysis in TEM mode provided a suitable correlation between nanostructural properties of CCTO films and deposition conditions and/or the substrate nature. Correlation between the nanostructure and optical/dielectric properties has been investigated exploiting spectroscopic ellipsometry.

Detailed Investigation of Core-Shell Precipitates in a Cu-Containing High Entropy Alloy

NASA Astrophysics Data System (ADS)

Alam, T.; Gwalani, B.; Viswanathan, G.; Fraser, H.; Banerjee, R.

2018-05-01

Due to the competing influences of configurational entropy and enthalpy of mixing, in recent years, secondary (including intermetallic) phases have been reported in many high entropy alloy (HEA) systems. These secondary phases offer great potential in terms of strengthening the HEA beyond the solid solution strengthening effects, and as such are of great interest in regards to alloy design for engineering applications. The present research investigates novel nano-scale core-shell precipitates forming within the disordered bcc matrix phase of an Al2CrCuFeNi2 HEA, utilizing complementary high-resolution microscopy techniques of atom probe tomography (APT) and transmission electron microscopy (TEM). The size, morphology, and local chemistry of these core-shell precipitates was measured by APT, and the composition was further corroborated by high-resolution scanning transmission electron microscopy-energy dispersive spectroscopy in an aberration-corrected TEM. Furthermore, high-resolution TEM imaging of the core-shell structure indicates that the Cu-rich core exhibits a bcc crystal structure.

Size distribution and volume fraction of T(1) phase precipitates from TEM images: Direct measurements and related correction.

PubMed

Dorin, Thomas; Donnadieu, Patricia; Chaix, Jean-Marc; Lefebvre, Williams; Geuser, Frédéric De; Deschamps, Alexis

2015-11-01

Transmission Electron Microscopy (TEM) can be used to measure the size distribution and volume fraction of fine scale precipitates in metallic systems. However, such measurements suffer from a number of artefacts that need to be accounted for, related to the finite thickness of the TEM foil and to the projected observation in two dimensions of the microstructure. We present a correction procedure to describe the 3D distribution of disc-like particles and apply this method to the plate-like T1 precipitates in an Al-Li-Cu alloy in two ageing conditions showing different particle morphologies. The precipitates were imaged in a High-Angular Annular Dark Field Microscope (HAADF-STEM). The corrected size distribution is further used to determine the precipitate volume fraction. Atom probe tomography (APT) is finally utilised as an alternative way to measure the precipitate volume fraction and test the validity of the electron microscopy results. Copyright © 2015 Elsevier Ltd. All rights reserved.

Dopant concentration dependent growth of Fe:ZnO nanostructures

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sahai, Anshuman; Goswami, Navendu, E-mail: navendugoswami@gmail.com

2016-05-23

Systematic investigations of structural properties of 1-10% Fe doped ZnO nanostructure (Fe:ZnO NS) prepared via chemical precipitation method have been reported. Structural properties were probed thoroughly employing scanning electron microscope (SEM) and transmission electron microscope (TEM), energy dispersive X-ray (EDAX) analysis and X-ray diffraction (XRD). Morphological transformation of nanostructures (NS) with Fe incorporation is evident in SEM/TEM images. Nanoparticles (NP) obtained with 1% Fe, evolve to nanorods (NR) for 3% Fe; NR transform to nanocones (NC) (for 5% and 7% Fe) and finally NC transform to nanoflakes (NF) at 10% Fe. Morover, primary phase of Zn{sub 1-x}Fe{sub x}O along withmore » secondary phases of ZnFe{sub 2}O{sub 4} and Fe{sub 2}O{sub 3} were also revealed through XRD measurements. Based on collective XRD, SEM, TEM, and EDAX interpretations, a model for morphological evolution of NS was proposed and the pivotal role of Fe dopant was deciphered.« less

Effect of cobalt doping on structural and optical properties of ZnO nanoparticles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Singh, J.; Chanda, A., E-mail: anupamamatsc@gmail.com; Gupta, S.

Cobalt doped ZnO nanoparticles of uniform sizes were prepared by a chemical method using ZnCl{sub 2} and NaOH as the source materials. The formation of Co-doped ZnO nanoparticles was confirmed by transmission electron microscopy (TEM), high resolution TEM (HR-TEM) and selected area electron diffraction (SAED) studies. The optical properties of obtained products were examined using room temperature UV-visible and FTIR spectroscopy. SAED of cobalt doped ZnO nanoparticles shows homogeneous distribution of nanoparticles with hexagonal structure. The HRTEM image of the Co-doped ZnO nanoparticles reveals a clear lattice spacing of 0.52 nm corresponding to the interplanar spacing of wurtzite ZnO (002) plane.more » The absorption band at 857 cm{sup −1} in FTIR spectra confirmed the tetrahedral coordination of Zn and a shift of absorption peak to shorter wavelength region and decrease in absorbance with Co doping.is observed in UV-Visible spectra.« less

Reduction reactions and densification during in situ TEM heating of iron oxide nanochains

NASA Astrophysics Data System (ADS)

Bonifacio, Cecile S.; Das, Gautom; Kennedy, Ian M.; van Benthem, Klaus

2017-12-01

The reduction reactions and densification of nanochains assembled from γ-Fe2O3 nanoparticles were investigated using in situ transmission electron microscopy (TEM). Morphological changes and reduction of the metal oxide nanochains were observed during in situ TEM annealing through simultaneous imaging and quantitative analysis of the near-edge fine structures of Fe L2,3 absorption edges acquired by spatially resolved electron energy loss spectroscopy. A change in the oxidation states during annealing of the iron oxide nanochains was observed with phase transformations due to continuous reduction from Fe2O3 over Fe3O4, FeO to metallic Fe. Phase transitions during the in situ heating experiments were accompanied with morphological changes in the nanochains, specifically rough-to-smooth surface transitions below 500 °C, neck formation between adjacent particles around 500 °C, and subsequent neck growth. At higher temperatures, coalescence of FeO particles was observed, representing densification.

Electron microscopy investigations of nanoparticles for cancer diagnostic applications

NASA Astrophysics Data System (ADS)

Koh, Ai Leen

This dissertation concerns electron microscopy characterization of magnetic (MNP) and surface enhanced Raman scattering (SERS) nanoparticles for in-vitro cancer diagnostic applications. Electron microscopy is an essential characterization tool owing to its (sub) nanometer spatial resolution. Structural information about the nanoparticles can be obtained using transmission electron microscopy (TEM), which can in turn be correlated to their physical characteristics. The scanning electron microscope (SEM) has excellent depth of field and can be effectively utilized to obtain high resolution information about nanoparticles binding onto cell surfaces. Part One of this thesis focuses on MNPs for bio-sensing and detection applications. As a preliminary study, chemically-synthesized, commercially-available iron oxide nanoparticles were compared against their laboratory-synthesized counterparts to assess their suitability for this application. The motivation for this initial study came about due to the lack of published data on commercially available iron oxide nanoparticles. TEM studies show that the latter are "beads" composed of multiple iron oxide cores encapsulated by a polymer shell, with large standard deviations in core diameter. Laboratory-synthesized iron oxide nanoparticles, on the other hand, are single core particles with small variations in diameter and therefore are expected to be better candidates for the required application. A key limitation in iron oxide nanoparticles is their relatively weak magnetic signals. The development of high moment Synthetic Anti-Ferromagnetic (SAF) nanoparticles aims to overcome this issue. SAFs are a novel class of MNPs fabricated using nanoimprint lithography, direct deposition of multilayer structure and final suspension into liquid medium (water). TEM analyses of cross-section specimens reveal that the SAFs possess characteristics similar to those of sputtered magnetic multilayer thin films. Their layered structure is preserved after a chemical etch. Magnetic measurements show a slight decrease in magnetic moment after ion milling. From TEM characterization, the introduction of oxygen into the copper release layer, prior the film deposition process, can effectively control the topography of the oxidized-copper grains and, consequently, lead to the production of SAF nanoparticles with flatter layers. Size distribution studies performed on SAFs fabricated using self-assembled stamps show that it is possible to produce monodisperse nanoparticles with diameters from 70 nm up. Part Two of the dissertation describes structural characterization experiments performed on Composite Organic-Inorganic Nanoparticles (COINs), which are a novel type of SERS nanoclusters formed by aggregating silver nanoparticles with Raman molecules, and then encapsulating them with an organic coating that stabilizes the aggregates and promotes subsequent functionalization with antibodies. Part Three of this dissertation focuses on the development and application of electron microscopy-based techniques to characterize the nanomaterial-biology interactions, to assess how, or indeed whether, nanoparticles are attaching to the cancer cells. The technique of negative staining was applied to simultaneously visualize inorganic nanoparticles and their biofunctionalized entities under the TEM and to verify the successful functionalization of nanoparticles with antibodies. The interpretation of the negatively-stained COINs was consistent with the EFTEM data. Next, the localization and characterization of CD54-functionalized COINs on the apicolateral portions of U937 leukemia cell lines was determined using TEM, SEM and Scanning Auger Microscopy. The analyses show that CD54 antigens are localized at a specific region on U937 leukemia cell surfaces. SEM imaging and SER spectroscopy correlation studies of different antibody-conjugated COINs attached onto different cancer cell lines show a direct correlation between the number of COINs binding to cells and the corresponding SER intensity. Finally, TEM was used to locate intra-cellularly labeled COINs and to trace the phospho-stat6 signaling pathway in U937 leukemia cells, demonstrating that COINs can be used to detect intracellular phosphorylation signaling events. These experiments demonstrate the importance of electron microscopy for analyzing the material-biology interface and for validating the attachment of nanoparticles on and in cells. Thus, electron microscope provides complementary imaging and spectroscopic information to current magnetic and SERS bio-detection technologies. (Abstract shortened by UMI.)

Electric current distribution of a multiwall carbon nanotube

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chen, Li-Ying; Chang, Chia-Seng, E-mail: jasonc@phys.sinica.edu.tw; Institute of Physics, Academia Sinica, Taipei 11529, Taiwan

2016-07-15

The electric current distribution in a multiwall carbon nanotube (MWCNT) was studied by in situ measuring the electric potential along an individual MWCNT in the ultra-high vacuum transmission electron microscope (TEM). The current induced voltage drop along each section of a side-bonded MWCNT was measured by a potentiometric probe in TEM. We have quantitatively derived that the current on the outermost shell depends on the applied current and the shell diameter. More proportion of the total electronic carriers hop into the inner shells when the applied current is increased. The larger a MWCNT’s diameter is, the easier the electronic carriersmore » can hop into the inner shells. We observed that, for an 8 nm MWCNT with 10 μA current applied, 99% of the total current was distributed on the outer two shells.« less

Revealing 3D Ultrastructure and Morphology of Stem Cell Spheroids by Electron Microscopy.

PubMed

Jaros, Josef; Petrov, Michal; Tesarova, Marketa; Hampl, Ales

2017-01-01

Cell culture methods have been developed in efforts to produce biologically relevant systems for developmental and disease modeling, and appropriate analytical tools are essential. Knowledge of ultrastructural characteristics represents the basis to reveal in situ the cellular morphology, cell-cell interactions, organelle distribution, niches in which cells reside, and many more. The traditional method for 3D visualization of ultrastructural components, serial sectioning using transmission electron microscopy (TEM), is very labor-intensive due to contentious TEM slice preparation and subsequent image processing of the whole collection. In this chapter, we present serial block-face scanning electron microscopy, together with complex methodology for spheroid formation, contrasting of cellular compartments, image processing, and 3D visualization. The described technique is effective for detailed morphological analysis of stem cell spheroids, organoids, as well as organotypic cell cultures.

In situ TEM study of the Li-Au reaction in an electrochemical liquid cell.

PubMed

Zeng, Zhiyuan; Liang, Wen-I; Chu, Ying-Hao; Zheng, Haimei

2014-01-01

We study the lithiation of a Au electrode in an electrochemical liquid cell using transmission electron microscopy (TEM). The commercial liquid electrolyte for lithium ion batteries (1 M lithium hexafluorophosphate LiPF6 dissolved in 1 : 1 (v/v) ethylene carbonate (EC) and diethyl carbonate (DEC)) was used. Three distinct types of morphology change during the reaction, including gradual dissolution, explosive reaction and local expansion/shrinkage, are observed. It is expected that significant stress is generated from lattice expansion during lithium-gold alloy formation. There is vigorous bubble formation from electrolyte decomposition, likely due to the catalytic effect of Au, while the bubble generation is less severe with titanium electrodes. There is an increase of current in response to electron beam irradiation, and electron beam effects on the observed electrochemical reaction are discussed.

Stable tetragonal phase and magnetic properties of Fe-doped HfO2 nanoparticles

NASA Astrophysics Data System (ADS)

Sales, T. S. N.; Cavalcante, F. H. M.; Bosch-Santos, B.; Pereira, L. F. D.; Cabrera-Pasca, G. A.; Freitas, R. S.; Saxena, R. N.; Carbonari, A. W.

2017-05-01

In this paper, the effect in structural and magnetic properties of iron doping with concentration of 20% in hafnium dioxide (HfO2) nanoparticles is investigated. HfO2 is a wide band gap oxide with great potential to be used as high-permittivity gate dielectrics, which can be improved by doping. Nanoparticle samples were prepared by sol-gel chemical method and had their structure, morphology, and magnetic properties, respectively, investigated by X-ray diffraction (XRD), transmission electron microscopy (TEM) and scanning electron microscopy (SEM) with electron back scattering diffraction (EBSD), and magnetization measurements. TEM and SEM results show size distribution of particles in the range from 30 nm to 40 nm with small dispersion. Magnetization measurements show the blocking temperature at around 90 K with a strong paramagnetic contribution. XRD results show a major tetragonal phase (94%).

A Shear Strain Route Dependency of Martensite Formation in 316L Stainless Steel.

PubMed

Kang, Suk Hoon; Kim, Tae Kyu; Jang, Jinsung; Oh, Kyu Hwan

2015-06-01

In this study, the effect of simple shearing on microstructure evolution and mechanical properties of 316L austenitic stainless steel were investigated. Two different shear strain routes were obtained by twisting cylindrical specimens in the forward and backward directions. The strain-induced martensite phase was effectively obtained by alteration of the routes. Formation of the martensite phase clearly resulted in significant hardening of the steel. Grain-size reduction and strain-induced martensitic transformation within the deformed structures of the strained specimens were characterized by scanning electron microscopy - electron back-scattered diffraction, X-ray diffraction, and the TEM-ASTAR (transmission electron microscopy - analytical scanning transmission atomic resolution, automatic crystal orientation/phase mapping for TEM) system. Significant numbers of twin networks were formed by alteration of the shear strain routes, and the martensite phases were nucleated at the twin interfaces.

Simultaneous cathodoluminescence and electron microscopy cytometry of cellular vesicles labeled with fluorescent nanodiamonds.

PubMed

Nagarajan, Sounderya; Pioche-Durieu, Catherine; Tizei, Luiz H G; Fang, Chia-Yi; Bertrand, Jean-Rémi; Le Cam, Eric; Chang, Huan-Cheng; Treussart, François; Kociak, Mathieu

2016-06-02

Light and Transmission Electron Microscopies (LM and TEM) hold potential in bioimaging owing to the advantages of fast imaging of multiple cells with LM and ultrastructure resolution offered by TEM. Integrated or correlated LM and TEM are the current approaches to combine the advantages of both techniques. Here we propose an alternative in which the electron beam of a scanning TEM (STEM) is used to excite concomitantly the luminescence of nanoparticle labels (a process known as cathodoluminescence, CL), and image the cell ultrastructure. This CL-STEM imaging allows obtaining luminescence spectra and imaging ultrastructure simultaneously. We present a proof of principle experiment, showing the potential of this technique in image cytometry of cell vesicular components. To label the vesicles we used fluorescent diamond nanocrystals (nanodiamonds, NDs) of size ≈150 nm coated with different cationic polymers, known to trigger different internalization pathways. Each polymer was associated with a type of ND with a different emission spectrum. With CL-STEM, for each individual vesicle, we were able to measure (i) their size with nanometric resolution, (ii) their content in different ND labels, and realize intracellular component cytometry. In contrast to the recently reported organelle flow cytometry technique that requires cell sonication, CL-STEM-based image cytometry preserves the cell integrity and provides a much higher resolution in size. Although this novel approach is still limited by a low throughput, the automatization of data acquisition and image analysis, combined with improved intracellular targeting, should facilitate applications in cell biology at the subcellular level.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Patel, Sangeeta, E-mail: spt658@aucklanduni.ac.nz; Wei, Shanghai; Han, Jie

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

Intrinsic microstructure of Si/GaAs heterointerfaces fabricated by surface-activated bonding at room temperature

NASA Astrophysics Data System (ADS)

Ohno, Yutaka; Yoshida, Hideto; Takeda, Seiji; Liang, Jianbo; Shigekawa, Naoteru

2018-02-01

The intrinsic microstructure of Si/GaAs heterointerfaces fabricated by surface-activated bonding at room temperature is examined by plane-view transmission electron microscopy (TEM) and cross-sectional scanning TEM using damage-free TEM specimens prepared only by mechanochemical etching. The bonded heterointerfaces include an As-deficient crystalline GaAs layer with a thickness of less than 1 nm and an amorphous Si layer with a thickness of approximately 3 nm, introduced by the irradiation of an Ar atom beam for surface activation before bonding. It is speculated that the interface resistance mainly originates from the As-deficient defects in the former layer.

3D TEM reconstruction and segmentation process of laminar bio-nanocomposites

DOE Office of Scientific and Technical Information (OSTI.GOV)

Iturrondobeitia, M., E-mail: maider.iturrondobeitia@ehu.es; Okariz, A.; Fernandez-Martinez, R.

2015-03-30

The microstructure of laminar bio-nanocomposites (Poly (lactic acid)(PLA)/clay) depends on the amount of clay platelet opening after integration with the polymer matrix and determines the final properties of the material. Transmission electron microscopy (TEM) technique is the only one that can provide a direct observation of the layer dispersion and the degree of exfoliation. However, the orientation of the clay platelets, which affects the final properties, is practically immeasurable from a single 2D TEM image. This issue can be overcome using transmission electron tomography (ET), a technique that allows the complete 3D characterization of the structure, including the measurement ofmore » the orientation of clay platelets, their morphology and their 3D distribution. ET involves a 3D reconstruction of the study volume and a subsequent segmentation of the study object. Currently, accurate segmentation is performed manually, which is inefficient and tedious. The aim of this work is to propose an objective/automated segmentation methodology process of a 3D TEM tomography reconstruction. In this method the segmentation threshold is optimized by minimizing the variation of the dimensions of the segmented objects and matching the segmented V{sub clay} (%) and the actual one. The method is first validated using a fictitious set of objects, and then applied on a nanocomposite.« less

Transmission electron microscopy of polyhydroxybutyrate-co-valerate (PHBV)/nanocrystalline cellulose (NCC) bio-nanocomposite prepared using cryo-ultramicrotomy

NASA Astrophysics Data System (ADS)

Ismarul, N. I.; Engku, A. H. E. U.; Siti, N. K.; Tay, K. Y.

2017-12-01

Environmental issues on disposal and end-of-life for product made from synthetic petroleum-derived polymers have gained increasing attention from materials scientist to search for new materials with similar physical and mechanical properties but environmental friendly in a way that they are renewable and biodegradable as well. This work is to study the effect of nanocrystalline cellulose in improving the thermal stability of polyhydroxybutyrate-co-valerate biopolymer for high temperature processing of packaging material. 10 % w/w PHBV-NCC bio-nanocomposite feedstock pellet prepared using RONDOL minilab compounder was used as the sample for the preparation of Transmission Electron Microscopy (TEM) sample. RMC Cryo-Ultramicrotomy equipment was used to prepare the ultra-thin slice of the bio-nanocomposite pellet under liquid nitrogen at - 60 °C. Diamond knife was used to slice off about 80-100 nm ultra-thin bio-nanocomposite films and was transferred into the lacey carbon film coated grid using cooled sugar solution. A few drops of phosphotungstic acid was used as negative stain to improve the contrast during the TEM analysis. HITACHI TEM systems was used to obtain the TEM micrograph of PHBV-NCC bio-nanocomposite using 80kV accelerating voltage. A well dispersed NCC in PHBV matrix, ranging from 5 to 25 nm in width was observed.

TEM heat transport and fluctuations in the HSX stellarator: experiments and comparison with gyrokinetic simulation

NASA Astrophysics Data System (ADS)

Smoniewski, J.; Faber, B. J.; Sánchez, E.; Calvo, I.; Pueschel, M. J.; Likin, K. M.; Deng, C. B.; Talmadge, J. N.

2017-10-01

The Helically Symmetric eXperiment (HSX) has demonstrated reduced neoclassical transport in the plasma core with quasi-symmetry [Lore Thesis 2010], while outside this region the electron thermal diffusivity is well above the neoclassical level, likely due to the Trapped Electron Mode (TEM) [Weir PoP 2015, Faber PoP 2015]. We compare gyrokinetic simulations of the TEM to experimental heat flux and density fluctuation measurements for two configurations: Quasi-Helical Symmetry (QHS) and broken symmetry (Mirror). Both experiment and simulation show that the heat flux for Mirror is larger than for QHS by about a factor of two. Initial interferometer measurements provide evidence that density-gradient-driven TEMs are driving turbulence. Calculations of the collisionless damping of zonal flows provide another perspective into the difference between geometries. Similar to other stellarators [Monreal PPCF 2016], the zonal flow residual goes to zero at long wavelengths in both configurations. Additionally, the very short time decay of the zonal flow due to neoclassical polarization is constant between configurations. However, the collisionless damping time is longer and the zonal flow oscillation frequency is smaller in QHS than Mirror, consistent with reduced radial particle drifts. Work supported by the US DOE under Grant DE-FG02-93ER54222.

Platinum blue as an alternative to uranyl acetate for staining in transmission electron microscopy.

PubMed

Inaga, Sumire; Katsumoto, Tetsuo; Tanaka, Keiichi; Kameie, Toshio; Nakane, Hironobu; Naguro, Tomonori

2007-04-01

This paper introduces an aqueous solution of platinum blue (Pt-blue) as an alternative to uranyl acetate (UA) for staining in transmission electron microscopy (TEM). Pt-blue was prepared from a reaction of cis-dichlorodiamine-platinum (II) (cis-platin) with thymidine. When Pt-blue was dried on a microgrid and observed by TEM it showed a uniform appearance with tiny particles less than 1 nm in diameter. The effect of Pt-blue as an electron stain was then examined not only for positive staining of conventional ultrathin resin sections and counterstaining of post-embedding immuno-electron microscopy but also for negative staining. In ultrathin sections of the rat liver and renal glomerulus, Pt-blue provided good contrast images, especially in double staining combined with a lead stain (Pb). Almost all cell organelles were clearly observed with high contrast in these sections. Glycogen granules in the hepatic parenchymal cells were particularly electron dense in Pt-blue stained sections compared with those treated with UA. In longitudinal and transverse sections of budding influenza A viruses, a specific arrangement of rod-like structures, which correspond to the ribonucleoprotein complexes, was clearly shown in each virion stained with Pt-blue and Pb. When post-embedding immunoelectron microscopy was performed in ultrathin sections of HeLa cells embedded in Lowicryl K4M, the localization of Ki-67 protein was sufficiently detected even after Pt-blue and Pb staining. The present study also revealed that Pt-blue could be used for the negative staining of E. coli, allowing the visualization of a flagellum. These findings indicate that Pt-blue is a useful, safe, and easily obtainable electron stain that is an alternative to UA for TEM preparations.

Fractographic Investigation of Micromechanisms of Fracture in Alumina Ceramics

DTIC Science & Technology

1981-11-30

mechanisms flaw linking work of fracture electron channeling crack branching environmental effects 20. A07 ACT (Continue an reverse side Of necessary and...CLASSIFICATION OF THIS PAGE(I hm Date "ftn.,a environments using multiple techniques such as SEM, TEM, selected area electron channeling , and...94 Selected area electron channeling (SAEC) .. .... ........ 99 V. CONCLUSIONS. .. ............................ 100 VI. REFERENCES

Automated SEM and TEM sample preparation applied to copper/low k materials

NASA Astrophysics Data System (ADS)

Reyes, R.; Shaapur, F.; Griffiths, D.; Diebold, A. C.; Foran, B.; Raz, E.

2001-01-01

We describe the use of automated microcleaving for preparation of both SEM and TEM samples as done by SELA's new MC500 and TEMstation tools. The MC500 is an automated microcleaving tool that is capable of producing cleaves with 0.25 μm accuracy resulting in SEM-ready samples. The TEMstation is capable of taking a sample output from the MC500 (or from SELA's earlier MC200 tool) and producing a FIB ready slice of 25±5 μm, mounted on a TEM-washer and ready for FIB thinning to electron transparency for TEM analysis. The materials selected for the tool set evaluation mainly included the Cu/TaN/HOSP low-k system. The paper is divided into three sections, experimental approach, SEM preparation and analysis of HOSP low-k, and TEM preparation and analysis of Cu/TaN/HOSP low-k samples. For the samples discussed, data is presented to show the quality of preparation provided by these new automated tools.

Three dimensional profile measurement using multi-channel detector MVM-SEM

NASA Astrophysics Data System (ADS)

Yoshikawa, Makoto; Harada, Sumito; Ito, Keisuke; Murakawa, Tsutomu; Shida, Soichi; Matsumoto, Jun; Nakamura, Takayuki

2014-07-01

In next generation lithography (NGL) for the 1x nm node and beyond, the three dimensional (3D) shape measurements such as side wall angle (SWA) and height of feature on photomask become more critical for the process control. Until today, AFM (Atomic Force Microscope), X-SEM (cross-section Scanning Electron Microscope) and TEM (Transmission Electron Microscope) tools are normally used for 3D measurements, however, these techniques require time-consuming preparation and observation. And both X-SEM and TEM are destructive measurement techniques. This paper presents a technology for quick and non-destructive 3D shape analysis using multi-channel detector MVM-SEM (Multi Vision Metrology SEM), and also reports its accuracy and precision.

Crystal induced phosphorescence from Benz(a)anthracene microcrystals at room temperature

NASA Astrophysics Data System (ADS)

Maity, Samir; Mazumdar, Prativa; Shyamal, Milan; Sahoo, Gobinda Prasad; Misra, Ajay

2016-03-01

Pure organic compounds that are also phosphorescent at room temperature are very rare in literature. Here, we report efficient phosphorescence emission from aggregated hydrosol of Benz(a)anthracene (BaA) at room temperature. Aggregated hydrosol of BaA has been synthesized by re-precipitation method and SDS is used as morphology directing agent. Morphology of the particles is characterized using optical and scanning electronic microcopy (SEM). Photophysical properties of the aggregated hydrosol are carried out using UV-vis, steady state and time resolved fluorescence study. The large stoke shifted structured emission from aggregated hydrosol of BaA has been explained due to phosphorescence emission of BaA at room temperature. In the crystalline state, the restricted intermolecular motions (RIM) such as rotations and vibrations are activated by crystal lattice. This rigidification effect makes the chromophore phosphorescent at room temperature. The possible stacking arrangement of the neighboring BaA within the aggregates has been substantiated by computing second order Fukui parameter as local reactivity descriptors. Computational study also reveals that the neighboring BaA molecules are present in parallel slipped conformation in its aggregated crystalline form.

The quest for inorganic fullerenes

NASA Astrophysics Data System (ADS)

Pietsch, Susanne; Dollinger, Andreas; Strobel, Christoph H.; Park, Eun Ji; Ganteför, Gerd; Seo, Hyun Ook; Kim, Young Dok; Idrobo, Juan-Carlos; Pennycook, Stephen J.

2015-10-01

Experimental results of the search for inorganic fullerenes are presented. MonSm- and WnSm- clusters are generated with a pulsed arc cluster ion source equipped with an annealing stage. This is known to enhance fullerene formation in the case of carbon. Analogous to carbon, the mass spectra of the metal chalcogenide clusters produced in this way exhibit a bimodal structure. The species in the first maximum at low mass are known to be platelets. Here, the structure of the species in the second maximum is studied by anion photoelectron spectroscopy, scanning transmission electron microscopy, and scanning tunneling microcopy. All experimental results indicate a two-dimensional structure of these species and disagree with a three-dimensional fullerene-like geometry. A possible explanation for this preference of two-dimensional structures is the ability of a two-element material to saturate the dangling bonds at the edges of a platelet by excess atoms of one element. A platelet consisting of a single element only cannot do this. Accordingly, graphite and boron might be the only materials forming nano-spheres because they are the only single element materials assuming two-dimensional structures.

Field emission scanning electron microscopy (FE-SEM) as an approach for nanoparticle detection inside cells.

PubMed

Havrdova, M; Polakova, K; Skopalik, J; Vujtek, M; Mokdad, A; Homolkova, M; Tucek, J; Nebesarova, J; Zboril, R

2014-12-01

When developing new nanoparticles for bio-applications, it is important to fully characterize the nanoparticle's behavior in biological systems. The most common techniques employed for mapping nanoparticles inside cells include transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM). These techniques entail passing an electron beam through a thin specimen. STEM or TEM imaging is often used for the detection of nanoparticles inside cellular organelles. However, lengthy sample preparation is required (i.e., fixation, dehydration, drying, resin embedding, and cutting). In the present work, a new matrix (FTO glass) for biological samples was used and characterized by field emission scanning electron microscopy (FE-SEM) to generate images comparable to those obtained by TEM. Using FE-SEM, nanoparticle images were acquired inside endo/lysosomes without disruption of the cellular shape. Furthermore, the initial steps of nanoparticle incorporation into the cells were captured. In addition, the conductive FTO glass endowed the sample with high stability under the required accelerating voltage. Owing to these features of the sample, further analyses could be performed (material contrast and energy-dispersive X-ray spectroscopy (EDS)), which confirmed the presence of nanoparticles inside the cells. The results showed that FE-SEM can enable detailed characterization of nanoparticles in endosomes without the need for contrast staining or metal coating of the sample. Images showing the intracellular distribution of nanoparticles together with cellular morphology can give important information on the biocompatibility and demonstrate the potential of nanoparticle utilization in medicine. Copyright © 2014 Elsevier Ltd. All rights reserved.

Surface phenomenon in Electrochemical Systems

NASA Astrophysics Data System (ADS)

Gupta, Tanya

Interfaces play a critical role in the performance of electrochemical systems. This thesis focusses on interfaces in batteries and covers aspects of interfacial morphologies of metal anodes, including Silicon, Lithium and Zinc. Growth and cycling of electrochemically grown Lithium and Zinc metal structures is investigated. A new morphology of Zinc, called Hyper Dendritic Zinc is introduced. It is cycled against Prussian Blue Analogues and is shown to improve the performance of this couple significantly. Characterization of materials is done using various electron microscopy techniques ranging from Low Energy Electron Microscope (LEEM), to high energy Transmission Electron Microscope (TEM). LEEM is used for capturing subtle surface phenomenon occurring during epitaxial process of electrolyte on anode. The system studied is Silicon (100) during Chemical Vapor Deposition of Ethylene Carbonate. A strain driven relaxation theory is modeled to explain the unusual restructuring of Si substrate. The other extreme, TEM, is often used to study electrochemical processes, without clear understanding of how the high-energy electron beam can influence the sample under investigation. Here, we study the radiolysis in liquid cell TEM and emphasize on the enhancement of radiation dose at interfaces of the liquid due to generation of secondary and backscattered electrons from adjoining materials. It is shown that this effect is localized in a 10 nm region around the interface and can play a dominating role if there is an interface of liquid with heavy metals like Gold and Platinum which are frequently used as electrode materials. This analysis can be used to establish guidelines for experimentalists to follow, for accurate interpretation of their results.

In Situ Electron Microscopy of Lactomicroselenium Particles in Probiotic Bacteria.

PubMed

Nagy, Gabor; Pinczes, Gyula; Pinter, Gabor; Pocsi, Istvan; Prokisch, Jozsef; Banfalvi, Gaspar

2016-06-30

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.

Oral astringent stimuli alter the enamel pellicle's ultrastructure as revealed by electron microscopy.

PubMed

Rehage, Melanie; Delius, Judith; Hofmann, Thomas; Hannig, Matthias

2017-08-01

This electron microscopic study aimed at investigating effects of oral astringent stimuli on the enamel pellicle's morphology. Pellicles were formed in situ within 30min on bovine enamel slabs, fixed to individuals' upper jaw splints. The pellicle-coated specimens were immersed in vitro in seven diverse astringent solutions and subsequently analyzed by scanning electron microscopy (SEM), energy dispersive X-ray (EDX) spectroscopy, as well as transmission electron microscopy (TEM). Four biocompatible astringents, namely the polyphenol epigallocatechin gallate, the metal salt iron(III) sulfate, the basic protein lysozyme, and the aminopolysaccharide chitosan, were additionally applied in situ. After rinsing the oral cavity with these compounds, the pellicle's ultrastructure was imaged by SEM and TEM, respectively. Untreated pellicle samples served as controls. Exposure to polyphenols and lysozyme induced particularly thicker and electron-denser pellicles in comparison to the control pellicle with similar characteristics in vitro and in situ. In contrast, acidic chitosan and metal salt solutions, respectively, revealed minor pellicle alterations. The incorporation of Fe and Al into the pellicles treated with the corresponding inorganic salts was verified by EDX analysis. Astringent-induced pellicle modifications were for the first time visualized by TEM. The ultrastructural alterations of the dental pellicle may partly explain the tooth-roughening effect caused by oral astringent stimuli. Astringents might modify the pellicle's protective properties against dental erosion, attrition, as well as bacterial adhesion, and by this means may influence tooth health. The findings may thus be particularly relevant for preventive dentistry. Copyright © 2017 Elsevier Ltd. All rights reserved.

Preparation of viral samples within biocontainment for ultrastructural analysis: Utilization of an innovative processing capsule for negative staining.

PubMed

Monninger, Mitchell K; Nguessan, Chrystal A; Blancett, Candace D; Kuehl, Kathleen A; Rossi, Cynthia A; Olschner, Scott P; Williams, Priscilla L; Goodman, Steven L; Sun, Mei G

2016-12-01

Transmission electron microscopy can be used to observe the ultrastructure of viruses and other microbial pathogens with nanometer resolution. In a transmission electron microscope (TEM), the image is created by passing an electron beam through a specimen with contrast generated by electron scattering from dense elements in the specimen. Viruses do not normally contain dense elements, so a negative stain that places dense heavy metal salts around the sample is added to create a dark border. To prepare a virus sample for a negative stain transmission electron microscopy, a virus suspension is applied to a TEM grid specimen support, which is a 3mm diameter fragile specimen screen coated with a few nanometers of plastic film. Then, deionized (dI) water rinses and a negative stain solution are applied to the grid. All infectious viruses must be handled in a biosafety cabinet (BSC) and many require a biocontainment laboratory environment. Staining viruses in biosafety levels (BSL) 3 and 4 is especially challenging because the support grids are small, fragile, and easily moved by air currents. In this study we evaluated a new device for negative staining viruses called mPrep/g capsule. It is a capsule that holds up to two TEM grids during all processing steps and for storage after staining is complete. This study reports that the mPrep/g capsule method is valid and effective to negative stain virus specimens, especially in high containment laboratory environments. Copyright © 2016 The Authors. Published by Elsevier B.V. All rights reserved.

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

PubMed

Wang, Yibing; Chen, Xin; Cao, Hongliang; Deng, Chao; Cao, Xiaodan; Wang, Ping

2015-01-01

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

The Morphology of Silver Layers on SU8 polymers prepared by Electroless Deposition

NASA Astrophysics Data System (ADS)

Dutta, Aniruddha; Yuan, Biao; Heinrich, Helge; Grabill, Chris; Williams, Henry; Kuebler, Stephen; Bhattacharya, Aniket

2010-03-01

Silver was deposited onto the functionalized surface of polymeric SU-8 where gold nanoparticles (Au-NPs) act as nucleation sites using electroless metallization chemistry. Here we report on the evolution of the nanoscale morphology of deposited Ag studied by Transmission Electron Microscopy (TEM). In TEM of sample cross sections correlations between the original gold and the silver nanoparticles were obtained while plan-view TEM results showed the distribution of nanoparticles on the surface. Scanning TEM with a high-angle annular dark field detector was used to obtain atomic number contrast. The morphology of the deposited Ag was controlled through the presence and absence of gum Arabic. The thickness and height fluctuations of the Ag layer were determined as a function of time and a statistical analysis of the growth process was conducted for the initial deposition periods.

Microcellular nanocomposite injection molding process

Treesearch

Mingjun Yuan; Lih-Sheng Turng; Rick Spindler; Daniel Caulfield; Chris Hunt

2003-01-01

This study aims to explore the processing benefits and property improvements of combining nanocomposites with microcellular injection molding. The molded parts produced based on the Design of Experiments (DOE) matrices were subjected to tensile testing, impact testing, and Scanning Electron Microscope (SEM), Transmission Electron Microscope (TEM), Dynamic Mechanical...

Templated synthesis of nanoporous titania/nanocarbon composites

NASA Astrophysics Data System (ADS)

Mistry, Jayur

Hexagonally patterned (honeycomb structured) nano-porous titania finds distinct applications in the field of material science, electronics, and catalysis. The preparation of titania/nanocarbon composites was carried out using titanium iso-propoxide precursor and a viscous surfactant templated system arranged into nanoscopic channels of water and iso-octane. Nanocarbon was introduced into the titania pores, as it was dispersed into the water (used to increase the W0), while making templets. Prepared titania/nanocarbon composites were analyzed under scanning electron microscopy (SEM), transmission electron microscope (TEM), and X-ray diffraction (XRD) after a specific heat treatment. SEM and TEM allows us to see the morphology of the hexagonally patterned templates and XRD shows the change in the crystallinity of the titania after the heat treatment. Further tests are run with the Solartron™ CellTest potentiostat syste, which, allows us to study the electrical properties of the nanocomposites. The composites synthesized have wide applications in number of fields, including energy, sensors and electronics.

Observation of trapped-electron-mode microturbulence in reversed field pinch plasmas

NASA Astrophysics Data System (ADS)

Duff, J. R.; Williams, Z. R.; Brower, D. L.; Chapman, B. E.; Ding, W. X.; Pueschel, M. J.; Sarff, J. S.; Terry, P. W.

2018-01-01

Density fluctuations in the large-density-gradient region of improved confinement Madison Symmetric Torus reversed field pinch (RFP) plasmas exhibit multiple features that are characteristic of the trapped-electron mode (TEM). Core transport in conventional RFP plasmas is governed by magnetic stochasticity stemming from multiple long-wavelength tearing modes. Using inductive current profile control, these tearing modes are reduced, and global confinement is increased to that expected for comparable tokamak plasmas. Under these conditions, new short-wavelength fluctuations distinct from global tearing modes appear in the spectrum at a frequency of f ˜ 50 kHz, which have normalized perpendicular wavenumbers k⊥ρs≲ 0.2 and propagate in the electron diamagnetic drift direction. They exhibit a critical-gradient threshold, and the fluctuation amplitude increases with the local electron density gradient. These characteristics are consistent with predictions from gyrokinetic analysis using the Gene code, including increased TEM turbulence and transport from the interaction of remnant tearing magnetic fluctuations and zonal flow.

Distinct turbulence sources and confinement features in the spherical tokamak plasma regime

DOE PAGES

Wang, W. X.; Ethier, S.; Ren, Y.; ...

2015-10-30

New turbulence contributions to plasma transport and confinement in the spherical tokamak (ST) regime are identified through nonlinear gyrokinetic simulations. The drift wave Kelvin-Helmholtz (KH) mode characterized by intrinsic mode asymmetry is shown to drive significant ion thermal transport in strongly rotating national spherical torus experiment (NSTX) L-modes. The long wavelength, quasi-coherent dissipative trapped electron mode (TEM) is destabilized in NSTX H-modes despite the presence of strong E x B shear, providing a robust turbulence source dominant over collisionless TEM. Dissipative trapped electron mode (DTEM)-driven transport in the NSTX parametric regime is shown to increase with electron collision frequency, offeringmore » one possible source for the confinement scaling observed in experiments. There exists a turbulence-free regime in the collision-induced collisionless trapped electron mode to DTEM transition for ST plasmas. In conclusion, this predicts a natural access to a minimum transport state in the low collisionality regime that future advanced STs may cover.« less

Manning the Army in 1990.

DTIC Science & Technology

1982-06-01

IIIIIIIIIIIIIl IIIIIIIII IIIIIIIluuumIIIII IIIIIIIIII 111 .0-0i MICROCOPY RESOLUTION TEST CHART NATION4AL BUREAU OF STANOARD$- 1963 - .°~ 2 NAVAL POSTGRADUATE...be encountered in attaining a sufficient number who can qualify in AFQT test categories I-111A. Accession For NTIS GRA&I DTIC- TAB U’nnnnounced El J...AFQT test categories I-IIIA 𔃾 TABLE OF ZONTENTS Io INTRODUCTION ................... 11 II. MANPOWER REQUI REMENT S .. .. . .. .. .. . .. 15 A

Simultaneous Estimation of Regression Functions for Marine Corps Technical Training Specialties.

DTIC Science & Technology

1985-01-03

Edmonton, Alberta CANADA 1 Dr. Frederic M. Lord Educational Testing Service 1 Dr. Earl Hunt Princeton, NJ 08541 Dept, of Psychology University of...111111-1.6 MICROCOPY RESOLUTION TEST CHART NATIONAL BUREAU OF STANDARDS-1963-A SIMIULTANEOUS ESTIMATION OF REGRESSION FUNCTIONS FOR MARINE CORPS...Bayesian techniques for simul- taneous estimation to the specification of regression weights for selection tests used in various technical training courses

Microcomputer Control of a Hydraulically Actuated Piston.

DTIC Science & Technology

1987-06-01

EhhhohEohEmhhE EhhmhhhohhhhhI M1l *2 112.2 Ll 6 111111.258 MICROCOPY RESOLUfION TEST CHART NATIONAL BUREAUJ nF SIANDARDS 1963 A W* %i r f U V ~ S i V...SYSTE.M............................I( E. I REQUENCY RESPONSE TEST ........................... F. MODEL V.ALIDATION ................................. 2...O RITH M (BA SIC) ................................. 43 APPENDIX D: DIGITAL SYSTEM SIMULATION CODE (DSL) ........... 44 APPENDIX E: DIGITAL LOGIC TEST

Correlative fluorescence microscopy and scanning transmission electron microscopy of quantum-dot-labeled proteins in whole cells in liquid.

PubMed

Dukes, Madeline J; Peckys, Diana B; de Jonge, Niels

2010-07-27

Correlative fluorescence microscopy and transmission electron microscopy (TEM) is a state-of-the-art microscopy methodology to study cellular function, combining the functionality of light microscopy with the high resolution of electron microscopy. However, this technique involves complex sample preparation procedures due to its need for either thin sections or frozen samples for TEM imaging. Here, we introduce a novel correlative approach capable of imaging whole eukaryotic cells in liquid with fluorescence microscopy and with scanning transmission electron microscopy (STEM); there is no additional sample preparation necessary for the electron microscopy. Quantum dots (QDs) were bound to epidermal growth factor (EGF) receptors of COS7 fibroblast cells. Fixed whole cells in saline water were imaged with fluorescence microscopy and subsequently with STEM. The STEM images were correlated with fluorescence images of the same cellular regions. QDs of dimensions 7x12 nm were visible in a 5 microm thick layer of saline water, consistent with calculations. A spatial resolution of 3 nm was achieved on the QDs.

Correlative Fluorescence Microscopy and Scanning Transmission Electron Microscopy of Quantum Dot Labeled Proteins in Whole Cells in Liquid

PubMed Central

Dukes, Madeline J.; Peckys, Diana B.; de Jonge, Niels

2010-01-01

Correlative fluorescence microscopy and transmission electron microscopy (TEM) is a state-of-the-art microscopy methodology to study cellular function, combining the functionality of light microscopy with the high resolution of electron microscopy. However, this technique involves complex sample preparation procedures due to its need for either thin sections or frozen samples for TEM imaging. Here, we introduce a novel correlative approach capable of imaging whole eukaryotic cells in liquid with fluorescence microscopy and with scanning transmission electron microscopy (STEM); there is no additional sample preparation necessary for the electron microscopy. Quantum dots (QDs) were bound to epidermal growth factor (EGF) receptors of COS7 fibroblast cells. Fixed whole cells in saline water were imaged with fluorescence microscopy and subsequently with STEM. The STEM images were correlated with fluorescence images of the same cellular regions. QDs of dimensions 7 × 12 nm were visible in a 5 μm thick layer of saline water, consistent with calculations. A spatial resolution of 3 nm was achieved on the QDs. PMID:20550177

A literature review of in situ transmission electron microscopy technique in corrosion studies.

PubMed

Song, Zhengwei; Xie, Zhi-Hui

2018-06-18

One of the biggest challenges in corrosion investigation is foreseeing precisely how and where materials will degenerate in a designated condition owing to scarceness of accurate corrosion mechanisms. Recent fast development of in situ transmission electron microscopy (TEM) technique makes it achievable to better understand the corrosion mechanism and physicochemical processes at the interfaces between samples and gases or electrolytes by dynamical capture the microstructural and chemical changes with high resolution within a realistic or near-realistic environment. However, a detailed and in-depth account summing up the development and latest achievements of in situ TEM techniques, especially the application of emerging liquid and electrochemical cells in the community of corrosion study in the last several years is lacking and is urgently needed for its heathy development. To fill this gap, this critical review summarizes firstly the key scientific issues in corrosion research, followed by introducing the configurations of several typical closed-type cells. Then, the achievements of in situ TEM using open-type or closed-type cells in corrosion study are presented in detail. The study directions in the future are commented finally in terms of spatial and temporal resolution, electron radiation, and linkage between microstructure and electrochemical performance in corrosion community. Copyright © 2018 Elsevier Ltd. All rights reserved.

Assessment of microcrystal quality by transmission electron microscopy for efficient serial femtosecond crystallography.

PubMed

Barnes, Christopher O; Kovaleva, Elena G; Fu, Xiaofeng; Stevenson, Hilary P; Brewster, Aaron S; DePonte, Daniel P; Baxter, Elizabeth L; Cohen, Aina E; Calero, Guillermo

2016-07-15

Serial femtosecond crystallography (SFX) employing high-intensity X-ray free-electron laser (XFEL) sources has enabled structural studies on microcrystalline protein samples at non-cryogenic temperatures. However, the identification and optimization of conditions that produce well diffracting microcrystals remains an experimental challenge. Here, we report parallel SFX and transmission electron microscopy (TEM) experiments using fragmented microcrystals of wild type (WT) homoprotocatechuate 2,3-dioxygenase (HPCD) and an active site variant (H200Q). Despite identical crystallization conditions and morphology, as well as similar crystal size and density, the indexing efficiency of the diffraction data collected using the H200Q variant sample was over 7-fold higher compared to the diffraction results obtained using the WT sample. TEM analysis revealed an abundance of protein aggregates, crystal conglomerates and a smaller population of highly ordered lattices in the WT sample as compared to the H200Q variant sample. While not reported herein, the 1.75 Å resolution structure of the H200Q variant was determined from ∼16 min of beam time, demonstrating the utility of TEM analysis in evaluating sample monodispersity and lattice quality, parameters critical to the efficiency of SFX experiments. Copyright © 2016 Elsevier Inc. All rights reserved.

Magnetic resonance investigation of magnetic-labeled baker's yeast cells

NASA Astrophysics Data System (ADS)

Godoy Morais, J. P. M.; Azevedo, R. B.; Silva, L. P.; Lacava, Z. G. M.; Báo, S. N.; Silva, O.; Pelegrini, F.; Gansau, C.; Buske, N.; Safarik, I.; Safarikova, M.; Morais, P. C.

2004-05-01

In this study, the interaction of DMSA-coated magnetite nanoparticles (5 and 10 nm core-size) with Saccharomyces cerevisae was investigated using magnetic resonance (MR) and transmission electron microscopy (TEM). The TEM micrographs revealed magnetite nanoparticles attached externally to the cell wall. The MR data support the strong interaction among the nanoparticles supported by the cells. A remarkable shift in the resonance field was used as signature of particle attachment to the cell wall.

Physics of Radiation Exposure and Characterization for Future Electronic Materials

DTIC Science & Technology

2014-12-01

TEM probe. These visits have included an invited talk at the Annual User’s Meeting at BNL in which the DTRA project was highlighted. • Columbia...at PNNL. • Columbia graduate student Luozhou Li was trained by BNL researchers Dr. Ming Lu on nanofabrication techniques related to the fabrication...Jacob Mower were trained by BNL researcher Kim Kisslinger on diamond membrane fabrication and TEM cross-section sample fabrication. • Columbia

In Vitro Toxicity of Silver Nanoparticles in Human Lung Epithelial Cells

DTIC Science & Technology

2009-03-01

software from the particle distributions measured and the polydispersity index (PdI) given is a measure of the size ranges present in the solution...Transmission Electron Microscopy Figure 22 shows the TEM primary particles size and distribution determined from measurement of over 100 particles from...nm uncoated. (B) Ag 80 nm uncoated. (C) Ag 10 nm coated. (D) Ag 80 nm coated Table 4 shows the TEM primary particles size and distribution

In situ sputter cleaning of thin film metal substrates for UHV-TEM corrosion studies.

NASA Technical Reports Server (NTRS)

Heinemann, K.; Poppa, H.

1973-01-01

A prerequisite for conducting valid corrosion experiments by in situ electron microscopy techniques is not only the achievement of UHV background pressure conditions at the site of the specimen but also the ability to clean the surface of the thin metal substrate specimen before initiation of the corrosive interaction. A miniaturized simple ion gun has been constructed for this purpose. The gun is small enough to be incorporated into an UHV electron microscope specimen chamber with hot stage in such a way as to permit bombardment of the substrate specimen while observing it by transmission electron microscopy TEM. It is shown that the ion beam generated is confined well enough to cause a sputtering removal of substrate material at a rate of approximately 5-10 A/min and to prevent the sputter deposition of contaminating material from the specimen holder.

Pd-Ni-MWCNT nanocomposite thin films: preparation and structure

NASA Astrophysics Data System (ADS)

Kozłowski, Mirosław; Czerwosz, ElŻbieta; Sobczak, Kamil

2017-08-01

The properties of nanocomposite palladium-nickel-multi-walled (Pd-Ni-MWCNT) films deposited on aluminum oxide (Al2O3) substrate have been prepared and investigated. These films were obtained by 3 step process consisted of PVD/CVD/PVD methods. The morphology and structure of the obtained films were characterized by Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM) techniques at various stages of the film formation. EDX spectrometer was used to measurements of elements segregation in the obtained film. TEM and STEM (Scanning Transmission Electron Microscopy) observations showed MWCNTs decorated with palladium nanoparticles in the film obtained in the last step of film formation (final PVD process). The average size of the palladium nanoparticles observed both on MWCNTs and carbonaceous matrix does not exceed 5 nm. The research was conducted on the use of the obtained films as potential sensors of gases (e.g. H2, NH3, CO2) and bio-sensors or optical sensors.

Scanning and transmission electron microscopic observation of the parasitic form of Trichophyton violaceum in the infected hair from tinea capitis.

PubMed

Zhuang, Kaiwen; Ran, Xin; Lei, Song; Zhang, Chaoliang; Lama, Jebina; Ran, Yuping

2014-01-01

Trichophyton violaceum is a pathogen of tinea capitis and usually cause infection of scalp and hair in children. To investigate the parasitic form of T. violaceum in the human hair tissue, the infected hair strands were collected from a 9-year-old boy with tinea capitis due to T. violaceum and observed under both the scanning electron microscope (SEM) and transmission electron microscope (TEM). The SEM and TEM findings revealed that T. violaceum parasitically lives in the hair shaft in various forms and the morphological transformation of the fungus from hyphae into arthrospores was noted. The involved hair shaft was damaged to the great extent and its ultrastructural changes were evident. Those morphological characteristics of T. violaceum and the three-dimensional ultastructure changes of infected hairs give a better knowledge about the host-fungus relationship in tinea capitis. © 2014 Wiley Periodicals, Inc.

Improving the Mechanical Performance and Thermal Stability of a PVA-Clay Nanocomposite by Electron Beam Irradiation

NASA Astrophysics Data System (ADS)

Shokuhi Rad, A.; Ebrahimi, D.

2017-07-01

The effects of electron beam irradiation and presence of clay on the mechanical properties and thermal stability of montmorillonite clay-modified polyvinyl alcohol nanocomposites were studied. By using the X-ray diffraction (XRD) and transmission electron microscopy (TEM), the microstructure of the nanocomposites was investigated. The results obtained from TEM and XRD tests showed that montmorillonite clay nanoparticles were located in the polyvinyl alcohol phase. The XRD analysis confirmed the formation of an exfoliated structure in nanocomposites samples. Increasing the amount of clay to 20 wt.% increased the tensile strength and modulus of the nanocomposite. Irradiation up to an absorbed dose of 100 kGy increased its mechanical properties and thermal stability, but at higher irradiation levels, the mechanical strength and thermal stability declined. The sample with 20 wt.% of the nanofiller, exposed to 100 kGy, showed the highest mechanical strength and thermal stability.

Scanning electron microscope cathodoluminescence imaging of subgrain boundaries, twins and planar deformation features in quartz

NASA Astrophysics Data System (ADS)

Hamers, M. F.; Pennock, G. M.; Drury, M. R.

2017-04-01

The study of deformation features has been of great importance to determine deformation mechanisms in quartz. Relevant microstructures in both growth and deformation processes include dislocations, subgrains, subgrain boundaries, Brazil and Dauphiné twins and planar deformation features (PDFs). Dislocations and twin boundaries are most commonly imaged using a transmission electron microscope (TEM), because these cannot directly be observed using light microscopy, in contrast to PDFs. Here, we show that red-filtered cathodoluminescence imaging in a scanning electron microscope (SEM) is a useful method to visualise subgrain boundaries, Brazil and Dauphiné twin boundaries. Because standard petrographic thin sections can be studied in the SEM, the observed structures can be directly and easily correlated to light microscopy studies. In contrast to TEM preparation methods, SEM techniques are non-destructive to the area of interest on a petrographic thin section.

Fine Structure in Multi-Phase Zr8Ni21-Zr7Ni10-Zr2Ni7 Alloy Revealed by Transmission Electron Microscope

PubMed Central

Shen, Haoting; Bendersky, Leonid A.; Young, Kwo; Nei, Jean

2015-01-01

The microstructure of an annealed alloy with a Zr8Ni21 composition was studied by both scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The presence of three phases, Zr8Ni21, Zr2Ni7, and Zr7Ni10, was confirmed by SEM/X-ray energy dispersive spectroscopy compositional mapping and TEM electron diffraction. Distribution of the phases and their morphology can be linked to a multi-phase structure formed by a sequence of reactions: (1) L → Zr2Ni7 + L’; (2) peritectic Zr2Ni7 + L’ → Zr2Ni7 + Zr8Ni21 + L”; (3) eutectic L” → Zr8Ni21 + Zr7Ni10. The effect of annealing at 960 °C, which was intended to convert a cast structure into a single-phase Zr8Ni21 structure, was only moderate and the resulting alloy was still multi-phased. TEM and crystallographic analysis of the Zr2Ni7 phase show a high density of planar (001) defects that were explained as low-energy boundaries between rotational variants and stacking faults. The crystallographic features arise from the pseudo-hexagonal structure of Zr2Ni7. This highly defective Zr2Ni7 phase was identified as the source of the broad X-ray diffraction peaks at around 38.4° and 44.6° when a Cu-K was used as the radiation source. PMID:28793460

Quantitative Cryo-Scanning Transmission Electron Microscopy of Biological Materials.

PubMed

Elbaum, Michael

2018-05-11

Electron tomography provides a detailed view into the 3D structure of biological cells and tissues. Physical fixation by vitrification of the aqueous medium provides the most faithful preservation of biological specimens in the native, fully hydrated state. Cryo-microscopy is challenging, however, because of the sensitivity to electron irradiation and due to the weak electron scattering of organic material. Tomography is even more challenging because of the dependence on multiple exposures of the same area. Tomographic imaging is typically performed in wide-field transmission electron microscopy (TEM) mode with phase contrast generated by defocus. Scanning transmission electron microscopy (STEM) is an alternative mode based on detection of scattering from a focused probe beam, without imaging optics following the specimen. While careful configuration of the illumination and detectors is required to generate useful contrast, STEM circumvents the major restrictions of phase contrast TEM to very thin specimens and provides a signal that is more simply interpreted in terms of local composition and density. STEM has gained popularity in recent years for materials science. The extension of STEM to cryomicroscopy and tomography of cells and macromolecules is summarized herein. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Precipitation in Ni-Si during electron and ion irradiation

NASA Astrophysics Data System (ADS)

Lucas, G. E.; Zama, T.; Ishino, S.

1986-11-01

This study was undertaken to further investigate how the nature of the irradiation condition affects precipitation in a dilute Ni-Si system. Transmission electron microscopy (TEM) discs of a solution annealed Ni alloy containing 5 at% Si were irradiated with 400 keV Ar + ions, 200 keV He + ions and 1 MeV electrons at average displacement rates in the range 2 × 10 -5dpa/s to 2 × 10 -3dpa/s at temperatures in the range 25°C to 450°C. Samples irradiated with electrons were observed in situ in an HVEM, while ion irradiated specimens were examined in a TEM after irradiation. Precipitation of Ni 3Si was detected by the appearance of superlattice spots in the electron diffraction patterns. It was found that as the mass of the irradiating species increased, the lower bound temperature at which Ni 3Si precipitation was first observed increased. For electron irradiation, the lower bound temperature at 2 × 10 -3dpa/s was ˜125°C, whereas for 400 keV Ar + irradiation at a similar average displacement rate the lower boundary was approximately 325°C. This suggests that cascade disordering competes with radiation induced solute segregation.

Distinct Particle Morphologies Revealed through Comparative Parallel Analyses of Retrovirus-Like Particles.

PubMed

Martin, Jessica L; Cao, Sheng; Maldonado, Jose O; Zhang, Wei; Mansky, Louis M

2016-09-15

The Gag protein is the main retroviral structural protein, and its expression alone is usually sufficient for production of virus-like particles (VLPs). In this study, we sought to investigate-in parallel comparative analyses-Gag cellular distribution, VLP size, and basic morphological features using Gag expression constructs (Gag or Gag-YFP, where YFP is yellow fluorescent protein) created from all representative retroviral genera: Alpharetrovirus, Betaretrovirus, Deltaretrovirus, Epsilonretrovirus, Gammaretrovirus, Lentivirus, and Spumavirus. We analyzed Gag cellular distribution by confocal microscopy, VLP budding by thin-section transmission electron microscopy (TEM), and general morphological features of the VLPs by cryogenic transmission electron microscopy (cryo-TEM). Punctate Gag was observed near the plasma membrane for all Gag constructs tested except for the representative Beta- and Epsilonretrovirus Gag proteins. This is the first report of Epsilonretrovirus Gag localizing to the nucleus of HeLa cells. While VLPs were not produced by the representative Beta- and Epsilonretrovirus Gag proteins, the other Gag proteins produced VLPs as confirmed by TEM, and morphological differences were observed by cryo-TEM. In particular, we observed Deltaretrovirus-like particles with flat regions of electron density that did not follow viral membrane curvature, Lentivirus-like particles with a narrow range and consistent electron density, suggesting a tightly packed Gag lattice, and Spumavirus-like particles with large envelope protein spikes and no visible electron density associated with a Gag lattice. Taken together, these parallel comparative analyses demonstrate for the first time the distinct morphological features that exist among retrovirus-like particles. Investigation of these differences will provide greater insights into the retroviral assembly pathway. Comparative analysis among retroviruses has been critically important in enhancing our understanding of retroviral replication and pathogenesis, including that of important human pathogens such as human T-cell leukemia virus type 1 (HTLV-1) and HIV-1. In this study, parallel comparative analyses have been used to study Gag expression and virus-like particle morphology among representative retroviruses in the known retroviral genera. Distinct differences were observed, which enhances current knowledge of the retroviral assembly pathway. Copyright © 2016, American Society for Microbiology. All Rights Reserved.

Effect of interparticle interactions on size determination of zirconia and silica based systems – A comparison of SAXS, DLS, BET, XRD and TEM

PubMed Central

Pabisch, Silvia; Feichtenschlager, Bernhard; Kickelbick, Guido; Peterlik, Herwig

2012-01-01

The aim of this work is a systematic comparison of size characterisation methods for two completely different model systems of oxide nanoparticles, i.e. amorphous spherical silica and anisotropic facet-shaped crystalline zirconia. Size and/or size distribution were determined in a wide range from 5 to 70 nm using small-angle X-ray scattering (SAXS), dynamic light scattering (DLS), nitrogen sorption (BET), X-ray diffraction (XRD) and transmission electron microscopy (TEM). A nearly perfect coincidence was observed only for SAXS and TEM for both types of particles. For zirconia nanoparticles considerable differences between different measurement methods were observed. PMID:22347721

Microstructure, strengthening mechanisms and hot deformation behavior of an oxide-dispersion strengthened UFG Al6063 alloy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Asgharzadeh, H.; Kim, H.S.; Simchi, A., E-mail: simchi@sharif.edu

2013-01-15

An ultrafine-grained Al6063/Al{sub 2}O{sub 3} (0.8 vol.%, 25 nm) nanocomposite was prepared via powder metallurgy route through reactive mechanical alloying and hot powder extrusion. Scanning electron microcopy, transmission electron microscopy, and back scattered electron diffraction analysis showed that the grain structure of the nanocomposite is trimodal and composed of nano-size grains (< 0.1 {mu}m), ultrafine grains (0.1-1 {mu}m), and micron-size grains (> 1 {mu}m) with random orientations. Evaluation of the mechanical properties of the nanocomposite based on the strengthening-mechanism models revealed that the yield strength of the ultrafine-grained nanocomposite is mainly controlled by the high-angle grain boundaries rather than nanometricmore » alumina particles. Hot deformation behavior of the material at different temperatures and strain rates was studied by compression test and compared to coarse-grained Al6063 alloy. The activation energy of the hot deformation process for the nanocomposite was determined to be 291 kJ mol{sup -1}, which is about 64% higher than that of the coarse-grained alloy. Detailed microstructural analysis revealed that dynamic recrystallization is responsible for the observed deformation softening in the ultrafine-grained nanocomposite. - Highlights: Black-Right-Pointing-Pointer The strengthening mechanisms of Al6063/Al{sub 2}O{sub 3} nanocomposite were evaluated. Black-Right-Pointing-Pointer Hot deformation behavior of the nanocomposite was studied. Black-Right-Pointing-Pointer The hot deformation activation energy was determined using consecutive models. Black-Right-Pointing-Pointer The restoration mechanisms and microstructural changes are presented.« less

Early detection of Candida albicans biofilms at porous electrodes.

PubMed

Congdon, Robert B; Feldberg, Alexander S; Ben-Yakar, Natalie; McGee, Dennis; Ober, Christopher; Sammakia, Bahgat; Sadik, Omowunmi A

2013-02-15

We describe the development of an electrochemical sensor for early detection of biofilm using Candida albicans. The electrochemical sensor used the ability of biofilms to accept electrons from redox mediators relative to the number of metabolically active cells present. Cyclic voltammetry and differential pulse voltammetry techniques were used to monitor the redox reaction of K(3)Fe(CN)(6) at porous reticulated vitreous carbon (RVC) (238.7 cm(2)) working electrodes versus Ag/AgCl reference. A shift in the peak potential occurred after 12 h of film growth, which is attributed to the presence of C. albicans. Moreover, the intensity of the ferricyanide reduction peak first increased as C. albicans deposited onto the porous electrodes at various growth times. The peak current subsequently decreased at extended periods of growth of 48 h. The reduction in peak current was attributed to the biofilm reaching its maximum growth thickness, which correlated with the maximum number of metabolically active cells. The observed diffusion coefficients for the bare RVC and biofilm-coated electrodes were 2.2 × 10(-3) and 7.0 × 10(-6) cm(2)/s, respectively. The increase in diffusivity from the bare electrode to the biofilm-coated electrode indicated some enhancement of electron transfer mediated by the biofilm to the porous electrode. Verification of the growth of biofilm was achieved using scanning electron microcopy and laser scanning confocal imaging microscopy. Validation with conventional plating techniques confirmed that the correlation (R(2) = 0.9392) could be achieved between the electrochemical sensors data and colony-forming units. Copyright © 2012 Elsevier Inc. All rights reserved.

High-Resolution Characterization of UMo Alloy Microstructure

DOE Office of Scientific and Technical Information (OSTI.GOV)

Devaraj, Arun; Kovarik, Libor; Joshi, Vineet V.

2016-11-30

This report highlights the capabilities and procedure for high-resolution characterization of UMo fuels in PNNL. Uranium-molybdenum (UMo) fuel processing steps, from casting to forming final fuel, directly affect the microstructure of the fuel, which in turn dictates the in-reactor performance of the fuel under irradiation. In order to understand the influence of processing on UMo microstructure, microstructure characterization techniques are necessary. Higher-resolution characterization techniques like transmission electron microscopy (TEM) and atom probe tomography (APT) are needed to interrogate the details of the microstructure. The findings from TEM and APT are also directly beneficial for developing predictive multiscale modeling tools thatmore » can predict the microstructure as a function of process parameters. This report provides background on focused-ion-beam–based TEM and APT sample preparation, TEM and APT analysis procedures, and the unique information achievable through such advanced characterization capabilities for UMo fuels, from a fuel fabrication capability viewpoint.« less

Microstructural Characterization of Aluminum-Lithium Alloys 1460 and 2195

NASA Technical Reports Server (NTRS)

Wang, Z. M.; Shenoy, R. N.

1998-01-01

Transmission electron microscopy (TEM) and differential scanning calorimetry (DSC) techniques were employed to characterize the precipitate distributions in lithium-containing aluminum alloys 1460 and 2195 in the T8 condition. TEM examinations revealed delta prime and T1 as the primary strengthening precipitates in alloys 1460 and 2195 respectively. TEM results showed a close similarity of the Russian alloy 1460 to the U.S. alloy 2090, which has a similar composition and heat treatment schedule. DSC analyses also indicate a comparable delta prime volume fraction. TEM study of a fractured tensile sample of alloy 1460 showed that delta prime precipitates are sheared by dislocations during plastic deformation and that intense stress fields arise at grain boundaries due to planar slip. Differences in fracture toughness of alloys 1460 and 2195 are rationalized on the basis of a literature review and observations from the present study.

TEM Systems Design: Using Full Maxwell FDTD Modelling to Study the Transient Response of Custom-madeTx and Rx Coils.

NASA Astrophysics Data System (ADS)

Chevalier, A.; Rejiba, F.; Schamper, C.; Thiesson, J.; Hovhannissian, G.

2016-12-01

From airborne applications to field scale measurements of Transient Electromagnetic Methods(TEM), an accurate knowledge of the sensitivity of the inductive coil sensors (system response) is aprerequisite to interpret the measured transient magnetic flux density into a subsurface distributionof conductivity. The system response is a term that refers to the cumulative effect of inductive andcapacitive couplings (cross-talks) between each component constituting a TEM apparatus and thenearby conductive structures. As a result, the frequency sensitivity of the voltage coil sensor (Rx)along with the emitted current waveform in the current emitting coil (Tx) are controlled by thegeometry and electronic characteristic of the set-up as well as the near surface electromagneticproperties. During the early development of an innovative airborne TEM solutions (French nationalTEMas project), determining the coil geometries and the impedance matching between all parts ofthe transmission link (electronic parts and coils) for various environmental set-ups, has been a majorissue. In this study, we review the required theoretical framework and propose a versatile numericalmethodology to ease the coil design and impedance matching process while extending ourunderstanding of short-time transient that operates from DC to moderately high frequencies (0 to 20Mhz). We used a full Maxwell equations FDTD model along with a semi-analytical 1D modeler to infercoils emitting and receiving properties, for various coil geometries and site-dependent conditions.Results highlight the influence of the environment on the emitting and sensing properties. Theincreasing effects of cross-talks between the Tx and the Rx coils depending on their size is shown.Strategies regarding the impedance adaptation between the electronical components and the coilsensors are then discussed for different geophysical specifications.

Nanorods, nanospheres, nanocubes: Synthesis, characterization and catalytic activity of nanoferrites of Mn, Co, Ni, Part-89

DOE Office of Scientific and Technical Information (OSTI.GOV)

Singh, Supriya; Srivastava, Pratibha; Singh, Gurdip, E-mail: gsingh4us@yahoo.com

2013-02-15

Graphical abstract: Prepared nanoferrites were characterized by FE-SEM and bright field TEM micrographs. The catalytic effect of these nanoferrites was evaluated on the thermal decomposition of ammonium perchlorate using TG and TG–DSC techniques. The kinetics of thermal decomposition of AP was evaluated using isothermal TG data by model fitting as well as isoconversional method. Display Omitted Highlights: ► Synthesis of ferrite nanostructures (∼20.0 nm) by wet-chemical method under different synthetic conditions. ► Characterization using XRD, FE-SEM, EDS, TEM, HRTEM and SAED pattern. ► Catalytic activity of ferrite nanostructures on AP thermal decomposition by thermal techniques. ► Burning rate measurements ofmore » CSPs with ferrite nanostructures. ► Kinetics of thermal decomposition of AP + nanoferrites. -- Abstract: In this paper, the nanoferrites of Mn, Co and Ni were synthesized by wet chemical method and characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), energy dispersive, X-ray spectra (EDS), transmission electron microscopy (TEM) and high resolution transmission electron microscopy (HR-TEM). It is catalytic activity were investigated on the thermal decomposition of ammonium perchlorate (AP) and composite solid propellants (CSPs) using thermogravimetry (TG), TG coupled with differential scanning calorimetry (TG–DSC) and ignition delay measurements. Kinetics of thermal decomposition of AP + nanoferrites have also been investigated using isoconversional and model fitting approaches which have been applied to data for isothermal TG decomposition. The burning rate of CSPs was considerably enhanced by these nanoferrites. Addition of nanoferrites to AP led to shifting of the high temperature decomposition peak toward lower temperature. All these studies reveal that ferrite nanorods show the best catalytic activity superior to that of nanospheres and nanocubes.« less

Silicon nitride grids are compatible with correlative negative staining electron microscopy and tip-enhanced Raman spectroscopy for use in the detection of micro-organisms.

PubMed

Lausch, V; Hermann, P; Laue, M; Bannert, N

2014-06-01

Successive application of negative staining transmission electron microscopy (TEM) and tip-enhanced Raman spectroscopy (TERS) is a new correlative approach that could be used to rapidly and specifically detect and identify single pathogens including bioterrorism-relevant viruses in complex samples. Our objective is to evaluate the TERS-compatibility of commonly used electron microscopy (EM) grids (sample supports), chemicals and negative staining techniques and, if required, to devise appropriate alternatives. While phosphortungstic acid (PTA) is suitable as a heavy metal stain, uranyl acetate, paraformaldehyde in HEPES buffer and alcian blue are unsuitable due to their relatively high Raman scattering. Moreover, the low thermal stability of the carbon-coated pioloform film on copper grids (pioloform grids) negates their utilization. The silicon in the cantilever of the silver-coated atomic force microscope tip used to record TERS spectra suggested that Si-based grids might be employed as alternatives. From all evaluated Si-based TEM grids, the silicon nitride (SiN) grid was found to be best suited, with almost no background Raman signals in the relevant spectral range, a low surface roughness and good particle adhesion properties that could be further improved by glow discharge. Charged SiN grids have excellent particle adhesion properties. The use of these grids in combination with PTA for contrast in the TEM is suitable for subsequent analysis by TERS. The study reports fundamental modifications and optimizations of the negative staining EM method that allows a combination with near-field Raman spectroscopy to acquire a spectroscopic signature from nanoscale biological structures. This should facilitate a more precise diagnosis of single viral particles and other micro-organisms previously localized and visualized in the TEM. © 2014 The Society for Applied Microbiology.

The Potential Protective Effects of 2-aminoethyl Diphenylborinate against Inner Ear Acoustic Trauma: Experimental Study Using Transmission and Scanning Electron Microscopy.

PubMed

Kaymakçı, Mustafa; Acar, Mustafa; Burukoglu, Dilek; Kutlu, Hatice Mehtap; Shojaolsadati, Paria; Cingi, Cemal; Bayar Muluk, Nuray

2015-04-01

In this prospective experimental study, we investigated the preventive effects of 2-aminoethyl diphenylborinate (2-APB) in rats exposed to acoustic trauma (AT). Light microscopic, transmission electron microscopic (TEM), and scanning electron microscopic (SEM) examinations were performed. Eighteen healthy Wistar albino rats were divided into the following three groups: groups 1 (control), 2 (AT), and 3 (AT+APB). The rats in groups 2 and 3 were exposed to AT; in group 3 rats, 2-APB at 2 mg/kg was also administered, initially transperitoneally, after 10 min. During the light microscopic, TEM, and SEM examinations, the structures of the cochlear hair cells, stereocilia, and Deiter's cells were normal in the control group. In the AT group, the organ of Corti and proximate structures were damaged according to the light microscopic examination. During the TEM examination, intense cellular damage and stereocilia loss were detected, while during the SEM examination, extensive damage and stereocilia loss were observed. Decreased damage with preserved cochlear structure was detected during the light microscopic examination in the AT+APB group than in the AT group. During the TEM and SEM examinations, although stereocilia loss occurred in the AT+APB group, near-normal cell, cilia, and tectorial membrane structures were also observed in the AT+APB group compared with the AT group. 2-APB may have protective effects against AT damage of the cochlea. The main mechanism underlying this effect is the inhibition of the vasoconstriction of the cochlear spiral modiolar artery, thereby improving cochlear blood flow. We conclude that 2-APB may also be effective if used immediately following AT.

Solar Flare Track Exposure Ages in Regolith Particles: A Calibration for Transmission Electron Microscope Measurements

NASA Technical Reports Server (NTRS)

Berger, Eve L.; Keller, Lindsay P.

2015-01-01

Mineral grains in lunar and asteroidal regolith samples provide a unique record of their interaction with the space environment. Space weathering effects result from multiple processes including: exposure to the solar wind, which results in ion damage and implantation effects that are preserved in the rims of grains (typically the outermost 100 nm); cosmic ray and solar flare activity, which result in track formation; and impact processes that result in the accumulation of vapor-deposited elements, impact melts and adhering grains on particle surfaces. Determining the rate at which these effects accumulate in the grains during their space exposure is critical to studies of the surface evolution of airless bodies. Solar flare energetic particles (mainly Fe-group nuclei) have a penetration depth of a few millimeters and leave a trail of ionization damage in insulating materials that is readily observable by transmission electron microscope (TEM) imaging. The density of solar flare particle tracks is used to infer the length of time an object was at or near the regolith surface (i.e., its exposure age). Track measurements by TEM methods are routine, yet track production rate calibrations have only been determined using chemical etching techniques [e.g., 1, and references therein]. We used focused ion beam-scanning electron microscope (FIB-SEM) sample preparation techniques combined with TEM imaging to determine the track density/exposure age relations for lunar rock 64455. The 64455 sample was used earlier by [2] to determine a track production rate by chemical etching of tracks in anorthite. Here, we show that combined FIB/TEM techniques provide a more accurate determination of a track production rate and also allow us to extend the calibration to solar flare tracks in olivine.

Nanocuvette: A Functional Ultrathin Liquid Container for Transmission Electron Microscopy.

PubMed

Wadell, Carl; Inagaki, Satoshi; Nakamura, Tomiro; Shi, Ji; Nakamura, Yoshio; Sannomiya, Takumi

2017-02-28

Advances in TEM techniques have spurred a renewed interest in a wide variety of research fields. A rather recent track within these endeavors is the use of TEM for in situ imaging in liquids. In this article, we show the fabrication of a liquid cell for TEM observations which we call the nanocuvette. The structure consists of a nanohole film sandwiched by carbon films, sealing liquid in the holes. The hole film can be produced using a variety of materials, tailored for the desired application. Since the fabrication is based on self-assembly, it is both cheap and straightforward. Compared to previously reported liquid cells, this structure allows for thinner liquid layers with better controlled cell structures, making it possible to achieve a high resolution even at lower acceleration voltages and electron doses. We demonstrate a resolution corresponding to an information transfer up to ∼2 nm at 100 kV for molecular imaging. Apart from the advantages arising from the thin liquid layer, the nanocuvette also enables the possibility to study liquid-solid interfaces at the side walls of the nanoholes. We illustrate the possibilities of the nanocuvette by studying several model systems: electron beam induced growth dynamics of silver nanoparticles in salt solution, polymer deposition from solution, and imaging of nonstained antibodies in solution. Finally, we show how the inclusion of a plasmonically active gold layer in the nanocuvette structure enables optical confirmation of successful liquid encapsulation prior to TEM studies. The nanocuvette provides an easily fabricated and flexible platform which can help further the understanding of reactions, processes, and conformation of molecules and atoms in liquid environments.

Field Emission Gun Scanning Electron (FEGSEM) and Transmission Electron (TEM) Microscopy of Phyllosilicates in Martian Meteorites ALH84001, Nakhla, and Shergotty

NASA Technical Reports Server (NTRS)

Thomas-Keprta, Kathie L.; Wentworth, Susan J.; McKay, David S.; Gibson, Everett K.

2000-01-01

Here we document the occurrence of phyllosilicates and alteration phases in three martian meteorites, suggest formation conditions required for phyllosilicate formation and speculate on the extent of fluid:rock interactions during the past history of Mars.

CHARACTERISTICS OF INDIVIDUAL PARTICLES AT A RURAL SITE IN THE EASTERN UNITED STATES

EPA Science Inventory

To determine the nature of aerosol particles in a rural area of the eastern United States, aerosol samples were collected at Deep Creek Lake, Maryland, on various substrates and analyzed by a scanning electron microscope (SEM) and a transmission electron microscope (TEM). SEM ana...

Comparison of dislocation content measured with transmission electron microscopy and micro-Laue diffraction based streak analysis

DOE PAGES

Zhang, C.; Balachandran, S.; Eisenlohr, P.; ...

2017-10-04

The subsurface dislocation content in a Ti-5Al-2.5Sn (wt%) uniaxial tension sample deformed at ambient temperature was characterized by peak streak analysis of micro-Laue diffraction patterns collected non-destructively by differential aperture X-raymicroscopy, and with focused ion beam transmission electron microscopy of material in the same volume. This comparison reveals that micro-Laue diffraction streak analysis based on an edge dislocation assumption can accurately identify the dominant dislocation slip system history (Burgers vector and plane observed by TEM), despite the fact that dislocations have predominantly screw character. As a result, other dislocations identified by TEM were not convincingly discernible from the peak streakmore » analysis.« less

Comparison of dislocation content measured with transmission electron microscopy and micro-Laue diffraction based streak analysis

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhang, C.; Balachandran, S.; Eisenlohr, P.

The subsurface dislocation content in a Ti-5Al-2.5Sn (wt%) uniaxial tension sample deformed at ambient temperature was characterized by peak streak analysis of micro-Laue diffraction patterns collected non-destructively by differential aperture X-raymicroscopy, and with focused ion beam transmission electron microscopy of material in the same volume. This comparison reveals that micro-Laue diffraction streak analysis based on an edge dislocation assumption can accurately identify the dominant dislocation slip system history (Burgers vector and plane observed by TEM), despite the fact that dislocations have predominantly screw character. As a result, other dislocations identified by TEM were not convincingly discernible from the peak streakmore » analysis.« less

Preparation of a novel breviscapine-loaded halloysite nanotubes complex for controlled release of breviscapine

NASA Astrophysics Data System (ADS)

Gao, Min; Lu, Liqian; Wang, Xiaoyue; Lin, Houke; Zhou, Qingsong

2017-11-01

For sustain the release rate and prolong half-life of breviscapine in vivo, the breviscapine-loaded halloysite nanotubes complex was prepared. The breviscapine was encapsulated into halloysite nanotubes (HNTs) using a vacuum process. The complex were investigated by scanning electron microscopy (SEM), differential scanning calorimetry (DSC), transmission electron microscope (TEM), X-ray diffraction (XRD) and fourier transform infrared spectroscopy(FT-IR). The formation of breviscapine-loaded HNTs complex was proved by the test results of SEM, DSC, TEM and IR analysise. The results confirmed that breviscapine was successfully loaded in the halloysite nanotubes. Additionally, the in vitro drug release of breviscapine from breviscapine-loaded HNTs complex was investigated, the result indicated this complex has apparent sustained-release effect.

Studying dynamic processes in liquids by TEM/STEM/DTEM

NASA Astrophysics Data System (ADS)

Abellan, Patricia; Evans, James; Woehl, Taylor; Jungjohann, Katherine; Parent, Lucas; Arslan, Ilke; Ristenpart, William; Browning, Nigel; Mater. Sci. Group Team; Microsc. Group Team; Catal. Sci. Group Collaboration; Ristenpart Res. Group Collaboration

2013-03-01

In order to study dynamic phenomena such as corrosion or catalysis, extreme environmental conditions must be reproduced around the specimen - these include high-temperatures, high-pressures, specific oxidizing/reducing atmospheres or a liquid environment. The use of environmental stages specifically designed to fit in any transmission electron microscope (TEM) allows us to apply the distinct capabilities of each instrument to study dynamic processes. Localized gas/fluid conditions are created around the sample and separated from the high vacuum inside the microscope using hermetically sealed windowed-cells. Advanced capabilities of these techniques include spatial resolutions of ~1 Angstrom or better in aberration corrected instruments or temporal resolutions in the microsecond-nanosecond range in a dynamic TEM (DTEM). Here, unique qualities of the DTEM that benefit the in-situ experiments with gas/fluid environmental cells will be discussed. We also present our results with a liquid stage allowing atomic resolution imaging of nanomaterials in a colloidal suspension, core EEL spectra acquisition, continuous flow, controlled growth of nanocrystals and systematic calibration of the effect of the electron dose on silver nuclei formation.

Rapid extra-/intracellular biosynthesis of gold nanoparticles by the fungus Penicillium sp.

NASA Astrophysics Data System (ADS)

Du, Liangwei; Xian, Liang; Feng, Jia-Xun

2011-03-01

In this work, the fungus Penicillium was used for rapid extra-/intracellular biosynthesis of gold nanoparticles. AuCl4 - ions reacted with the cell filtrate of Penicillium sp. resulting in extracellular biosynthesis of gold nanoparticles within 1 min. Intracellular biosynthesis of gold nanoparticles was obtained by incubating AuCl4 - solution with fungal biomass for 8 h. The gold nanoparticles were characterized by means of visual observation, UV-Vis absorption spectroscopy, X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), and energy-dispersive X-ray spectroscopy (EDX). The extracellular nanoparticles exhibited maximum absorbance at 545 nm in UV-Vis spectroscopy. The XRD spectrum showed Bragg reflections corresponding to the gold nanocrystals. TEM exhibited the formed spherical gold nanoparticles in the size range from 30 to 50 nm with an average size of 45 nm. SEM and TEM revealed that the intracellular gold nanoparticles were well dispersed on the cell wall and within the cell, and they are mostly spherical in shape with an average diameter of 50 nm. The presence of gold was confirmed by EDX analysis.

Investigation of defect clusters in ion-irradiated Ni and NiCo using diffuse X-ray scattering and electron microscopy

DOE PAGES

Olsen, Raina J.; Jin, Ke; Lu, Chenyang; ...

2015-11-23

The nature of defect clusters in Ni and Nimore » $$_{50}$$Co$$_{50}$$ (NiCo) irradiated at room temperature with 2–16 MeV Ni ions is studied using asymptotic diffuse X-ray scattering and transmission electron microscopy (TEM). Analysis of the scattering data provides separate size distributions for vacancy and interstitial type defect clusters, showing that both types of defect clusters have a smaller size and higher density in NiCo than in Ni. Diffuse scattering results show good quantitative agreement with TEM results for cluster sizes greater than 4 nm diameter, but find that the majority of vacancy clusters are under 2 nm in NiCo, which, if not detected, would lead to the conclusion that defect density was actually lower in the alloy. Interstitial dislocation loops and stacking fault tetrahedra are identified by TEM. Lastly comparison of diffuse scattering lineshapes to those calculated for dislocation loops and SFTs indicates that most of the vacancy clusters are SFTs.« less

Virus Particle Detection by Convolutional Neural Network in Transmission Electron Microscopy Images.

PubMed

Ito, Eisuke; Sato, Takaaki; Sano, Daisuke; Utagawa, Etsuko; Kato, Tsuyoshi

2018-06-01

A new computational method for the detection of virus particles in transmission electron microscopy (TEM) images is presented. Our approach is to use a convolutional neural network that transforms a TEM image to a probabilistic map that indicates where virus particles exist in the image. Our proposed approach automatically and simultaneously learns both discriminative features and classifier for virus particle detection by machine learning, in contrast to existing methods that are based on handcrafted features that yield many false positives and require several postprocessing steps. The detection performance of the proposed method was assessed against a dataset of TEM images containing feline calicivirus particles and compared with several existing detection methods, and the state-of-the-art performance of the developed method for detecting virus was demonstrated. Since our method is based on supervised learning that requires both the input images and their corresponding annotations, it is basically used for detection of already-known viruses. However, the method is highly flexible, and the convolutional networks can adapt themselves to any virus particles by learning automatically from an annotated dataset.

Twinning and martensite in a 304 austenitic stainless steel

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shen, Yongfeng; Li, Xi; Sun, Xin

2012-08-30

The microstructure characteristics and deformation behavior of 304L stainless steel during tensile deformation at two different strain rates have been investigated by means of interrupted tensile tests, electron-backscatter-diffraction (EBSD) and transmission electron microscopy (TEM) techniques. The volume fractions of transformed martensite and deformation twins at different stages of the deformation process were measured using X-ray diffraction method and TEM observations. It is found that the volume fraction of martensite monotonically increases with increasing strain but decreases with increasing strain rate. On the other hand, the volume fraction of twins increases with increasing strain for strain level less than 57%. Beyondmore » that, the volume fraction of twins decreases with increasing strain. Careful TEM observations show that stacking faults (SFs) and twins preferentially occur before the nucleation of martensite. Meanwhile, both {var_epsilon}-martensite and {alpha}{prime}-martensite are observed in the deformation microstructures, indicating the co-existence of stress induced- transformation and strain-induced-transformation. We also discussed the effects of twinning and martensite transformation on work-hardening as well as the relationship between stacking faults, twinning and martensite transformation.« less

LDRD Final Report - In Operando Liquid Cell TEM Characterization of Nickel-Based Electrocatalyst

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nielsen, M. H.

2016-11-07

A commercial electrochemistry stage for transmission electron microscopy (TEM) was tested to determine whether to purchase one for the microscopes at Lawrence Livermore National Lab (LLNL). Deposition of a nickel-based electrocatalyst was pursued as a material system for the purpose of testing the stage. The stage was found to be problematic with recurring issues in the electrical connections and vacuum sealing, which has thus far precluded a systematic investigation of the original material system. However, the electrochemical cells purchased through this FS will allow the Lawrence Fellow (Nielsen) to continue testing the stage. Furthermore, discussions with a second vendor, whichmore » released a similar electrochemical TEM stage during the course of this FS, have resulted in an upcoming longterm loan of their stage at Lawrence Berkeley National Lab (LBNL) for testing. In addition, low-loss electron energy-loss spectroscopy (EELS) measurements on nickel-bearing electrolyte solutions led to a broader EELS investigation of solvents and salt solutions. These measurements form the basis of a manuscript in preparation on EELS measurements of the liquid phase.« less

Scanning transmission X-ray, laser scanning, and transmission electron microscopy mapping of the exopolymeric matrix of microbial biofilms.

PubMed

Lawrence, J R; Swerhone, G D W; Leppard, G G; Araki, T; Zhang, X; West, M M; Hitchcock, A P

2003-09-01

Confocal laser scanning microscopy (CLSM), transmission electron microscopy (TEM), and soft X-ray scanning transmission X-ray microscopy (STXM) were used to map the distribution of macromolecular subcomponents (e.g., polysaccharides, proteins, lipids, and nucleic acids) of biofilm cells and matrix. The biofilms were developed from river water supplemented with methanol, and although they comprised a complex microbial community, the biofilms were dominated by heterotrophic bacteria. TEM provided the highest-resolution structural imaging, CLSM provided detailed compositional information when used in conjunction with molecular probes, and STXM provided compositional mapping of macromolecule distributions without the addition of probes. By examining exactly the same region of a sample with combinations of these techniques (STXM with CLSM and STXM with TEM), we demonstrate that this combination of multimicroscopy analysis can be used to create a detailed correlative map of biofilm structure and composition. We are using these correlative techniques to improve our understanding of the biochemical basis for biofilm organization and to assist studies intended to investigate and optimize biofilms for environmental remediation applications.

Microstructure and composition analysis of low-Z/low-Z multilayers by combining hard and resonant soft X-ray reflectivity

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rao, P. N., E-mail: pnrao@rrcat.gov.in; Rai, S. K.; Srivastava, A. K.

2016-06-28

Microstructure and composition analysis of periodic multilayer structure consisting of a low electron density contrast (EDC) material combination by grazing incidence hard X-ray reflectivity (GIXR), resonant soft X-ray reflectivity (RSXR), and transmission electron microscopy (TEM) are presented. Measurements of reflectivity at different energies allow combining the sensitivity of GIXR data to microstructural parameters like layer thicknesses and interfacing roughness, with the layer composition sensitivity of RSXR. These aspects are shown with an example of 10-period C/B{sub 4}C multilayer. TEM observation reveals that interfaces C on B{sub 4}C and B{sub 4}C on C are symmetric. Although GIXR provides limited structural informationmore » when EDC between layers is low, measurements using a scattering technique like GIXR with a microscopic technique like TEM improve the microstructural information of low EDC combination. The optical constants of buried layers have been derived by RSXR. The derived optical constants from the measured RSXR data suggested the presence of excess carbon into the boron carbide layer.« less

Immunoglobulins and Disease.

DTIC Science & Technology

1987-02-06

MICROCOPY RESOLUTION TEST CHART NA7 UNAL hu AT ’N Ad . . 0 0 10 PROCEEDINGS THE TWENTY-SIXTH MIDWINTER CONFERENCE OF IMMUNOLOGISTS January 17-20, 1987...monoclonal BA5 has also been used to study the abnormal regulation of expression of BCGF receptors in common variable ilmmunodeficiency, SLE , and B cell...antigen, we have shown that membrane Ig-mediated antigen presentation by small B cells to rabbit globulin - specific T cell lines results in a vigorous

Summary of Research Activities Academic Departments 1981-1982.

DTIC Science & Technology

1982-10-01

M12 MICROCOPY RESOLUTIONI TEST CHART NATION4AL BUREAU OF STAN4DARDS- 1963-A SUMMARY OF RESEARCH ACTIVITIES ACADEMIC I DEPARTMENTS 1 1981-1982 42 4...r I OFFICE OF THE ACADEMIC DEAN I UNITED STATES NAVAL ACADEMY ANNAPOLIS, MARYLAND li. 6 4 | I I SUMMARY OF IRESEARCH ACTIVITIES [ 1981 - 1982 i... activities that contribute to the professional growth of the faculty and outstanding midshipmen may flourish. * The research activities of the faculty

Application of the Satellite Triaxial Accelerometer Experiment to Atmospheric Density and Wind Studies.

DTIC Science & Technology

1982-03-04

AL. 84 MAR 82 UNCLASSIFIED RFGL-ERP-774 F/G 22/3, N ’IN ~11 IP LA M °3 MICROCOP MWoWNo TEST CHART MICROCOPY RESOLUTION TEST CHART M ATO MF OF SO MBS...V 0 . To refine the solution a new V = x Vy& VOZ ) is used to calculate a new p. This new p is then used to calculate new velocities. The process is

Effect of Endodontic Access on the Failure Load of Lithium Disilicate and Resin Nano-ceramic CADCAM Crowns

DTIC Science & Technology

2017-06-09

3 August 2016 Douglas D. Lancaster, COL, DC Army Post Graduate Dental School Effect of Endodontic Access on the Failure Load of Lithium...University of the Health Sciences, Bethesda, MD; Schofield Barracks Dental Clinic, Schofield Barracks, HI; Tripler Army Medical Center, Honolulu...underlying die was reached. (Neo Diamond, Microcopy Dental ). The access outline was then completed with a medium (100-110µm) grit round-ended

Metal Oxide Solubility and Molten Salt Corrosion.

DTIC Science & Technology

1982-03-29

METAL OXIDE SOLUBILITY AND MOLTEN SALT CORROSION .(U) MAR 82 K H STERN UNCLASSI E DL R L-4772NL EL .2. MICROCOPY RESOLUTION TEST CHART NATIONAL BURALU...21 l 7 3 ..... l DTIC NSPECT I" ’I cCPY INSECE( METAL OXIDE SOLUBILITY AND MOLTEN SALT CORROSION I. INTRODUCTION Molten ...discussed in terms of its importance to the understanding of molten salt corrosion . II. PROTECTIVE COATINGS Since most structural metals and alloys are

Application and Interpretation of Bioassay and Biomonitoring: A Planning Document.

DTIC Science & Technology

1987-10-13

TNO (The Hague) 9.00 Ecotoxicological risks (drs. tarquenie) 9.20 Hamburg (dr. Tent) - development of dredging and disposal - problems and solutions...MICROCOPY RESOLUTION TEST CHART NATIJAL BURIAU O’ STANU4RDS %, a KTJO86 4-47 Aquatic -estuarine- macrophytes as monitoring organisms for trace metals Dr...that specific aquatic macrophytes may serve as good bio-accumulators of heavy metals and that these plants could be used to quantify the

The Preliminary Pollutant Limit Value Approach: Procedures and Data Base.

DTIC Science & Technology

1984-06-01

IIllfllfflfflffllfllf IIIIIIIIIIIEI 41. ILE. 1 . 0 * n I s . 8c .5 11111 * 1 .6 flu IL MICROCOPY RESOLUTION TEST CHART NATIONAL BUREAU OF STANDARDS...AMEW,&A PROMS wD VE.OIWT coWma PAWIKIOK MARYAI 21701 *. ~~0 1 U..... .~-N:\\W-***- NOTICE * Disclaimer The findings in this report are not to be...APPENDIX HI: NOTATION. .. . .. ...................................... 106.- FIGURE S 1 . Model to derive SPPPLV for pathway 7 (meat consumption

Coaxial Dump Ramjet Combustor Combustion Instabilities. Part I. Parametric Test Data.

DTIC Science & Technology

1981-07-01

AD-AIII 355 COAXIAL DUP RA8.? COMBUSTOR COMBUSTION INSTABILITIES I/~ PART I PARAUER1C. 1111 AIR FORCE WRIONT AERONUTICAL LAOS WRIOIII-PATTERSOll...MICROCOPY RESOLUTION TEST CHART NATIONAL BUREAU OF STANOAROS - 193- A AFWAL-TR-81 -2047 Part 1 COAXIAL DUMP RAMJET COMBUSTOR COMBUSTION INSTABILITIES PART...COMBUSTOR Interim Report for Period COMBUSTION INSTABILITIES February 1979 - March 1980 Part I - Parametric Test Data S. PERFORMING ORG. REPORT NUMBER 7

Evaluation of Used Crankcase Oils Using Computerized Infrared Spectrometry. Appendices.

DTIC Science & Technology

1984-06-01

JUN 84 J0AP-TSC-84-81-APP F/G 20/6 ’ NL BBBBBBB •Tva-.j’.-n^r. r.T T.~C^ 01^ lite MICROCOPY RESOLUTION TEST CHART NATIONAL BUREAU OF...7>- a—-»tc-o ru" »Tier be vrf ->or-co. O SNOOCOOx IVOO 5COO!oOo 5COO 30 irm-i- ivmoc orc>0 •circec OP<IVNI ^l^Of«•. oc

Warranties in Weapon System Procurement: An Analysis of Practice and Theory.

DTIC Science & Technology

1987-04-01

MICROCOPY RESOLUTION TEST CHART NATIONAL BUREAU OF SIANDARDS 1963 A fD r ILE GW cm AD-A190 933 IDA PAPER P-2024 WARRANTIES IN WEAPON SYSTEM PROCUREMENT...EPWT Essential Performance Warranty Test FAR Federal Acquisition Regulation GCS Guidance Control Section GLD Ground Laser Locator Designator GS General...Service IDA Institute for Defense Analyses I&L Installations and Logistics IPT Initial Production Test LDR Laser Designator Rangefimder MLDT Mean

A Case Study of an Aeronautical Systems Division System Program Office.

DTIC Science & Technology

1982-09-01

11111 -’.-- m 1 1.25 111111.4 1 1.6_ MICROCOPY RESOLUTION TEST CHART NATIONAL BUREAU OF STANDARDS-1963-A If. t 1’ I I( N 2> - .~.. * .~ .~-I ~ k~’ ~K ~r...office....assesses.................. 8 Section 11 The Standard Aircraft Sensor UnitProgram........ 32 Section III Terms and Defnition ...contracts with industry, (b) test programs with both industry and other DOD organizations, (c) aircraft production or modification programs with both

On the threshold conditions for electron beam damage of asbestos amosite fibers in the transmission electron microscope (TEM).

PubMed

Martin, Joannie; Beauparlant, Martin; Sauvé, Sébastien; L'Espérance, Gilles

2016-12-01

Asbestos amosite fibers were investigated to evaluate the damage caused by a transmission electron microscope (TEM) electron beam. Since elemental x-ray intensity ratios obtained by energy dispersive x-ray spectroscopy (EDS) are commonly used for asbestos identification, the impact of beam damage on these ratios was evaluated. It was determined that the magnesium/silicon ratio best represented the damage caused to the fiber. Various tests showed that most fibers have a current density threshold above which the chemical composition of the fiber is modified. The value of this threshold current density varied depending on the fiber, regardless of fiber diameter, and in some cases could not be determined. The existence of a threshold electron dose was also demonstrated. This value was dependent on the current density used and can be increased by providing a recovery period between exposures to the electron beam. This study also established that the electron beam current is directly related to the damage rate above a current density of 165 A/cm 2 . The large number of different results obtained suggest, that in order to ensure that the amosite fibers are not damaged, analysis should be conducted below a current density of 100 A/cm 2 .

A Study of Material and Optical Properties of Nano Diamond Wires

DTIC Science & Technology

2016-02-24

These nanomaterials were further characterized by transmission electron microscopy (TEM) in Figure 6. This analysis was made possible by the...development of a new methodology: direct growth on a SiOx-supported TEM grid. These preliminary characterizations suggested the grown nanomaterials are... currently valid OMB control number. PLEASE DO NOT RETURN YOUR FORM TO THE ABOVE ORGANIZATION. 1. REPORT DATE (DD-MM-YYYY)      09-11-2016 2. REPORT TYPE Final

TEM study of the martensitic phases in the ductile DyCu and YCu intermetallic compounds [The martensitic phase transformation in ductile DyCu and YCu intermetallic compounds

DOE PAGES

Cao, G. H.; Oertel, C. -G.; Schaarschuch, R.; ...

2017-05-03

DyCu and YCu are representatives of the family of CsCl-type B2 rare earth intermetallic compounds that exhibit high room temperature ductility. Structure, orientation relationship, and morphology of the martensites in the equiatomic compounds DyCu and YCu are examined using transmission electron microscopy (TEM). TEM studies show that the martensite structures in DyCu and YCu alloys are virtually identical. The martensite is of orthorhombic CrB-type B33 structure with lattice parameters a = 0.38 nm, b = 1.22 nm, and c = 0.40 nm. (021¯) twins were observed in the B33 DyCu and YCu martensites. The orientation relationship of B33 and B2more » phases is (111¯)[112]B33 || (110)[001]B2. The simulated electron diffraction patterns of the B33 phase are consistent with those of experimental observations. TEM investigations also reveal that a dominant orthorhombic FeB-type B27 martensite with lattice parameters a = 0.71 nm, b = 0.45 nm, and c = 0.54 nm exists in YCu alloy. (11¯ 1) twins were observed in the B27 YCu martensite. As a result, the formation mechanism of B2 to B33 and B2 to B27 phase transformation is discussed.« less

Transmission electron microscopy characterization of the interfacial structure of a galvanized dual-phase steel

DOE Office of Scientific and Technical Information (OSTI.GOV)

Aslam, I., E-mail: ia31@msstate.edu

2016-10-15

Site-specific studies were carried out to characterize the interface of a galvanized dual-phase (DP) steel. Focused ion beam (FIB) was used to prepare specimens in the interface region (~ 100 nm thick) between the coating and the substrate. Transmission electron microscopy (TEM), scanning TEM (STEM), and high resolution TEM (HRTEM) were performed to resolve the phases and the structures at the interface between the zinc (Zn) coating and the steel substrate. The STEM and TEM results showed that a continuous manganese oxide (MnO) film with a thickness of ~ 20 nm was present on the surface of the substrate whilemore » no silicon (Si) oxides were resolved. Internal oxide particles were observed as well in the sub-surface region. Despite the presence of the continuous oxide film, a well-developed inhibition layer was observed right on top of the oxide film. The inhibition layer has a thickness of ~ 100 nm. Possible mechanisms for the growth of the inhibition layer were discussed. - Highlights: •Site-specific examinations were performed on the Zn/steel interface. •Continuous external MnO oxides (20 nm) were observed at the interface. •No Si oxides were observed at the interface. •Internal oxide particles were distributed in the subsurface. •A continuous inhibition layer grew on top of the external oxides.« less

Structure and Dynamics of Domains in Ferroelectric Nanostructures. In-situ TEM Studies

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pan, Xiaoqing

2015-06-30

The goal of this project was to explore the structure and dynamic behaviors of ferroelectric domains in ferroelectric thin films and nanostructures by advanced transmission electron microscopy (TEM) techniques in close collaboration with phase field modeling. The experimental techniques used include aberration-corrected sub-Å resolution TEM and in-situ TEM using a novel scanning tunneling microscopy (STM) - TEM holder that allows the direct observation of nucleation and dynamic evolution of ferroelectric domains under applied electric field. Specifically, this project was aimed to (1) to study the roles of static electrical boundary conditions and electrical charge in controlling the equilibrium domain structuresmore » of BiFeO 3 thin films with controlled substrate constraints, (2) to explore the fundamental mechanisms of ferroelectric domain nucleation, growth, and switching under an applied electric field in both uniform thin films and nanostructures, and to understand the roles of crystal defects such as dislocations and interfaces in these processes, (3) to understand the physics of ferroelectric domain walls and the influence of defects on the electrical switching of ferroelectric domains.« less

Strains on the nano- and microscale in nickel-titanium: An advanced TEM study

NASA Astrophysics Data System (ADS)

Tirry, Wim

2007-12-01

A general introduction to shape memory behavior and the martensitic transformation is given in chapter 1, with speck information concerning the NiTi material. The technique used to study the material is transmission electron microscopy (TEM) of which the basics are explained in chapter 2 as well as information concerning the NiTi material. The main goal was to apply more advanced TEM techniques in order to measure some aspects in a quantitative way rather than qualitative, which is mostly the case in conventional TEM. (1) Quantitative electron diffraction was used to refine the structure of Ni4Ti3 precipitates, this was done by using the MSLS method in combination with density functional theory (DFT) calculations. (2) These Ni4Ti3 precipitates are (semi-)coherent which results in a strain field in the matrix close to the precipitate. High resolution TEM (HRTEM) in combination with image processing techniques was used to measure these strain fields. The obtained results are compared to the Eshelby model for elliptical inclusions, and major difference is an underestimation of the strain magnitude by the model. One of the algorithms used to extract strain information from HRTEM images is the geometric phase method. (3) The Ni4Ti3-Ni4Ti3 and Ni4Ti3-precipitate interface was investigated with HRTEM showing that the Ni4Ti3-precipitate interface might be diffuse over a range of 3nm. (4) In-situ straining experiments were performed on single crystalline and superelastic polycrystalline NiTi samples. It seems that the strain induced martensite planes in the polycrystalline sample show no sign of twinning. This is in contradiction to what is expected and is discussed in the view of the crystallographic theory of martensite, in addition a first model explaining this behavior is proposed. In this dissertation the main attention is divided over the material aspects of NiTi and on how to apply these more advanced TEM techniques.

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

NASA Astrophysics Data System (ADS)

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 <111> identified by post-mortem scanning TEM (STEM) imaging correspond to hotspots on the heatmap, whereas positions of dislocation loops with b = <100> do not correspond to hotspots. Further, MicroViBe enables consistent, objective quantitative approximation of the b = ½ <111> dislocation loop number density.

Growing Carbon Nanotubes

DOE Office of Scientific and Technical Information (OSTI.GOV)

None

In situ transmission electron microscope (TEM) video (accelerated 10 times) of nucleation and self-organization of a high-density carbon nanotube network from catalytic iron nanoparticles, forming a vertically aligned forest.

High-Resolution Mineralogical Characterization and Biogeochemical Modeling of Uranium Reduction Pathways at the NABIR Field-Research Center

DOE Office of Scientific and Technical Information (OSTI.GOV)

David R. Veblen; Chen Zhu; Lee Krumholz

The effectiveness and feasibility of bioremediation at the field scale cannot be fully assessed until the mechanisms of immobilization and U speciation in the solid matrix are resolved. However, characterization of the immobilized U and its valence states is extremely difficult, because microbially mediated mineral precipitates are generally nanometer (nm)-sized, poorly crystalline, or amorphous. We are developing combined field emission gun--scanning electron microscopy (FEG-SEM, at Indiana University) and FEG transmission electron microscopy (TEM, at Hopkins) to detect and isolate uranium containing phases; (1) method developments for TEM sample preparations and parallel electron energy loss spectroscopy (EELS) determination of uranium valence;more » and (2) to determine the speciation, fate, reactivity, valence states of immobilized uranium, using the state-of-the-art 300-kV, FEG-TEM. We have obtained preliminary results on contaminated sediments from Area 3 at the Oak Ridge Field Research Center (FRC). TEM results show that the sediments contain numerous minerals, including quartz, mica/clay (muscovite and/or illite), rutile, ilmenite, zircon, and an Al-Sr-Ce-Ca phosphate mineral, none of which contain uranium above the EDS detection limit. Substantial U (up to {approx}2 wt.%) is, however, clearly associated with two materials: (1) the Fe oxyhydroxide and (2) clots of a chemically complex material that is likely a mixture of several nm-scale phases. The Fe oxyhydroxide was identified as goethite from its polycrystalline SAED pattern and EDS analysis showing it to be very Fe-rich; the aggregate also displays one of several morphologies that are common for goethite. U is strongly sorbed to goethite in the FRC sediment, and the ubiquitous association with phosphorous suggests that complexes containing both U and P may play an important role in that sorption. Results from bulk analysis and SEM had previously demonstrated the association of U with Fe and thus suggested that U may be sorbed by Fe oxide or oxyhydroxide (Dr. Roh, image presented by David Watson). However, rigorous identification of the host minerals for U requires TEM results such as these involving imaging, electron diffraction, and spectroscopic analysis. An even higher concentration of U occurs in the chemically complex material noted above. These ''clots'' are high in Fe but also contain C, O, Mg, Al, Si, P, S, Cl, K, Ca, Mn, and U. This chemical complexity strongly suggests that they consist of aggregates of carbonate, silicate, phosphate, and sulfate phases, and TEM images also suggest that they may be intergrowths of numerous exceedingly small nanoparticles. EELS and EFTEM studies should be able to resolve these various components and identify precisely where the uranium is in these complex materials. From the results, it is clear that the FEG-SEM and FEG-TEM can readily detect uranium in the FRC samples. The FEG-SEM allows a wide field of view of the samples and can detect U-rich aggregates as small as 20-30 nm. The FEG-TEM can then focus on these aggregates and use SAED, EDS, EFTEM, and PEELS techniques to determine the valence states, structures, and compositional data for these aggregates. This research will provide a crucial component for a complete understanding of the efficacy of uranium bioremediation.« less

Transmission electron microscope studies of extraterrestrial materials

NASA Technical Reports Server (NTRS)

Keller, Lindsay P.

1995-01-01

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

Three-dimensional imaging of adherent cells using FIB/SEM and STEM.

PubMed

Villinger, Clarissa; Schauflinger, Martin; Gregorius, Heiko; Kranz, Christine; Höhn, Katharina; Nafeey, Soufi; Walther, Paul

2014-01-01

In this chapter we describe three different approaches for three-dimensional imaging of electron microscopic samples: serial sectioning transmission electron microscopy (TEM), scanning transmission electron microscopy (STEM) tomography, and focused ion beam/scanning electron microscopy (FIB/SEM) tomography. With these methods, relatively large volumes of resin-embedded biological structures can be analyzed at resolutions of a few nm within a reasonable expenditure of time. The traditional method is serial sectioning and imaging the same area in all sections. Another method is TEM tomography that involves tilting a section in the electron beam and then reconstruction of the volume by back projection of the images. When the scanning transmission (STEM) mode is used, thicker sections (up to 1 μm) can be analyzed. The third approach presented here is focused ion beam/scanning electron microscopy (FIB/SEM) tomography, in which a sample is repeatedly milled with a focused ion beam (FIB) and each newly produced block face is imaged with the scanning electron microscope (SEM). This process can be repeated ad libitum in arbitrary small increments allowing 3D analysis of relatively large volumes such as eukaryotic cells. We show that resolution of this approach is considerably improved when the secondary electron signal is used. However, the most important prerequisite for three-dimensional imaging is good specimen preparation. For all three imaging methods, cryo-fixed (high-pressure frozen) and freeze-substituted samples have been used.

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

PubMed

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.

Bio-derived hierarchically macro-meso-micro porous carbon anode for lithium/sodium ion batteries

NASA Astrophysics Data System (ADS)

Elizabeth, Indu; Singh, Bhanu Pratap; Trikha, Sunil; Gopukumar, Sukumaran

2016-10-01

Nitrogen doped hierarchically porous carbon derived from prawn shells have been efficiently synthesized through a simple, economically viable and environmentally benign approach. The prawn shell derived carbon (PSC) has high inherent nitrogen content (5.3%) and possesses a unique porous structure with the co-existence of macro, meso and micropores which can afford facile storage and transport channels for both Li and Na ions. PSC is well characterized using X-ray diffraction (XRD), Field Emission Scanning Electron Microscopy (FE-SEM), Transmission electron Microscopy (TEM), High resolution TEM (HR-TEM) and X-ray photoelectron spectroscopy (XPS). Electron Paramagnetic Resonance (EPR) and Solid state-Nuclear Magnetic Resonance (NMR) studies have been conducted on pristine PSC and Li/Na interacted PSC. PSC as anode for Lithium ion batteries (LIBs) delivers superior electrochemical reversible specific capacity (740 mAh g-1 at 0.1 Ag-1 current density for 150 cycles) and high rate capability. When used as anode material for Sodium ion batteries (SIBs), PSC exhibits excellent reversible specific capacity of 325 mAh g-1 at 0.1 Ag-1 for 200 cycles and rate capability of 107 mAh g-1 at 2 Ag-1. Furthermore, this study demonstrates the employment of natural waste material as a potential anode for both LIB and SIB, which will definitively make a strike in the energy storage field.

Anterior lens epithelium in intumescent white cataracts - scanning and transmission electron microscopy study.

PubMed

Andjelic, Sofija; Drašlar, Kazimir; Hvala, Anastazija; Hawlina, Marko

2016-02-01

Our purpose was to study the structure of the lens epithelial cells (LECs) of intumescent white cataracts (IC) in comparison with nuclear cataracts (NC) in order to investigate possible structural reasons for development of IC. The anterior lens capsule (aLC: basement membrane and associated LECs) were obtained from cataract surgery and prepared for scanning electron microscopy (SEM) and transmission electron microscopy (TEM). We observed by SEM that in IC, LEC swelling was pronounced with the clefts surrounding the groups of LECs. Another structural feature was spherical formations, that were observed on the apical side of LEC's, towards the fibre cell layer, both by SEM and TEM. Development of these structures, bulging out from the apical cell membrane of the LEC's and disrupting it, could be followed in steps towards the sphere formation. The degeneration of the lens epithelium and the structures of the aLC in IC similar to Morgagnian globules were also observed. None of these structural changes were observed in NC. We show by SEM and TEM that, in IC, LECs have pronounced structural features not observed in NC. This supports the hypothesis that the disturbed structure of LECs plays a role in water accumulation in the IC lens. We also suggest that, in IC, LECs produce bulging spheres that represent unique structures of degenerated material, extruded from the LEC.

Amperometric glucose biosensor based on glucose oxidase dispersed in multiwalled carbon nanotubes/graphene oxide hybrid biocomposite.

PubMed

Palanisamy, Selvakumar; Cheemalapati, Srikanth; Chen, Shen-Ming

2014-01-01

An amperometric glucose biosensor based on enhanced and fast direct electron transfer (DET) of glucose oxidase (GOx) at enzyme dispersed multiwalled carbon nanotubes/graphene oxide (MWCNT/GO) hybrid biocomposite was developed. The fabricated hybrid biocomposite was characterized by transmission electron microscopy (TEM), Raman and infrared spectroscopy (IR). The TEM image of hybrid biocomposite reveals that a thin layer of GOx was covered on the surface of MWCNT/GO hybrid composite. IR results validate that the hybrid biocomposite was formed through the electrostatic interactions between GOx and MWCNT/GO hybrid composite. Further, MWCNT/GO hybrid composite has also been characterized by TEM and UV-visible spectroscopy. A pair of well-defined redox peak was observed for GOx immobilized at the hybrid biocomposite electrode than that immobilized at the MWCNT modified electrode. The electron transfer rate constant (Ks) of GOx at the hybrid biocomposite was calculated to be 11.22s(-1). The higher Ks value revealed that fast DET of GOx occurred at the electrode surface. Moreover, fabricated biosensor showed a good sensitivity towards glucose oxidation over a linear range 0.05-23.2mM. The limit of detection (LOD) was estimated to be 28μM. The good features of the proposed biosensor could be used for the accurate detection of glucose in the biological samples. © 2013.

Electronic structure, magnetic and structural properties of Ni doped ZnO nanoparticles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kumar, Shalendra, E-mail: shailuphy@gmail.com; Vats, Prashant; Gautam, S.

Highlights: • XRD, and HR-TEM results show the single phase nature of Ni doped ZnO nanoparticles. • dc magnetization results indicate the RT-FM in Ni doped ZnO nanoparticles. • Ni L{sub 3,2} edge NEXAFS spectra infer that Ni ions are in +2 valence state. • O K edge NEXAFS spectra show that O vacancy increases with Ni doping in ZnO. - Abstract: We report structural, magnetic and electronic structural properties of Ni doped ZnO nanoparticles prepared by auto-combustion method. The prepared nanoparticles were characterized by using X-ray diffraction (XRD), high resolution transmission electron microscopy (HR-TEM), near edge X-ray absorption finemore » structure (NEXAFS) spectroscopy, and dc magnetization measurements. The XRD and HR-TEM results indicate that Ni doped ZnO nanoparticles have single phase nature with wurtzite lattice and exclude the presence of secondary phase. NEXAFS measurements performed at Ni L{sub 3,2}-edges indicates that Ni ions are in +2 valence state and exclude the presence of Ni metal clusters. O K-edge NEXAFS spectra indicate an increase in oxygen vacancies with Ni-doping, while Zn L{sub 3,2}-edge show the absence of Zn-vacancies. The magnetization measurements performed at room temperature shows that pure and Ni doped ZnO exhibits ferromagnetic behavior.« less

Study on the Electrochemical Reaction Mechanism of ZnFe2O4 by In Situ Transmission Electron Microscopy

PubMed Central

Su, Qingmei; Wang, Shixin; Yao, Libing; Li, Haojie; Du, Gaohui; Ye, Huiqun; Fang, Yunzhang

2016-01-01

A family of mixed transition–metal oxides (MTMOs) has great potential for applications as anodes for lithium ion batteries (LIBs). However, the reaction mechanism of MTMOs anodes during lithiation/delithiation is remain unclear. Here, the lithiation/delithiation processes of ZnFe2O4 nanoparticles are observed dynamically using in situ transmission electron microscopy (TEM). Our results suggest that during the first lithiation process the ZnFe2O4 nanoparticles undergo a conversion process and generate a composite structure of 1–3 nm Fe and Zn nanograins within Li2O matrix. During the delithiation process, volume contraction and the conversion of Zn and Fe take place with the disappearance of Li2O, followed by the complete conversion to Fe2O3 and ZnO not the original phase ZnFe2O4. The following cycles are dominated by the full reversible phase conversion between Zn, Fe and ZnO, Fe2O3. The Fe valence evolution during cycles evidenced by electron energy–loss spectroscopy (EELS) techniques also exhibit the reversible conversion between Fe and Fe2O3 after the first lithiation, agreeing well with the in situ TEM results. Such in situ TEM observations provide valuable phenomenological insights into electrochemical reaction of MTMOs, which may help to optimize the composition of anode materials for further improved electrochemical performance. PMID:27306189

Organic-inorganic random copolymers from methacrylate-terminated poly(ethylene oxide) with 3-methacryloxypropylheptaphenyl polyhedral oligomeric silsesquioxane: synthesis via RAFT polymerization and self-assembly behavior.

PubMed

Wei, Kun; Li, Lei; Zheng, Sixun; Wang, Ge; Liang, Qi

2014-01-14

In this contribution, we report the synthesis of organic-inorganic random polymers from methacrylate-terminated poly(ethylene oxide) (MAPEO) (Mn = 950) and 3-methacryloxypropylheptaphenyl polyhedral oligomeric silsesquioxane (MAPOSS) macromers via reversible addition-fragmentation chain transfer (RAFT) polymerization with 4-cyano-4-(thiobenzoylthio) valeric acid (CTBTVA) as the chain transfer agent. The organic-inorganic random copolymers were characterized by means of (1)H NMR spectroscopy, gel permeation chromatography (GPC) and differential scanning calorimetry (DSC). The results of GPC indicate that the polymerizations were carried out in a controlled fashion. Transmission electron microscopy (TEM) showed that the organic-inorganic random copolymers in bulk were microphase-separated and the POSS microdomains were formed via POSS-POSS interactions. In aqueous solutions the organic-inorganic random copolymers were capable of self-assembling into spherical nanoobjects as evidenced by transmission electron microscopy (TEM) and dynamic laser scattering (DLS). The self-assembly behavior of the organic-inorganic random copolymers was also found to occur in the mixtures with the precursors of epoxy. The nanostructures were further fixed via subsequent curing reaction and thus the organic-inorganic nanocomposites were obtained. The formation of nanophases in epoxy thermosets was confirmed by transmission electron microscopy (TEM) and dynamic mechanical thermal analysis (DMTA). The organic-inorganic nanocomposites displayed the enhanced surface hydrophobicity as evidenced by surface contact angle measurements.

Structural analysis of ion-implanted chemical-vapor-deposited diamond by transmission electron microscope

NASA Astrophysics Data System (ADS)

Jiang, N.; Deguchi, M.; Wang, C. L.; Won, J. H.; Jeon, H. M.; Mori, Y.; Hatta, A.; Kitabatake, M.; Ito, T.; Hirao, T.; Sasaki, T.; Hiraki, A.

1997-04-01

A transmission electron microscope (TEM) study of ion-implanted chemical-vapor-deposited (CVD) diamond is presented. CVD diamond used for transmission electron microscope observation was directly deposited onto Mo TEM grids. As-deposited specimens were irradiated by C (100 keV) ions at room temperature with a wide range of implantation doses (10 12-10 17/cm 2). Transmission electron diffraction (TED) patterns indicate that there exists a critical dose ( Dc) for the onset of amorphization of CVD diamond as a result of ion induced damage and the value of critical dose is confirmed to be about 3 × 10 15/cm 2. The ion-induced transformation process is clearly revealed by high resolution electron microscope (HREM) images. For a higher dose implantation (7 × 10 15/cm 2) a large amount of diamond phase is transformed into amorphous carbon and many tiny misoriented diamond blocks are found to be left in the amorphous solid. The average size of these misoriented diamond blocks is only about 1-2 nm. Further bombardment (10 17/cm 2) almost kills all of the diamond phase within the irradiated volume and moreover leads to local formation of micropolycrystalline graphite.

Synthesis of carbon-encapsulated metal nanoparticles from wood char

Treesearch

Yicheng Du; Chuji Wang; Hossein Toghiani; Zhiyong Cai; Xiaojian Liu; Jilei Zhang; Qiangu Yan

2010-01-01

Carbon-encapsulated metal nanoparticles were synthesized by thermal treatment of wood char, with or without transition metal ions pre-impregnated, at 900ºC to 1,100ºC. Nanoparticles with concentric multilayer shells were observed. The nanoparticles were analyzed by scanning electron microscopy, transmission electron microscopy (TEM), X-ray diffraction...

The Application of High-Resolution Electron Microscopy to Problems in Solid State Chemistry: The Exploits of a Peeping TEM.

ERIC Educational Resources Information Center

Eyring, LeRoy

1980-01-01

Describes methods for using the high-resolution electron microscope in conjunction with other tools to reveal the identity and environment of atoms. Problems discussed include the ultimate structure of real crystalline solids including defect structure and the mechanisms of chemical reactions. (CS)

Collaboration at the Nanoscale: Exploring Viral Genetics with Electron Microscopy

ERIC Educational Resources Information Center

Duboise, S. Monroe; Moulton, Karen D.; Jamison, Jennifer L.

2009-01-01

The Maine Science Corps is a project sponsored by the National Science Foundation's (NSF) Graduate Teaching Fellows in K-12 Education (GK-12 ) program. Through this program, the University of Southern Maine's (USM) virology and transmission electron microscopy (TEM) research group provides high school teachers and students in rural areas with…

Controllable synthesis and electrochemical hydrogen storage properties of Sb₂Se₃ ultralong nanobelts with urchin-like structures.

PubMed

Jin, Rencheng; Chen, Gang; Pei, Jian; Sun, Jingxue; Wang, Yang

2011-09-01

The controlled synthesis of one-dimensional and three-dimensional Sb(2)Se(3) nanostructures has been achieved by a facile solvothermal process in the presence of citric acid. By simply controlling the concentration of citric acid, the nucleation, growth direction and exposed facet can be readily tuned, which brings the different morphologies and nanostructures to the final products. The as-prepared products have been characterized by means of X-ray diffraction, field-emission scanning electron microscopy, transmission electron microscopy (TEM), high-resolution TEM and selected area electron diffraction. Based on the electron microscope observations, a possible growth mechanism of Sb(2)Se(3) with distinctive morphologies including ultralong nanobelts, hierarchical urchin-like nanostructures is proposed and discussed in detail. The electrochemical hydrogen storage measurements reveal that the morphology plays a key role on the hydrogen storage capacity of Sb(2)Se(3) nanostructures. The Sb(2)Se(3) ultralong nanobelts with high percentage of {-111} facets exhibit higher hydrogen storage capacity (228.5 mA h g(-1)) and better cycle stability at room temperature.

Ciliary body toxicities of systemic oxcarbazepine and valproic acid treatments: electron microscopic study.

PubMed

Göktaş, Güleser; Aktaş, Zeynep; Erdoğan, Deniz; Seymen, Cemile Merve; Karaca, Emine Esra; Cansu, Ali; Serdaroğlu, Ayşe; Kaplanoğlu, Gülnur Take

2015-01-01

Ciliary body is responsible for humour aqueous production in posterior chamber. Valproic acid (VPA) has been widely used for the treatment of epilepsy and other neuropsychiatric diseases such as bipolar disease and major depression. Oxcarbazepine (OXC) is a new anti-epileptic agent that has been used recently for childhood epilepsies such as VPA. In this study, we aimed to investigate the effects of VPA and OXC treatments used as antiepileptic in ciliary body by electron microscopy. In our study, 40 Wistar rats (21 days old) were divided equally into four groups which were applied saline (group 1), VPA (group 2), OXC (group 3) and VPA + OXC (group 4). The as-prepared ocular tissues were characterized by transmission electron microscopy (TEM) technique in scanning and transmission electron microscopy (SEM-TEM) (Carl Zeiss EVO LS10). The results confirmed that VPA caused dense ciliary body degeneration. Additionally, ciliary body degeneration in group 4 was supposed to be due to VPA treatment. Ciliary body damage and secondary outcomes should be considered in patients with long-term VPA therapy.

Electron microscopy characterization of Ni-Cr-B-Si-C laser deposited coatings.

PubMed

Hemmati, I; Rao, J C; Ocelík, V; De Hosson, J Th M

2013-02-01

During laser deposition of Ni-Cr-B-Si-C alloys with high amounts of Cr and B, various microstructures and phases can be generated from the same chemical composition that results in heterogeneous properties in the clad layer. In this study, the microstructure and phase constitution of a high-alloy Ni-Cr-B-Si-C coating deposited by laser cladding were analyzed by a combination of several microscopy characterization techniques including scanning electron microscopy in secondary and backscatter imaging modes, energy dispersive spectroscopy (EDS), electron backscatter diffraction (EBSD), and transmission electron microscopy (TEM). The combination of EDS and EBSD allowed unequivocal identification of micron-sized precipitates as polycrystalline orthorhombic CrB, single crystal tetragonal Cr5B3, and single crystal hexagonal Cr7C3. In addition, TEM characterization showed various equilibrium and metastable Ni-B, Ni-Si, and Ni-Si-B eutectic products in the alloy matrix. The findings of this study can be used to explain the phase formation reactions and to tune the microstructure of Ni-Cr-B-Si-C coatings to obtain the desired properties.

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

PubMed

Harris, J Robin

2015-09-01

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

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

NASA Astrophysics Data System (ADS)

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 as dip-coating and drop-casting, commonly used for depositing nanoparticles on a surface via convective-capillary assembly. Theoretical analysis suggests that the observed particle motion and aggregation are caused by gradients in surface tension and disjoining pressure in the thin liquid film.

Evaluation of poly (vinyl alcohol) based cryogel-zinc oxide nanocomposites for possible applications as wound dressing materials.

PubMed

Chaturvedi, Archana; Bajpai, Anil K; Bajpai, Jaya; K Singh, Sunil

2016-08-01

In this investigation cryogels composed of poly (vinyl alcohol) (PVA) were prepared by repeated freeze thaw method followed by in situ precipitation of zinc oxide nanoparticles within the cryogel networks. Fourier transformed infrared spectroscopy (FTIR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray diffraction (XRD), Energy dispersive X-ray spectroscopy (EDX) were used to characterize the nanocomposites. The morphologies of native PVA cryogels and PVA cryogel-ZnO nanocomposites were observed by scanning electron microscopy (SEM), transmission electron microscopy (TEM) techniques. The SEM analysis suggested that cryogels show a well-defined porous morphology whereas TEM micrographs revealed the presence of nearly spherical and well separated zinc oxide nanoparticles with diameter<100nm. XRD results showed all relevant Bragg's reflections for crystal structure of zinc oxide nanoparticles. Thermo gravimetric-differential thermal analysis (TG-DTA) was conducted to evaluate thermal stability of the nanocomposites. Mechanical properties of nanocomposites were determined in terms of tensile strength and percent elongation. Biocompatible nature was ascertained by anti-haemolytic activity, bovine serum albumin (blood protein) adsorption and in vitro cytotoxicity tests. The prepared nanocomposites were also investigated for swelling and deswelling behaviours. The results revealed that both the swelling and deswelling process depend on the chemical composition of the nanocomposites, number of freeze-thaw cycles, pH and temperature of the swelling medium. The developed biocompatible PVA cryogel-ZnO nanocomposites were also tested for antibacterial activities against both Gram-negative and Gram-positive bacteria. Copyright © 2016 Elsevier B.V. All rights reserved.

Interstitial Hardening of Stainless Steel for Enhanced Corrosion Resistance for Naval Applications

DTIC Science & Technology

2017-03-01

CASE WESTERN ]\\!:SERVE U N I V E R S I T Y EST. 1826 March 1, 2017 Defense Technical Information Center 8725 John J Kingman Road , Sute 0944...electron microscopy (TEM) ~o ·determ: t;<: the origin of the dramatic surface roughness effect just described. A cross-sectional TEM image obtained from...CASE WESTERN RESERVE UNIVERSITY REPORT NUMBER 10900 EUCLID AVE. CLEVELAND, OHIO 44106-7015 9. SPONSORING/MONITORING AGENCY NAME(S) AND ADDRESS(ES) 10

Size Dependent Pore Formation in Germanium Nanowires Undergoing Reversible Delithiation Observed by In Situ TEM

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lu, Xiaotang; He, Yang; Mao, Scott X.

Germanium (Ge) nanowires coated with an amorphous silicon (Si) shell undergoing lithiation and delithiation were studied using in situ transmission electron microscopy (TEM). Delithiation creates pores in nanowires with diameters larger than ~25 nm, but not in smaller diameter nanowires. The formation of pores in Ge nanowires undergoing delithiation has been observed before in in situ TEM experiments, but there has been no indication that a critical diameter exists below which pores do not form. Pore formation occurs as a result of fast lithium diffusion compared to vacancy migration. We propose that a short diffusion path for vacancies to themore » nanowire surface plays a role in limiting pore formation even when lithium diffusion is fast.« less

Quantitative characterization of nanoparticle agglomeration within biological media

NASA Astrophysics Data System (ADS)

Hondow, Nicole; Brydson, Rik; Wang, Peiyi; Holton, Mark D.; Brown, M. Rowan; Rees, Paul; Summers, Huw D.; Brown, Andy

2012-07-01

Quantitative analysis of nanoparticle dispersion state within biological media is essential to understanding cellular uptake and the roles of diffusion, sedimentation, and endocytosis in determining nanoparticle dose. The dispersion of polymer-coated CdTe/ZnS quantum dots in water and cell growth medium with and without fetal bovine serum was analyzed by transmission electron microscopy (TEM) and dynamic light scattering (DLS) techniques. Characterization by TEM of samples prepared by plunge freezing the blotted solutions into liquid ethane was sensitive to the dispersion state of the quantum dots and enabled measurement of agglomerate size distributions even in the presence of serum proteins where DLS failed. In addition, TEM showed a reduced packing fraction of quantum dots per agglomerate when dispersed in biological media and serum compared to just water, highlighting the effect of interactions between the media, serum proteins, and the quantum dots. The identification of a heterogeneous distribution of quantum dots and quantum dot agglomerates in cell growth medium and serum by TEM will enable correlation with the previously reported optical metrology of in vitro cellular uptake of this quantum dot dispersion. In this paper, we present a comparative study of TEM and DLS and show that plunge-freeze TEM provides a robust assessment of nanoparticle agglomeration state.

Immunology Research in Israel.

DTIC Science & Technology

1985-11-14

sonCLSIIDFG6S 1 .01 56 *3 2 . 1.8. 11111.2 1111 . MICROCOPY RESOLU TION TEST CHART W NAIN L 8UE OSTNA1936 - Ilile I.. - t"t 4-. r; I...pursued by Israel.i scientists include investigation of irmuno- globulin genes, structure-f unction analysis of antibodies and regulation of antibody...investigation of immuno- that had been first formulated by M. globulin genes, structure-function anal- Sela and R. Arnon. D. Givol pioneered in ysis of

Integrated Services Digital Network (ISDN).

DTIC Science & Technology

1985-06-01

U.S. Digital Networks," Telephony, February 6, 1984. Gerla, Mario and Pazos -Rangel, Rodolfo A ., "Bandwidth Allocation and Routing in ISDN’s," IEEE...111116o 1312. jf IL5 11111.4 MICROCOPY RESOLUTION TEST CHART NATIONAL BUREAU OF STANDARDS-1963 A • .4 i U-~ U. NAVAL POSTGRADUATE SCHOOL G ,.Monterey...Thesis Advisor: C. R. Jones P: A -nroved for nublic release; distribution unlimited 85o 09 s0 082 1--𔃻- S **. -: -* *.- -. ..-. * SECURITY CLASSIFICATION

Simulators for Mariner Training and Licensing. Phase 2: Investigation of Simulator Characteristics for Training Senior Mariners,

DTIC Science & Technology

1981-10-01

GYNTHER. .J A GRASSO UNCLASSIFIED CAORF5 7 15-02 USCG-D-Os-82 NL mhmmmmhhhhhhu -EEomhEmhEEEEI liiiW,- 11 12B .0 MICROCOPY RESOLUIOCN TEST CHART CAORF 0701...1981 Simulator Characteristics for Training Senior Mariners 6 7 . Author~sd U. Palo * eu misatioul "as MSe e. T. J. Hamnmell, J1. W. Gynther, J. A...2- 7 2A Experimental Procedures .................................................... 2-13 2.5 Data Analysis

Helping Patients Cope with Inflammatory Bowel Disease.

DTIC Science & Technology

1984-01-01

84-65T UNCLSSIFIED FG 63 NL I flflflflmfl. LuN _ 11L1 la Ig 1.125 ll._4 11. MICROCOPY RESOLUTION TEST CHART NATIONAL BUREAU OF STANDARDS-1963-A...relationship with psychological factors such as marital discord, anxiety related to children, loss of a loved one, and other obsessional worries. On the...disease, not the cause of it (Mendeloff, at. al., 1970, & Sparberg, 1982). It is this psychological aspect that is at the center of mis- conception about

Health and Performance of Antarctic Winter-Over Personnel: A Follow-Up Study.

DTIC Science & Technology

1985-06-01

PALINKAS JUN 95 I UNCLSSIFIED NHRSCHSC05-18-1 F/O6/1NL IlflONfl w2.2 1.2511.4 11.IIII1III MICROCOPY RESOLUTION TEST CHART NATIONAL BURtAU OF STANOAROS...isolation during this period is associated with numerous social and psychological strebsors, in addition to physiological changes. Objective The...winter. The pro- longed isolation during this period is associated with numerous social and psychological stressors. Polarization of subgroups of civilian

Hospitalizations for Accidents and Injuries in the U.S. Navy. III. Time in Assignment and Seniority.

DTIC Science & Technology

1985-09-01

MICROCOPY RESOLUTION TEST CHART NATIONAL BJREAU OF STANARDS 1963 A 2i ... ........................ . . . . . . . . . . . . AD-A161 677 HOSPITALIZATIONS FOR...formula ( Lilienfeld and Lilien- feld, 19801: p ± 1.96 (p)(l-P) N Relative risk levels were then computed as the ratio of these rates; 95% confidence...financial change, etc.) which bring about a significant change * in an individual’s ongoing life pattern may cause psychological turrmoil that can

A Relational Data Dictionary Compatible with the National Bureau of Standards Information Resource Dictionary System.

DTIC Science & Technology

1985-12-01

85 UNCLSSIFIED F/ 3/2 NL mhhhhhhhhhhhhl 4y 1.0 &32 MICROCOPY RESOLUTIOf TEST CKART. N NAVAL POSTGRADUATE SCHOOL Monterey, California DTIC ELECTE...Concern over corporate information resources has resulted from the explosive growth in the size, complexity and number of data bases available to...validity, and relevance, and usability of the data that is available. As a result , there has been a growing interest in two tools which .,%... provide

High-contrast imaging of mycobacterium tuberculosis using third-harmonic generation microscopy

NASA Astrophysics Data System (ADS)

Kim, Bo Ram; Lee, Eungjang; Park, Seung-Han

2015-07-01

Nonlinear optical microcopy has become an important tool in investigating biomaterials due to its various advantages such as label-free imaging capabilities. In particular, it has been shown that third-harmonic generation (THG) signals can be produced at interfaces between an aqueous medium (e.g. cytoplasm, interstitial fluid) and a mineralized lipidic surface. In this work, we have demonstrated that label-free high-contrast THG images of the mycobacterium tuberculosis can be obtained using THG microscopy.

The Shock and Vibration Digest. Volume 12, Number 6,

DTIC Science & Technology

1980-06-01

I 20 .. I%25 1.4~ iu±.6 MICROCOPY RESOLUTION TESI CHARI 1 AIIONAL BURtAU Ua SIANDARDS I63 4 i’U 00 SVIC NOTES The weight saving advantages of...34Theoretical and Manifolds by Using Lumped Parameter De - Experimental Investigation of Valve Movement scriptions," J. Sound Vib., 64 (3), pp 387-402 and...COMPUTATIONAL TECHNIQUES work for the textbook through definitions and de - FOR INTERFACE PROBLEMS scriptions of dynamic systems, modeling procedures

Archaeological Test Sampling of Sites within the La Quinta Flood Control Channel Easement,

DTIC Science & Technology

1980-03-01

J L CRAIB MAR 80UNCLASSIFIED DACW@9-80-M-0975 F/G 5/6 NL | EmhhhhhhommhhlmEEIE hhhhhl I E5Ehhhhhhhhlh IIllfllfflfflffllfllf U-IIIIII a J 12 !EM imi.I...ima ii~ti -- I .u 1111125 11114 111116 MICROCOPY RESOLUTION TEST CHART NATIONAL BUR.AU OF STANDARDS-1963- A K- Lo’ • ~ ~ ~ ~ ~ ~ ~ ~ e 4e...66 REFERENCES CITED ............................................... 71 APPENDIX A - Triangulation Points for Site Datum Stakes ........ 73

Estimating the Imputed Social Cost of Errors of Measurement.

DTIC Science & Technology

1983-10-01

social cost of an error of measurement in the score on a unidimensional test, an asymptotic method, based on item response theory, is developed for...11111111 ij MICROCOPY RESOLUTION TEST CHART NATIONAL BUREAU OF STANDARDS-1963-A.5. ,,, I v.P I RR-83-33-ONR 4ESTIMATING THE IMPUTED SOCIAL COST S OF... SOCIAL COST OF ERRORS OF MEASUREMENT Frederic M. Lord This research was sponsored in part by the Personnel and Training Research Programs Psychological

DOE Office of Scientific and Technical Information (OSTI.GOV)

Masih Das, Paul; Danda, Gopinath; Cupo, Andrew

Black phosphorus (BP) is a highly anisotropic allotrope of phosphorus with high promise for fast functional electronics and optoelectronics. We demonstrate that high-resolution and controlled structural modification of few-layer BP along arbitrary crystal direction can be achieved with nanometer-scale precision on a few-minute timescales leading to the formation of sub-nm wide armchair and zigzag BP nanoribbons. The nanoribbons are assembled, along with nanopores and nanogaps, using a combination of mechanical-liquid exfoliation and in situ transmission electron microscope (TEM) and scanning TEM nanosculpting. Here we report time-dependent structural properties of the one-dimensional systems under electron irradiation and probe their oxidation propertiesmore » with electron energy-loss spectroscopy (EELS). Finally, we demonstrate the use of STEM to controllably narrow and thin the nanoribbons until they break into nanogaps. The observations are rationalized using density functional theory for transition state calculations and electronic band-structure evolution for the various stages of the narrowing procedure. In particular, we predict that the sub- and few-nm wide BP nanoribbons realized experimentally possess clear one-dimensional quantum confinement, even when the systems are made up of a few layers. We find the demonstration of this procedure is key for the development of BP-based electronic, optoelectronic, thermoelectric, and other applications in reduced dimensions.« less

Controlled Sculpture of Black Phosphorus Nanoribbons

DOE PAGES

Masih Das, Paul; Danda, Gopinath; Cupo, Andrew; ...

2016-05-18

Black phosphorus (BP) is a highly anisotropic allotrope of phosphorus with high promise for fast functional electronics and optoelectronics. We demonstrate that high-resolution and controlled structural modification of few-layer BP along arbitrary crystal direction can be achieved with nanometer-scale precision on a few-minute timescales leading to the formation of sub-nm wide armchair and zigzag BP nanoribbons. The nanoribbons are assembled, along with nanopores and nanogaps, using a combination of mechanical-liquid exfoliation and in situ transmission electron microscope (TEM) and scanning TEM nanosculpting. Here we report time-dependent structural properties of the one-dimensional systems under electron irradiation and probe their oxidation propertiesmore » with electron energy-loss spectroscopy (EELS). Finally, we demonstrate the use of STEM to controllably narrow and thin the nanoribbons until they break into nanogaps. The observations are rationalized using density functional theory for transition state calculations and electronic band-structure evolution for the various stages of the narrowing procedure. In particular, we predict that the sub- and few-nm wide BP nanoribbons realized experimentally possess clear one-dimensional quantum confinement, even when the systems are made up of a few layers. We find the demonstration of this procedure is key for the development of BP-based electronic, optoelectronic, thermoelectric, and other applications in reduced dimensions.« less

The influence of structure depth on image blurring of micrometres-thick specimens in MeV transmission electron imaging.

PubMed

Wang, Fang; Sun, Ying; Cao, Meng; Nishi, Ryuji

2016-04-01

This study investigates the influence of structure depth on image blurring of micrometres-thick films by experiment and simulation with a conventional transmission electron microscope (TEM). First, ultra-high-voltage electron microscope (ultra-HVEM) images of nanometer gold particles embedded in thick epoxy-resin films were acquired in the experiment and compared with simulated images. Then, variations of image blurring of gold particles at different depths were evaluated by calculating the particle diameter. The results showed that with a decrease in depth, image blurring increased. This depth-related property was more apparent for thicker specimens. Fortunately, larger particle depth involves less image blurring, even for a 10-μm-thick epoxy-resin film. The quality dependence on depth of a 3D reconstruction of particle structures in thick specimens was revealed by electron tomography. The evolution of image blurring with structure depth is determined mainly by multiple elastic scattering effects. Thick specimens of heavier materials produced more blurring due to a larger lateral spread of electrons after scattering from the structure. Nevertheless, increasing electron energy to 2MeV can reduce blurring and produce an acceptable image quality for thick specimens in the TEM. Copyright © 2016 Elsevier Ltd. All rights reserved.

To study the effect of doping concentration of silver on structural and optical properties of cadmium oxide (CdO) nanostructure

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kumar, Rajesh, E-mail: rkkaushik06@gmail.com; Dept. of Physics, Vaish College of Engineering, Rohtak-124001, Haryana; Sharma, Ashwani

The present work deals with study of structural and optical properties of Silver (Ag) doped Cadmium oxide (CdO) nanostructured synthesized by Chemical Co-precipitation Techniques followed by calcinations at small temperature. The doping concentrations were changing from 0.1 to 10 at% respectively. Structural analysis study of these calcined materials is carried out by X-ray diffraction (XRD), Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM). The optical properties of calcined samples were investigating by Fourier transformation infrared (FTIR)spectroscopy, UV-Visible Spectroscopy (UV-Vis). The structural properties analysis results revels that crystallite size are in the range of nano region and TEM results aremore » quite in accordance with XRD results.« less

An ultrahigh vacuum multipurpose specimen chamber with sample introduction system for in situ transmission electron microscopy investigations

NASA Technical Reports Server (NTRS)

Heinemann, K.; Poppa, H.

1986-01-01

A commercial transmission electron microscope (TEM), with flat-plate upper pole piece configuration of the objective lens, and top-entry specimen introduction was modified by introducing an ultrahigh vacuum (UHV) specimen chamber for in situ TEM experimentation. The pumping and design principles and special features of this UHV chamber, which makes it possible to obtain 5 x 10 to the -10th mbar pressure at the site of the specimen, while maintaining the airlock system that allows operation in the 10 to the -10th mbar range within 15 min after specimen change, are described. Design operating pressures and image quality (resolution of metal particles smaller than 1 nm in size) were achieved. Schematic drawings and design dimensions are included.

NASA Astrophysics Data System (ADS)

Wang, Mao-Hua; Zhang, Bo; Zhou, Fu

2014-07-01

Silica was homogeneously coated on the surface of CaCu3Ti4O12 (CCTO) particles via the sol-gel method. The obtained powders were characterized by x-ray diffraction analysis, Fourier-transform infrared spectroscopy, transmission electron microscopy (TEM), energy-dispersive spectroscopy, scanning electron microscopy, and zeta potential analysis. The results demonstrate that there were silica layers on the surface of the CCTO particles. Physical and dielectric properties of silica-coated CCTO were also studied. TEM imaging showed that the thickness of the silica layer on the CCTO particles was about 20 nm to 35 nm. The specimen coated with 1.0 wt.% silica showed the maximum relative density of 96.7% with high dielectric constant (12.78 × 104) and low dielectric loss (0.005) at 20°C after sintering at 1000°C for 6 h.

Evolution of the magnesium incorporated amorphous calcium phosphate to nano-crystallized hydroxyapatite in alkaline solution

NASA Astrophysics Data System (ADS)

Zhang, Xiao-Juan; Lin, Dong-Yang; Yan, Xiao-Hui; Wang, Xiao-Xiang

2011-12-01

A homogeneous amorphous calcium phosphate (ACP) coating containing magnesium was achieved on titanium substrates by electrochemical deposition (ECD). Its amorphous structure is confirmed by transmission electron microscope (TEM) together with grazing reflection absorption infrared spectroscopy (IR) spectrometer. In the images of high-resolution transmission electron microscope (HRTEM), the ACP spheres are assembled by nano-particles with the diameter of 5-10 nm. In the alkaline environment, nucleation of hydroxyapatite (HAP) occurs on the surfaces of ACP spheres. By consuming the Ca and PO 4 ions inside the ACP spheres, the HAP nuclei grow outward. Confirmed by TEM, the ACP spheres converse to hollow HAP spheres composed of HAP nano-needles. The coating is finally constructed by the HAP nano-needles, which are themselves aggregated by numerous nano-particles.

Hydroxyapatite nanocrystals: simple preparation, characterization and formation mechanism.

PubMed

Mohandes, Fatemeh; Salavati-Niasari, Masoud; Fathi, Mohammadhossein; Fereshteh, Zeinab

2014-12-01

Crystalline hydroxyapatite (HAP) nanoparticles and nanorods have been successfully synthesized via a simple precipitation method. To control the shape and particle size of HAP nanocrystals, coordination ligands derived from 2-hydroxy-1-naphthaldehyde were first prepared, characterized by Fourier transform infrared (FT-IR) and proton nuclear magnetic resonance ((1)H-NMR) spectroscopies, and finally applied in the synthesis process of HAP. On the other hand, the HAP nanocrystals were also characterized by several techniques including powder X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). According to the FE-SEM and TEM micrographs, it was found that the morphology and crystallinity of the HAP powders depended on the coordination mode of the ligands. Copyright © 2014 Elsevier B.V. All rights reserved.

Development of regenerated cellulose/halloysites nanocomposites via ionic liquids.

PubMed

Hanid, Nurbaiti Abdul; Wahit, Mat Uzir; Guo, Qipeng; Mahmoodian, Shaya; Soheilmoghaddam, Mohammad

2014-01-01

In this study, regenerated cellulose/halloysites (RC/HNT) nanocomposites with different nanofillers loading were fabricated by dissolving the cellulose in 1-ethyl-3-methylimidazolium chloride (EMIMCl) ionic liquid. The films were prepared via solution casting method and were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The mechanical properties were investigated by tensile testing. It clearly displayed a good enhancement of both tensile strength and Young's modulus with HNT loading up to 5 wt%. As the HNT loadings increased to 5 wt%, the thermal behaviour and water resistance rate was also increased. The TEM and SEM images also depicted even dispersion of the HNT and a good intertubular interaction between the HNT and the cellulose matrix. Copyright © 2013 Elsevier Ltd. All rights reserved.

Synthesis and characterization of dextran-coated iron oxide nanoparticles

NASA Astrophysics Data System (ADS)

Predescu, Andra Mihaela; Matei, Ecaterina; Berbecaru, Andrei Constantin; Pantilimon, Cristian; Drăgan, Claudia; Vidu, Ruxandra; Predescu, Cristian; Kuncser, Victor

2018-03-01

Synthesis and characterization of iron oxide nanoparticles coated with a large molar weight dextran for environmental applications are reported. The first experiments involved the synthesis of iron oxide nanoparticles which were coated with dextran at different concentrations. The synthesis was performed by a co-precipitation technique, while the coating of iron oxide nanoparticles was carried out in solution. The obtained nanoparticles were characterized by using scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction spectrometry, Fourier transform infrared spectroscopy and superconducting quantum interference device magnetometry. The results demonstrated a successful coating of iron oxide nanoparticles with large molar weight dextran, of which agglomeration tendency depended on the amount of dextran in the coating solution. SEM and TEM observations have shown that the iron oxide nanoparticles are of about 7 nm in size.

Electron Microscopy of Ebola Virus-Infected Cells.

PubMed

Noda, Takeshi

2017-01-01

Ebola virus (EBOV) replicates in host cells, where both viral and cellular components show morphological changes during the process of viral replication from entry to budding. These steps in the replication cycle can be studied using electron microscopy (EM), including transmission electron microscopy (TEM) and scanning electron microscopy (SEM), which is one of the most useful methods for visualizing EBOV particles and EBOV-infected cells at the ultrastructural level. This chapter describes conventional methods for EM sample preparation of cultured cells infected with EBOV.

Transmission Electron Microscope Measures Lattice Parameters

NASA Technical Reports Server (NTRS)

Pike, William T.

1996-01-01

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

Ponderomotive phase plate for transmission electron microscopes

DOEpatents

Reed, Bryan W [Livermore, CA

2012-07-10

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

Growth and Electronic Structure of Heusler Compounds for Use in Electron Spin Based Devices

DTIC Science & Technology

2015-06-01

either Co– or MnSi– initiated films on c(4x4) GaAs. Studies using x - ray photoemission spectroscopy (XPS), STM/STS, and transmission electron microscopy...Co– or MnSi– initiated films on c(4x4) GaAs. Studies using x - ray photoemission spectroscopy (XPS), STM/STS, and transmission electron microscopy (TEM...diagram of the Palmstrøm lab in-situ growth and char- acterization setup, with 6 MBE growth chambers, 3 scanning probe microscopes, an x - ray

Scanning and transmission electron microscopic observations of the acute morphological response of the mouse urinary bladder to 4-ethylsulfonylnaphthalene-1-sulfonamide.

PubMed

Frith, C H; Ayres, P H; Shinohara, Y; West, R

1986-01-01

A total of 75 BALB/cStCrlfC3H/Nctr male weanling mice were administered either 0 or 250 ppm of 4 ethylsulfonylnaphthalene-1-sulfonamide (ENS) in the diet for periods up to 14 days to evaluate the early morphological changes of the transitional epithelium of the urinary bladder with scanning (SEM) and transmission (TEM) electron microscopy. Primary TEM changes included hyperplasia of the epithelium, loosening of the intercellular junctions, autophagic vacuoles and electron dense granules in the mitochondria. Primary SEM changes included sloughing of epithelial cells, irregularity in the size and shape of the transitional epithelial cells and the presence of microvilli. Although pleomorphic microvilli were present after only three days of treatment with ENS, it appears that they are a transient observation in a series of morphological changes. The reversibility or transient nature of the pleomorphic microvilli may indicate that they are an acute toxic response and may not necessarily indicate a preneoplastic change.

Tem Observation of Precipitates in Ag-Added Al-Mg-Si Alloys

NASA Astrophysics Data System (ADS)

Nagai, Takeshi; Matsuda, Kenji; Nakamura, Junya; Kawabata, Tokimasa; Marioara, Calin; Andersen, Sigmund J.; Holmestad, Randi; Hirosawa, Shoichi; Horita, Zenji; Terada, Daisuke; Ikeno, Susumu

The influence of addition of the small amount of transition metals to Al-Mg-Si alloy had reported by many researchers. In the previous our work, β' phase in alloys Al — 1.0 mass% Mg2Si -0.5 mass% Ag (Ag-addition) and Al -1.0 mass% Mg2Si (base) were investigated by high resolution transmission electron microscopy (HRTEM) and selected area electron diffraction (SAED), in order to understand the effect of Ag. In addition, the distribution of Ag was investigated by energy filtered mapping and high annular angular dark field scanning transmission electron microscopy (HAADF-STEM). One Ag-containing atomic column was observed per β' unit cell, and the unit cell symmetry is slightly changed as compared with the Ag-free β'. In this work, the microstructure of G.P. zone and β'' phase was investigated by TEM observation, which were formed before β' phase. The deformed sample by high pressure torsion (HPT) technique before aging was also investigated to understand its effect for aging in this alloy.

The use of castor oil and ricinoleic acid in lead chalcogenide nanocrystal synthesis

NASA Astrophysics Data System (ADS)

Kyobe, Joseph W. M.; Mubofu, Egid B.; Makame, Yahya M. M.; Mlowe, Sixberth; Revaprasadu, Neerish

2016-08-01

A green solution-based thermolysis method for the synthesis of lead chalcogenide (PbE, E = S, Se, Te) nanocrystals in castor oil (CSTO) and its isolate ricinoleic acid (RA) is described. The blue shift observed from the optical spectra of CSTO and RA-capped PbE nanocrystals (NCs) confirmed the evidence of quantum confinement. The dimensions of PbE NCs obtained from NIR absorption spectra, transmission electron microscopy (TEM), and X-ray diffraction (XRD) studies were in good agreement. The particle sizes estimated were in the range of 20, 25, and 130 nm for castor oil-capped PbS, PbSe, and PbTe, respectively. Well-defined close to cubic-shaped particles were observed in the scanning electron microscopy (SEM) images of PbSe and PbTe nanocrystals. The high-resolution TEM and selective area electron diffraction (SAED) micrographs of the as-synthesized crystalline PbE NCs showed distinct lattice fringes with d-spacing distances corroborating with the standard values reported in literature.

Visible cathodoluminescence of Er ions in β-Ga(2)O(3) nanowires and microwires.

PubMed

Nogales, E; Méndez, B; Piqueras, J

2008-01-23

Erbium doped β-Ga(2)O(3) nanowires and microwires have been obtained by a vapour-solid process from an initial mixture of Ga(2)O(3) and Er(2)O(3) powders. X-ray diffraction (XRD) analysis reveals the presence of erbium gallium garnet as well as β-Ga(2)O(3) phases in the microwires. Scanning electron microscopy (SEM) images show that the larger microwires have a nearly rectangular cross-section. Transmission electron microscopy (TEM) and high-resolution TEM (HRTEM) analysis show good crystal quality of the β-Ga(2)O(3) nanowires. The nanostructures have been studied by means of the cathodoluminescence technique in the scanning electron microscope. Er intraionic blue, green and red emission lines are observed in luminescence spectra even at room temperature, which confirms the optical activity of the rare earth ions in the grown structures. Mapping of the main 555 nm emission intensity shows a non-homogeneous distribution of Er ions in the microstructures.

Microstructural Study of Micron-Sized Craters Simulating Stardust Impacts in Aluminum 1100 Targets

NASA Technical Reports Server (NTRS)

Leroux, Hugues; Borg, Janet; Troadec, David; Djouadi, Zahia; Horz, Friedrich

2006-01-01

Various microscopic techniques were used to characterize experimental micro- craters in aluminium foils to prepare for the comprehensive analysis of the cometary and interstellar particle impacts in aluminium foils to be returned by the Stardust mission. First, SEM (Scanning Electron Microscopy) and EDS (Energy Dispersive X-ray Spectroscopy) were used to study the morphology of the impact craters and the bulk composition of the residues left by soda-lime glass impactors. A more detailed structural and compositional study of impactor remnants was then performed using TEM (Transmission Electron Microscopy), EDS, and electron diffraction methods. The TEM samples were prepared by Focused Ion Beam (FIB) methods. This technique proved to be especially valuable in studying impact crater residues and impact crater morphology. Finally, we also showed that InfraRed microscopy (IR) can be a quick and reliable tool for such investigations. The combination of all of these tools enables a complete microscopic characterization of the craters.

Synthesis and characterization of bovine femur bone hydroxyapatite containing silver nanoparticles for the biomedical applications

NASA Astrophysics Data System (ADS)

Nirmala, R.; Sheikh, Faheem A.; Kanjwal, Muzafar A.; Lee, John Hwa; Park, Soo-Jin; Navamathavan, R.; Kim, Hak Yong

2011-05-01

Bovine femur bone hydroxyapatite (HA) containing silver (Ag) nanoparticles was synthesized by thermal decomposition method and subsequent reduction of silver nitrate with N, N-dimethylformamide (DMF) in the presence of poly(vinylacetate) (PVAc). The structural, morphological, and chemical properties of the HA-Ag nanoparticles were characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), and X-ray photoelectron spectroscopy (XPS). TEM images showed that the Ag nanoparticles with size ranging from 8 to 20 nm and were arranged at the periphery of HA crystals. Bactericidal activity of HA-Ag with different concentration of Ag nanoparticles immobilized on the surface of HA was investigated against gram-positive Staphylococcus aureus ( S. aureus, non-MRSA), Methicillin resistant S. aureus (MRSA) and gram-negative Escherichia coli ( E. coli) by the disc diffusion susceptibility test. The HA-Ag nanoparticles showed that broad spectrum activity against non-MRSA, MRSA, and E. coli bacterial strains.

Hydrothermal-reduction synthesis of manganese oxide nanomaterials for electrochemical supercapacitors.

PubMed

Zhang, Xiong; Chen, Yao; Yu, Peng; Ma, Yanwei

2010-11-01

In the present work, amorphous manganese oxide nanomaterials have been synthesized by a common hydrothermal method based on the redox reaction between MnO4(-) and Fe(2+) under an acidic condition. The synthesized MnO2 samples were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), and electrochemical studies. XRD results showed that amorphous manganese oxide phase was obtained. XPS quantitative analysis revealed that the atomic ratio of Mn to Fe was 3.5 in the MnO2 samples. TEM images showed the porous structure of the samples. Electrochemical properties of the MnO2 electrodes were studied using cyclic voltammetry and galvanostatic charge-discharge cycling in 1 M Na2SO4 aqueous electrolyte, which showed excellent pseudocapacitance properties. A specific capacitance of 192 Fg(-1) at a current density of 0.5 Ag(-1) was obtained at the potential window from -0.1 to 0.9 V (vs. SCE).

Microstructural characterization of AA5183 aluminum clad AISI 1018 steel prepared by electro spark deposition

NASA Astrophysics Data System (ADS)

Rastkerdar, E.; Aghajani, H.; Kianvash, A.; Sorrell, C. C.

2018-04-01

The application of a simple and effective technique, electro spark deposition (ESD), to create aluminum clad steel plate has been studied. AA5183 aluminum rods were used as the rotating electrode for cladding of the AISI 1018 steel. The microstructure of the interfacial zone including the intermetallic compounds (IMC) layer and the clad metal have been investigated by scanning electron microscopy (SEM) equipped with energy dispersive spectroscopy (EDS) and transmission electron microscopy (TEM and STEM). According to the results sound aluminum clad with thickness up to 25–30 μm can be achieved. Very thin (<4 μm) IMC layer was formed at the Al/Fe interface and the structural (electron diffraction pattern) and chemical analysis (STEM) conducted by TEM confirmed that the layer is constituted of Fe rich phases, both implying a much improved mechanical properties. Investigation of the orientations of phases at the interfacial zone confirmed absence of any preferred orientation.

Correlation study of nanocrystalline carbon doped thin films prepared by a thermionic vacuum arc deposition technique

NASA Astrophysics Data System (ADS)

Dinca-Balan, Virginia; Vladoiu, Rodica; Mandes, Aurelia; Prodan, Gabriel

2017-11-01

The synthesis of Ag, Mg and Si nanocrystalline, embedded in a hydrogen-free amorphous carbon (a-C) matrix, deposited by a high vacuum and free buffer gas technique, were investigated. The films with compact structures and extremely smooth surfaces were prepared using the thermionic vacuum arc method in one electron gun configuration, on glass and silicon substrates. The surface morphology and wettability of the obtained multifunctional thin films were investigated using transmission electron microscopy (TEM), scanning electron microscopy (SEM) and free surface energy (FSE) by See System. The results from the TEM measurements show how the Ag, Mg and Si interacted with carbon and the influence these materials have on the thin film structure formation and the grain size distribution. SEM correlated with EDX results reveal a very precise comparative study, regarding the quantity of the elements that morphed into carbides nanostructures. Also, the FSE results prove how different materials in combination with carbon can make changes to the surface properties.

Morphological and Microstructural Evolution of Phosphorous-Rich Layer in SnAgCu/Ni-P UBM Solder Joint

NASA Astrophysics Data System (ADS)

Lin, Yung-Chi; Shih, Toung-Yi; Tien, Shih-Kang; Duh, Jenq-Gong

2007-11-01

Interfacial morphologies and microstructure of Sn-3Ag-0.5Cu/Ni-P under bump metallization (UBM) with various phosphorous contents were investigated by transmission electron microscope (TEM) and field emission electron probe microanalyzer (FE-EPMA). It was revealed that as the Ni-Sn-P compound was formed between the solder matrix and Ni-P UBM, the conventionally so-called phosphorous-rich (P-rich) layer was transformed to a series of layer compounds, including Ni3P, Ni12P5 and Ni2P. The relationship between Ni-Sn-P formation and evolution of P-rich layers was probed by electron microscopic characterization with the aid of the phase diagram of Ni-P. On the basis of the TEM micrograph, the selected area diffraction (SAD) pattern, and the FE-EPMA results, the detailed phase evolution of P-rich layers in the SnAgCu/Ni-P joint was revealed and proposed.

Copper silicide/silicon nanowire heterostructures: in situ TEM observation of growth behaviors and electron transport properties.

PubMed

Chiu, Chung-Hua; Huang, Chun-Wei; Chen, Jui-Yuan; Huang, Yu-Ting; Hu, Jung-Chih; Chen, Lien-Tai; Hsin, Cheng-Lun; Wu, Wen-Wei

2013-06-07

Copper silicide has been studied in the applications of electronic devices and catalysts. In this study, Cu3Si/Si nanowire heterostructures were fabricated through solid state reaction in an in situ transmission electron microscope (TEM). The dynamic diffusion of the copper atoms in the growth process and the formation mechanism are characterized. We found that two dimensional stacking faults (SF) may retard the growth of Cu3Si. Due to the evidence of the block of edge-nucleation (heterogeneous) by the surface oxide, center-nucleation (homogeneous) is suggested to dominate the silicidation. Furthermore, the electrical transport properties of various silicon channel length with Cu3Si/Si heterostructure interfaces and metallic Cu3Si NWs have been investigated. The observations not only provided an alternative pathway to explore the formation mechanisms and interface properties of Cu3Si/Si, but also suggested the potential application of Cu3Si at nanoscale for future processing in nanotechnology.

Synthesis and characterization of Ag@polycarbazole coaxial nanocables and their enhanced dispersion behavior

NASA Astrophysics Data System (ADS)

Zahoor, Ahmad; Teng, Qiu; Wang, Haiqiao; Choudhry, M. A.; Li, Xiaoyu

2011-06-01

Ag@polycarbazole coaxial nanocables (CNCs) have been successfully fabricated by the oxidative polymerization of carbazole over Ag nanowires (NWs) in acetonitrile. The morphology of Ag NWs and CNCs was studied by employing a transmission electron microscope (TEM) and a scanning electron microscope (SEM), which showed them to be a monodisperse material. The thickness of the polymer sheath was found to be 5 nm to 8 nm by observation under a high-resolution transmission electron microscope (HR-TEM). Energy dispersive X-ray spectroscopy (EDS), FT-IR and Raman measurements were used to characterize the polymer sheath, which demonstrated it to be a carbon material in polycarbazole form. X-ray photoelectron spectroscopy (XPS) was used for an interfacial study, which revealed that Ag surface atoms remained intact during polymer growth. In the end, zeta potential showed that the dispersion stability of Ag NWs increased due to polymer encapsulation, which is significant to obtain a particular alignment for anisotropic measurement of electrical conductivity.

Green synthesis of gold nanoparticles using aqueous extract of Dillenia indica

NASA Astrophysics Data System (ADS)

Sett, Arghya; Gadewar, Manoj; Sharma, Pragya; Deka, Manab; Bora, Utpal

2016-06-01

In this study, we report a novel method of gold nanoparticle (AuNP) synthesis using aqueous fruit extract of Dillenia indica. The phytochemicals present in the fruit extract act as an effective reducing and capping agent to synthesize AuNPs. The synthesized AuNPs were characterized by spectrophotometry, transmission electron microscopy (TEM), x-ray diffraction (XRD), and Fourier transform infrared (FTIR) spectroscopy. TEM studies revealed the particles of various sizes and mainly spherical in shape. Selected-area electron diffraction (SAED) patterns and high-resolution transmission electron microscopy (HRTEM) images confirmed the crystallinity of the particles. The XRD patterns showed peaks at (111), (200), (220) which exhibited preferential orientation of the AuNPs as face-centered cubic crystal. FTIR measurements confirmed the coating of phenolic compounds on the AuNPs indicating a possible role of biomolecules for the capping and efficient stabilization of the AuNPs. The synthesized AuNPs did not show any form of cytotoxicity in the normal fibroblast cell line L929.

Characterization of some biological specimens using TEM and SEM

NASA Astrophysics Data System (ADS)

Ghosh, Nabarun; Smith, Don W.

2009-05-01

The advent of novel techniques using the Transmission and Scanning Electron Microscopes improved observation on various biological specimens to characterize them. We studied some biological specimens using Transmission and Scanning Electron Microscopes. We followed negative staining technique with Phosphotungstic acid using bacterial culture of Bacillus subtilis. Negative staining is very convenient technique to view the structural morphology of different samples including bacteria, phage viruses and filaments in a cell. We could observe the bacterial cell wall and flagellum very well when trapped the negative stained biofilm from bacterial culture on a TEM grid. We cut ultra thin sections from the fixed root tips of Pisum sativum (Garden pea). Root tips were pre fixed with osmium tetroxide and post fixed with uranium acetate and placed in the BEEM capsule for block making. The ultrathin sections on the grid under TEM showed the granular chromatin in the nucleus. The protein bodies and large vacuoles with the storage materials were conspicuous. We followed fixation, critical point drying and sputter coating with gold to view the tissues with SEM after placing on stubs. SEM view of the leaf surface of a dangerous weed Tragia hispida showed the surface trichomes. These trichomes when break on touching releases poisonous content causing skin irritation. The cultured tissue from in vitro culture of Albizia lebbeck, a tree revealed the regenerative structures including leaf buds and stomata on the tissue surface. SEM and TEM allow investigating the minute details characteristic morphological features that can be used for classroom teaching.

Structural and morphological study of Zn0.9Mn0.05Fe0.05O synthesized by sol-gel wet chemical precipitation route

NASA Astrophysics Data System (ADS)

Jain, S. K.; Dolia, S. N.; Choudhary, B. L.; Prashant, B. L.

2018-04-01

Transition metal substituted Zinc oxide (ZnO) has drawn a great deal of attention due to its excellent properties. Zn0.9Mn0.05Fe0.05O sample synthesized was by Sol-gel wet chemical precipitation route at temperature 350°C. The crystallinity and the structure of Zn0.9Mn0.05Fe0.05O was determined by X-ray diffraction by Cu-Kα radiations operated at 40kV and 35mA in the range of 20° to 80°. The pattern gets indexed in wurtzite (hexagonal) structure with lattice constants a=b=3.2525Å and c=5.2071Å and approves the single phase material with no impurity. The values of particle size assessed by Debye Scherer’s (DS) formula lie in the range of 13nm to 33nm indicating the nano-crystalline nature of the sample. The morphological analysis of the sample was performed by Scanning electron microscopy (SEM) and Transmission electron microscopy (TEM) measurements. The observed size of Zn0.9Mn0.05Fe0.05O nanoparticles by TEM micrograph exhibits the similar trend with the size calculated by Debye-Scherer formula. TEM image show the irregular shape of the nanoparticles and particle size lies in the range of 10-35nm. Similar to SEM image, the slight agglomeration of the nanoparticles have been observed from TEM.

Simple route to (NH4)xWO3 nanorods for near infrared absorption

NASA Astrophysics Data System (ADS)

Guo, Chongshen; Yin, Shu; Dong, Qiang; Sato, Tsugio

2012-05-01

Described here is how to synthesize one-dimensional ammonium tungsten bronze ((NH4)xWO3) by a facile solvothermal approach in which ethylene glycol and acetic acid were employed as solvents and ammonium paratungstate was used as a starting material, as well as how to develop the near infrared absorption properties of (NH4)xWO3 nanorods for application as a solar light control filter. The as-obtained product was characterized by field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), thermogravimetry (TG), atomic force microscope (AFM) and UV-Vis-NIR spectra. The SEM and TEM images clearly revealed that the obtained sample possessed rod/fiber-like morphologies with diameters around 120 nm. As determined by UV-Vis-NIR optical measurement, the thin film consisted of (NH4)xWO3 nanoparticles, which can selectively transmit most visible lights, but strongly absorb the near-infrared (NIR) lights and ultraviolet rays. These interesting optical properties make the (NH4)xWO3 nanorods suitable for the solar control windows.Described here is how to synthesize one-dimensional ammonium tungsten bronze ((NH4)xWO3) by a facile solvothermal approach in which ethylene glycol and acetic acid were employed as solvents and ammonium paratungstate was used as a starting material, as well as how to develop the near infrared absorption properties of (NH4)xWO3 nanorods for application as a solar light control filter. The as-obtained product was characterized by field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), thermogravimetry (TG), atomic force microscope (AFM) and UV-Vis-NIR spectra. The SEM and TEM images clearly revealed that the obtained sample possessed rod/fiber-like morphologies with diameters around 120 nm. As determined by UV-Vis-NIR optical measurement, the thin film consisted of (NH4)xWO3 nanoparticles, which can selectively transmit most visible lights, but strongly absorb the near-infrared (NIR) lights and ultraviolet rays. These interesting optical properties make the (NH4)xWO3 nanorods suitable for the solar control windows. Electronic supplementary information (ESI) available. See DOI: 10.1039/c2nr30612c

A Chemical and Structural Study of the A1N-Si Interface

NASA Technical Reports Server (NTRS)

George, T.; Beye, R.

1997-01-01

Samples of A1N grown on silicon [111] subtrates were examined using electron enery loss spectroscopy (EELS) and selected area diffraction (SAD) with high-resolution transmission electron microscopy (TEM) to determine the source of out-of-place tilts and in-plane rotations of the A1N crystallites at the Si interface.

Transfer and alignment of random single-walled carbon nanotube films by contact printing.

PubMed

Liu, Huaping; Takagi, Daisuke; Chiashi, Shohei; Homma, Yoshikazu

2010-02-23

We present a simple method to transfer large-area random single-walled carbon nanotube (SWCNT) films grown on SiO(2) substrates onto another surface through a simple contact printing process. The transferred random SWCNT films can be assembled into highly ordered, dense regular arrays with high uniformity and reproducibility by sliding the growth substrate during the transfer process. The position of the transferred SWCNT film can be controlled by predefined patterns on the receiver substrates. The process is compatible with a variety of substrates, and even metal meshes for transmission electron microscopy (TEM) can be used as receiver substrates. Thus, suspended web-like SWCNT networks and aligned SWCNT arrays can be formed over the grids of TEM meshes, so that the structures of the transferred SWCNTs can be directly observed by TEM. This simple technique can be used to controllably transfer SWCNTs for property studies, for the fabrication of devices, or even as support films for TEM meshes.

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Van Renterghem, W.; Leenaers, A.; Van den Berghe, S.

2015-10-01

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

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

NASA Astrophysics Data System (ADS)

Yano, K. H.; Swenson, M. J.; Wu, Y.; Wharry, J. P.

2017-01-01

The growing role of charged particle irradiation in the evaluation of nuclear reactor candidate materials requires the development of novel methods to assess mechanical properties in near-surface irradiation damage layers just a few micrometers thick. In situ transmission electron microscopic (TEM) mechanical testing is one such promising method. In this work, microcompression pillars are fabricated from a Fe2+ ion irradiated bulk specimen of a model Fe-9%Cr oxide dispersion strengthened (ODS) alloy. Yield strengths measured directly from TEM in situ compression tests are within expected values, and are consistent with predictions based on the irradiated microstructure. Measured elastic modulus values, once adjusted for the amount of deformation and deflection in the base material, are also within the expected range. A pillar size effect is only observed in samples with minimum dimension ≤100 nm due to the low inter-obstacle spacing in the as received and irradiated material. TEM in situ micropillar compression tests hold great promise for quantitatively determining mechanical properties of shallow ion-irradiated layers.

Artifacts introduced by ion milling in Al-Li-Cu alloys.

PubMed

Singh, A K; Imam, M A; Sadananda, K

1988-04-01

Ion milling is commonly used to prepare specimens for observation under transmission electron microscope (TEM). This technique sometimes introduces artifacts in specimens contributing to misleading interpretation of TEM results as observed in the present investigation of Al-Li-Cu alloys. This type of alloy, in general, contains several kinds of precipitates, namely delta', T1, and theta'. It is found that ion milling even for a short time produces drastic changes in the precipitate characteristics as compared to standard electropolishing methods of specimen preparation for TEM. Careful analysis of selected area diffraction patterns and micrographs shows that after ion milling delta' precipitates are very irregular, whereas other precipitates coarsen and they are surrounded by misfit dislocations. In situ hot-stage TEM experiments were performed to relate the microstructure to that observed in the ion-milled specimen. Results and causes of ion milling effects on the microstructure are discussed in relation to standard electropolishing techniques and in situ hot-stage experiment.

GISAXS modelling of helium-induced nano-bubble formation in tungsten and comparison with TEM

NASA Astrophysics Data System (ADS)

Thompson, Matt; Sakamoto, Ryuichi; Bernard, Elodie; Kirby, Nigel; Kluth, Patrick; Riley, Daniel; Corr, Cormac

2016-05-01

Grazing-incidence small angle x-ray scattering (GISAXS) is a powerful non-destructive technique for the measurement of nano-bubble formation in tungsten under helium plasma exposure. Here, we present a comparative study between transmission electron microscopy (TEM) and GISAXS measurements of nano-bubble formation in tungsten exposed to helium plasma in the Large Helical Device (LHD) fusion experiment. Both techniques are in excellent agreement, suggesting that nano-bubbles range from spheroidal to ellipsoidal, displaying exponential diameter distributions with mean diameters μ=0.68 ± 0.04 nm and μ=0.6 ± 0.1 nm measured by TEM and GISAXS respectively. Depth distributions were also computed, with calculated exponential depth distributions with mean depths of 8.4 ± 0.5 nm and 9.1 ± 0.4 nm for TEM and GISAXS. In GISAXS modelling, spheroidal particles were fitted with an aspect ratio ε=0.7 ± 0.1. The GISAXS model used is described in detail.

Direct Observation Through In Situ Transmission Electron Microscope of Early States of Crystallization in Nanoscale Metallic Glasses

NASA Astrophysics Data System (ADS)

Xie, Y.; Sohn, S.; Schroers, J.; Cha, J. J.

2017-11-01

Crystallization is a complex process that involves multiscale physics such as diffusion of atomic species over multiple length scales, thermodynamic energy considerations, and multiple possible intermediate states. In situ crystallization experiments inside a transmission electron microscope (TEM) using nanostructured metallic glasses (MGs) provide a unique platform to study directly crystallization kinetics and pathways. Here, we study the embryonic state of eutectic growth using Pt-Ni-Cu-P MG nanorods under in situ TEM. We directly observe the nucleation and growth of a Ni-rich polymorphic phase, followed by the nucleation and slower growth of a Cu-rich phase. The suppressed growth kinetics of the Cu-rich phase is attributed to locally changing chemical compositions. In addition, we show that growth can be controlled by incorporation of an entire nucleus instead of individual atoms. Such a nucleus has to align with the crystallographic orientation of a larger grain before it can be incorporated into the crystal. By directly observing the crystallization processes, particularly the early stages of non-polymorphic growth, in situ TEM crystallization studies of MG nanostructures provide a wealth of information, some of which can be applied to typical bulk crystallization.

Structural, magnetic and electronic structural properties of Mn doped CeO2 nanoparticles

NASA Astrophysics Data System (ADS)

Kumari, Kavita; Vij, Ankush; Hashim, Mohd.; Chae, K. H.; Kumar, Shalendra

2018-05-01

Nanoparticles of Ce1-xMnxO2, (x=0.0, 0.01, and 0.05) have been synthesized by using co-precipitation method, and then characterized by x-ray diffraction (XRD), transmission electron microscopy (TEM), near edge x-ray absorption fine structure (NEXAFS) spectroscopy and dc magnetization measurements. XRD results clearly showed that the all the samples have single phase nature and exclude the presence of any secondary phase. The average particle size calculated using XRD TEM measurements found to decrease with increase in Mn doping in the range of 4.0 - 9.0 nm. The structural parameters such as strain, interplaner distance and lattice parameter is observed to decrease with increase in doping. The morphology of Ce1-xMnxO2 nanoparticles measured using TEM micrographs indicate that nanoparticle have spherical shape morphology. Magnetic hysteresis curve for Ce1-xMnxO2, (x = 0.0, 0.01, and 0.05) confirms the ferromagnetic ordering room temperature. The value of saturation magnetization is observed to decrease with increase in temperature from 10 K to 300 K. The NEXAFS spectra measured at Ce M4,5 edge reveals that Ce-ions are in +4 valance state.

Effects of the environmental factors on the casein micelle structure studied by cryo transmission electron microscopy and small-angle x-ray scattering/ultrasmall-angle x-ray scattering

NASA Astrophysics Data System (ADS)

Marchin, Stéphane; Putaux, Jean-Luc; Pignon, Frédéric; Léonil, Joëlle

2007-01-01

Casein micelles are colloidal protein-calcium-transport complexes whose structure has not been unequivocally elucidated. This study used small-angle x-ray scattering (SAXS) and ultrasmall angle x-ray scattering (USAXS) as well as cryo transmission electron microscopy (cryo-TEM) to provide fine structural details on their structure. Cryo-TEM observations of native casein micelles fractionated by differential centrifugation showed that colloidal calcium phosphate appeared as nanoclusters with a diameter of about 2.5nm. They were uniformly distributed in a homogeneous tangled web of caseins and were primarily responsible for the intensity distribution in the SAXS profiles at the highest q vectors corresponding to the internal structure of the casein micelles. A specific demineralization of casein micelles by decreasing the pH from 6.7 to 5.2 resulted in a reduced granular aspect of the micelles observed by cryo-TEM and the existence of a characteristic point of inflection in SAXS profiles. This supports the hypothesis that the smaller substructures detected by SAXS are colloidal calcium phosphate nanoclusters rather than putative submicelles.

Microstructural analysis of 800H steel exposed at test operation in HTHL by using FIB-SEM and HRTEM techniques

NASA Astrophysics Data System (ADS)

Marušáková, Daniela; Bublíková, Petra; Berka, Jan; Vávrovcová, Zuzana; Burda, Jaroslav

2017-09-01

To understand the degradation process of metal materials which are used in power engineering, appropriate evaluation procedure is necessary to ensure. In that order, the degradation of alloy 800H during the first period of test operation in High Temperature Helium Loop (HTHL) was tested. Experiment was carried out in atmosphere of pure technical helium with purity 4.6 containing only residual concentration of moisture up to 300 vppm. Parameters during the operation test were not constant, process was interrupted several times. The maximum temperature on specimens during this period was 750 °C, average temperature was 460 °C, gas pressure ranged from 3 to 6 MPa and gas flow from 3 to 9 gs-1. Total duration of the test was 264 h. After the exposure the degradation of specimens was investigated by Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM). Using the technique of Focused Ion Beam (FIB) integrated within SEM the transparent samples with quality surface parameters were obtained for TEM analysis. FIB technique in combination with High Resolution TEM ensured the guaranteed methodology of exposed sample preparation and precise description of changes in this kind of material.

Microstructural change in electroformed copper liners of shaped charges upon plastic deformation at ultra-high strain rate

NASA Astrophysics Data System (ADS)

Tian, W. H.; Hu, S. L.; Fan, A. L.; Wang, Z.

2002-01-01

Transmission electron microscopy (TEM) observations were carried out for examining the as-formed and post-deformed microstructures in a variety of electroformed copper liners of shaped charges. The deformation was carried out at an ultra-high strain rate. Specifically, the electron backscattering Kikuchi pattern (EBSP) technique was utilized to examine the micro-texture of these materials. TEM observations revealed that these electroformed copper liners of shaped charges have a grain size of about 1-3 mum, EBSP analysis demonstrated that the as-grown copper liners of shaped charges exhibit a l 10) fiber micro-texture which is parallel to the normal direction of the surface of the liners of shaped charges. Having undergone plastic deformation at ultra-high strain rate (10(7) s(-1)), the specimens which were recovered from the copper slugs were found to have grain size of the same order as that before deformation. EBSP analysis revealed that the (110) fiber texture existed in the as-formed copper liners disappears in the course of deformation. TEM examination results indicate that dynamic recovery and recrystallization play a significant role in this deformation process.

Microstructural observation of fuel cell catalyst inks by Cryo-SEM and Cryo-TEM.

PubMed

Shimanuki, Junichi; Takahashi, Shinichi; Tohma, Hajime; Ohma, Atsushi; Ishihara, Ayumi; Ito, Yoshiko; Nishino, Yuri; Miyazawa, Atsuo

2017-06-01

In order to improve the electricity generation performance of fuel cell electric vehicles, it is necessary to optimize the microstructure of the catalyst layer of a polymer electrolyte fuel cell. The catalyst layer is formed by a wet coating process using catalyst inks. Therefore, it is very important to observe the microstructure of the catalyst ink. In this study, the morphology of carbon-supported platinum (Pt/C) particles in catalyst inks with a different solvent composition was investigated by cryogenic scanning electron microscopy (cryo-SEM). In addition, the morphology of the ionomer, which presumably influences the formation of agglomerated Pt/C particles in a catalyst ink, was investigated by cryogenic transmission electron microscopy (cryo-TEM). The results of a cryo-SEM observation revealed that the agglomerated Pt/C particles tended to become coarser with a higher 1-propanol (NPA) weight fraction. The results of a cryo-TEM observation indicated that the actual ionomer dispersion in a catalyst ink formed a network structure different from that of the ionomer in the solvent. © The Author 2017. 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.

Green synthesis and characterization of graphene nanosheets

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tavakoli, Farnosh; Salavati-Niasari, Masoud, E-mail: salavati@kashanu.ac.ir; Department of Inorganic Chemistry, Faculty of Chemistry, University of Kashan, Kashan, P. O. Box. 87317-51167, Islamic Republic of Iran

Highlights: • For the first time, we have synthesized graphene nanosheets in the presence of pomegranate juice. • Here pomegranate juice was used not only as reductant but also as capping agent. • FT-IR, XRD, SEM, EDS and TEM were used to characterize the samples. • According to TEM image, graphene nanosheet is individually exfoliated after stirring for 24 h. • As shown in the TEM image, graphene monolayer is obtained. - Abstract: For the first time, we have successfully synthesized graphene nanosheets in the presence of pomegranate juice. In this approach, pomegranate juice was used not only as reductantmore » but also as capping agent to form graphene nanosheets. At first, the improved Hummer method to oxidize graphite for the synthesis of graphene oxide (GO) was applied, and then the as-produced graphene oxide was reduced by pomegranate juice to form graphene nanosheets. Fourier transformed infrared (FT-IR), X-ray powder diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectrometry (EDS), high resolution transmission electron microscopy (HRTEM), atomic force microscopy (AFM) and raman were used to characterize the samples. The results obtained from the characterization techniques proved high purity of the final products.« less

Purchase of a Transmission Electron Microscope for Xavier University of Louisiana

DTIC Science & Technology

2015-05-15

imaging facility on the second floor of the Pharmacy Addition at Xavier University that already includes two scanning electron microscopes. The new TEM...is now in use. Xavier University has formally pledged to provide funds for the 1. REPORT DATE (DD-MM-YYYY) 4. TITLE AND SUBTITLE 13. SUPPLEMENTARY...for Public Release; Distribution Unlimited Final Report: Purchase of a Transmission Electron Microscope for Xavier University of Louisiana The views

Preparation of the porous cerium dioxide film by two-step anodization and heat treating method

NASA Astrophysics Data System (ADS)

Liu, Xiaozhen; Zhu, Bolun; Liu, Yuze; Wang, Shanshan; Chen, Jie; Wang, Xiaoyu

2017-12-01

The porous cerium dioxide films were prepared with cerium foils as raw materials by two-step anodization and heat treating method. The anodic cerium oxide films were heat treated in 25∼400°C respectively. The cerium dioxide films were characterized with X-ray diffraction (XRD), Fourier transform infrared (FTIR) techniques, energy-dispersive analyses of X-ray (EDAX) and scanning electron microcopy (SEM), respectively. The anodic cerium oxide film is composed of Ce(OH)3, CeO2 and Ce2O3. When the anodic cerium oxide films were heat treated in 300°C∼400°C for 2h, Ce(OH)3 and Ce2O3 in the anodic cerium oxide films may be converted to CeO2, and the heat treated anodic cerium oxide films are the cerium dioxide films. Water, ethylene glycol and CO2 are adsorbed in the anodic cerium oxide film. The adsorbing water, ethylene glycol and CO2 in the anodic cerium oxide film are removed at 300°C. The cerium dioxide film has strong absorption in the range of 1600∼4000cm-1. The structure of the cerium dioxide film is the porous.

Antimicrobial Cu-bearing stainless steel scaffolds.

PubMed

Wang, Qiang; Ren, Ling; Li, Xiaopeng; Zhang, Shuyuan; Sercombe, Timothy B; Yang, Ke

2016-11-01

Copper-bearing stainless steel scaffolds with two different structures (Body Centered Cubic and Gyroid labyrinth) at two solid fractions (25% and 40%) were fabricated from both 316L powder and a mixture of 316L and elemental Cu powder using selective laser melting, and relative 316L scaffolds were served as control group. After processing, the antimicrobial testing demonstrated that the 316L-Cu scaffolds presented excellent antimicrobial activity against Escherichia coli and Staphylococcus aureus, and the cell viability assay indicated that there was no cytotoxic effect of 316L-Cu scaffolds on rat marrow mesenchymal stem cells. As such, these have the potential to reduce implant-associated infections. The Cu was also found to homogeneously distribute within the microstructure by scanning electronic microcopy. The addition of Cu would not significantly affect its strength and stiffness compared to 316L scaffold, and the stiffness of all the scaffolds (3-20GPa) is similar to that of bone and much less than that of bulk stainless steel. Consequently, fabrication of such low stiffness porous structures, especially coupled with the addition of antimicrobial Cu, may provide a new direction for medical stainless steels. Copyright © 2016 Elsevier B.V. All rights reserved.

The quest for inorganic fullerenes

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pietsch, Susanne; Dollinger, Andreas; Strobel, Christoph H.

2015-10-02

Experimental results of the search for inorganic fullerenes are presented. Mo nS m - and W nS m - clusters are generated with a pulsed arc cluster ion source equipped with an annealing stage. This is known to enhance fullerene formation in the case of carbon. Analogous to carbon, the mass spectra of the metal chalcogenide clusters produced in this way exhibit a bimodal structure. Moreover, the species in the first maximum at low mass are known to be platelets. The structure of the species in the second maximum is studied by anion photoelectron spectroscopy, scanning transmission electron microscopy,more » and scanning tunneling microcopy. All experimental results indicate a two-dimensional structure of these species and disagree with a three-dimensional fullerene-like geometry. A possible explanation for this preference of two-dimensional structures is the ability of a two-element material to saturate the dangling bonds at the edges of a platelet by excess atoms of one element. A platelet consisting of a single element only cannot do this. Likewise, graphite and boron might be the only materials forming nano-spheres because they are the only single element materials assuming two-dimensional structures.« less

The quest for inorganic fullerenes

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pietsch, Susanne; Dollinger, Andreas; Strobel, Christoph H.

2015-10-07

Experimental results of the search for inorganic fullerenes are presented. Mo{sub n}S{sub m}{sup −} and W{sub n}S{sub m}{sup −} clusters are generated with a pulsed arc cluster ion source equipped with an annealing stage. This is known to enhance fullerene formation in the case of carbon. Analogous to carbon, the mass spectra of the metal chalcogenide clusters produced in this way exhibit a bimodal structure. The species in the first maximum at low mass are known to be platelets. Here, the structure of the species in the second maximum is studied by anion photoelectron spectroscopy, scanning transmission electron microscopy, andmore » scanning tunneling microcopy. All experimental results indicate a two-dimensional structure of these species and disagree with a three-dimensional fullerene-like geometry. A possible explanation for this preference of two-dimensional structures is the ability of a two-element material to saturate the dangling bonds at the edges of a platelet by excess atoms of one element. A platelet consisting of a single element only cannot do this. Accordingly, graphite and boron might be the only materials forming nano-spheres because they are the only single element materials assuming two-dimensional structures.« less

Molecular modeling of the microstructure evolution during carbon fiber processing

NASA Astrophysics Data System (ADS)

Desai, Saaketh; Li, Chunyu; Shen, Tongtong; Strachan, Alejandro

2017-12-01

The rational design of carbon fibers with desired properties requires quantitative relationships between the processing conditions, microstructure, and resulting properties. We developed a molecular model that combines kinetic Monte Carlo and molecular dynamics techniques to predict the microstructure evolution during the processes of carbonization and graphitization of polyacrylonitrile (PAN)-based carbon fibers. The model accurately predicts the cross-sectional microstructure of the fibers with the molecular structure of the stabilized PAN fibers and physics-based chemical reaction rates as the only inputs. The resulting structures exhibit key features observed in electron microcopy studies such as curved graphitic sheets and hairpin structures. In addition, computed X-ray diffraction patterns are in good agreement with experiments. We predict the transverse moduli of the resulting fibers between 1 GPa and 5 GPa, in good agreement with experimental results for high modulus fibers and slightly lower than those of high-strength fibers. The transverse modulus is governed by sliding between graphitic sheets, and the relatively low value for the predicted microstructures can be attributed to their perfect longitudinal texture. Finally, the simulations provide insight into the relationships between chemical kinetics and the final microstructure; we observe that high reaction rates result in porous structures with lower moduli.

Plasmonic Three-Dimensional Transparent Conductor Based on Al-Doped Zinc Oxide-Coated Nanostructured Glass Using Atomic Layer Deposition

DOE PAGES

Malek, Gary A.; Aytug, Tolga; Liu, Qingfeng; ...

2015-04-02

Transparent nanostructured glass coatings, fabricated on glass substrates, with a unique three-dimensional (3D) architecture were utilized as the foundation for the design of plasmonic 3D transparent conductors. Transformation of the non-conducting 3D structure to a conducting 3D network was accomplished through atomic layer deposition of aluminum-doped zinc oxide (AZO). After AZO growth, gold nanoparticles (AuNPs) were deposited by electronbeam evaporation to enhance light trapping and decrease the overall sheet resistance. Field emission scanning electron microscopy and atomic force microcopy images revealed the highly porous, nanostructured morphology of the AZO coated glass surface along with the in-plane dimensions of the depositedmore » AuNPs. Sheet resistance measurements conducted on the coated samples verified that the electrical properties of the 3D network are comparable to that of the untextured two-dimensional AZO coated glass substrates. In addition, transmittance measurements of the glass samples coated with various AZO thicknesses showed preservation of the highly transparent nature of each sample, while the AuNPs demonstrated enhanced light scattering as well as light-trapping capability.« less

Plasmonic Three-Dimensional Transparent Conductor Based on Al-Doped Zinc Oxide-Coated Nanostructured Glass Using Atomic Layer Deposition

DOE Office of Scientific and Technical Information (OSTI.GOV)

Malek, Gary A.; Aytug, Tolga; Liu, Qingfeng

Transparent nanostructured glass coatings, fabricated on glass substrates, with a unique three-dimensional (3D) architecture were utilized as the foundation for the design of plasmonic 3D transparent conductors. Transformation of the non-conducting 3D structure to a conducting 3D network was accomplished through atomic layer deposition of aluminum-doped zinc oxide (AZO). After AZO growth, gold nanoparticles (AuNPs) were deposited by electronbeam evaporation to enhance light trapping and decrease the overall sheet resistance. Field emission scanning electron microscopy and atomic force microcopy images revealed the highly porous, nanostructured morphology of the AZO coated glass surface along with the in-plane dimensions of the depositedmore » AuNPs. Sheet resistance measurements conducted on the coated samples verified that the electrical properties of the 3D network are comparable to that of the untextured two-dimensional AZO coated glass substrates. In addition, transmittance measurements of the glass samples coated with various AZO thicknesses showed preservation of the highly transparent nature of each sample, while the AuNPs demonstrated enhanced light scattering as well as light-trapping capability.« less

Electrochemical synthesis of nanostructured Se-doped SnS: Effect of Se-dopant on surface characterizations

NASA Astrophysics Data System (ADS)

Kafashan, Hosein; Azizieh, Mahdi; Balak, Zohre

2017-07-01

SnS1-xSex nanostructures with different Se-dopant concentrations were deposited on fluorine doped tin oxide (FTO) substrate through cathodic electrodeposition technique. The pH, temperature, applied potential (E), and deposition time remained were 2.1, 60 °C, -1 V, and 30 min, respectively. SnS1-xSex nanostructures were characterized using X-ray diffraction (XRD), field emission scanning electron microcopy (FESEM), energy dispersive X-ray spectroscopy (EDX), room temperature photoluminescence (PL), and UV-vis spectroscopy. The XRD patterns revealed that the SnS1-xSex nanostructures were polycrystalline with orthorhombic structure. FESEM showed various kinds of morphologies in SnS1-xSex nanostructures due to Se-doping. PL and UV-vis spectroscopy were used to evaluate the optical properties of SnS1-xSex thin films. The PL spectra of SnS1-xSex nanostructures displayed four emission peaks, those are a blue, a green, an orange, and a red emission. UV-vis spectra showed that the optical band gap energy (Eg) of SnS1-xSex nanostructures varied between 1.22-1.65 eV, due to Se-doping.