Asymmetrical flow field-flow fractionation with multi-angle light scattering and quasi-elastic light scattering for characterization of polymersomes: comparison with classical techniques.

PubMed

Till, Ugo; Gaucher-Delmas, Mireille; Saint-Aguet, Pascale; Hamon, Glenn; Marty, Jean-Daniel; Chassenieux, Christophe; Payré, Bruno; Goudounèche, Dominique; Mingotaud, Anne-Françoise; Violleau, Frédéric

2014-12-01

Polymersomes formed from amphiphilic block copolymers, such as poly(ethyleneoxide-b-ε-caprolactone) (PEO-b-PCL) or poly(ethyleneoxide-b-methylmethacrylate), were characterized by asymmetrical flow field-flow fractionation coupled with quasi-elastic light scattering (QELS), multi-angle light scattering (MALS), and refractive index detection, leading to the determination of their size, shape, and molecular weight. The method was cross-examined with more classical ones, like batch dynamic and static light scattering, electron microscopy, and atomic force microscopy. The results show good complementarities between all the techniques; asymmetrical flow field-flow fractionation being the most pertinent one when the sample exhibits several different types of population.

Phase-space foundations of electron holography

NASA Astrophysics Data System (ADS)

Lubk, A.; Röder, F.

2015-09-01

We present a unified formalism for describing various forms of electron holography in quantum mechanical phase space including their extensions to quantum-state reconstructions. The phase-space perspective allows for taking into account partial coherence as well as the quantum mechanical detection process typically hampering the unique reconstruction of a wave function. We elaborate on the limitations imposed by the electron optical elements of the transmission electron microscope as well as the scattering at the target. The results provide the basis for vastly extending the scope of electron holographic techniques towards analyzing partially coherent signals such as inelastically scattered electrons or electron pulses used in ultrafast transmission electron microscopy.

Curcumin Inhibits Tau Aggregation and Disintegrates Preformed Tau Filaments in vitro.

PubMed

Rane, Jitendra Subhash; Bhaumik, Prasenjit; Panda, Dulal

2017-01-01

The pathological aggregation of tau is a common feature of most of the neuronal disorders including frontotemporal dementia, Parkinson's disease, and Alzheimer's disease. The inhibition of tau aggregation is considered to be one of the important strategies for treating these neurodegenerative diseases. Curcumin, a natural polyphenolic molecule, has been reported to have neuroprotective ability. In this work, curcumin was found to bind to adult tau and fetal tau with a dissociation constant of 3.3±0.4 and 8±1 μM, respectively. Molecular docking studies indicated a putative binding site of curcumin in the microtubule-binding region of tau. Using several complementary techniques, including dynamic light scattering, thioflavin S fluorescence, 90° light scattering, electron microscopy, and atomic force microscopy, curcumin was found to inhibit the aggregation of tau. The dynamic light scattering analysis and atomic force microscopic images revealed that curcumin inhibits the oligomerization of tau. Curcumin also disintegrated preformed tau oligomers. Using Far-UV circular dichroism, curcumin was found to inhibit the β-sheets formation in tau indicating that curcumin inhibits an initial step of tau aggregation. In addition, curcumin inhibited tau fibril formation. Furthermore, the effect of curcumin on the preformed tau filaments was analyzed by atomic force microscopy, transmission electron microscopy, and 90° light scattering. Curcumin treatment disintegrated preformed tau filaments. The results indicated that curcumin inhibited the oligomerization of tau and could disaggregate tau filaments.

Plasmon-enhanced electron scattering in nanostructured thin metal films revealed by low-voltage scanning electron microscopy

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

Mikhailovskii, V., E-mail: v.mikhailovskii@spbu.ru; IRC for Nanotechnology, Research Park, St.-Petersburg State University; Petrov, Yu.

2016-06-17

The drastic enhancement of backscattered electrons (BSE) yield from nanostructured thin metal film which exceeded well the one from massive metal was observed at accelerating voltages below 400 V. The dependences of BSE signal from nanostructured gold film on accelerating voltage and on retarding grid potential applied to BSE detector were investigated. It was shown that enhanced BSE signal was formed by inelastic scattered electrons coming from the gaps between nanoparticles. A tentative explanation of the mechanism of BSE signal enhancement was suggested.

Visualizing electron pockets in cuprate superconductors

NASA Astrophysics Data System (ADS)

Das, Tanmoy; Markiewicz, R. S.; Bansil, A.; Balatsky, A. V.

2012-06-01

Fingerprints of the electron pocket in cuprates have been obtained only in numerous magnetotransport measurements, but its absence in spectroscopic observations poses a long-standing mystery. We develop a theoretical tool to provide ways to detect electron pockets via spectroscopies including scanning tunneling microscopy (STM) spectra, inelastic neutron scattering (INS), and angle-resolved photoemission spectroscopy (ARPES). We show that the quasiparticle-interference (QPI) pattern, measured by STM, shows an additional seven q vectors associated with the scattering on the electron pocket than that on the hole pocket. Furthermore, the Bogolyubov quasiparticle scatterings of the electron pocket lead to a second magnetic resonance mode in the INS spectra at a higher resonance energy. Finally, we reanalyze some STM, INS, and ARPES experimental data of several cuprates which dictates the direct fingerprints of electron pockets in these systems.

Label-free real-time imaging of myelination in the Xenopus laevis tadpole by in vivo stimulated Raman scattering microscopy

NASA Astrophysics Data System (ADS)

Hu, Chun-Rui; Zhang, Delong; Slipchenko, Mikhail N.; Cheng, Ji-Xin; Hu, Bing

2014-08-01

The myelin sheath plays an important role as the axon in the functioning of the neural system, and myelin degradation is a hallmark pathology of multiple sclerosis and spinal cord injury. Electron microscopy, fluorescent microscopy, and magnetic resonance imaging are three major techniques used for myelin visualization. However, microscopic observation of myelin in living organisms remains a challenge. Using a newly developed stimulated Raman scattering microscopy approach, we report noninvasive, label-free, real-time in vivo imaging of myelination by a single-Schwann cell, maturation of a single node of Ranvier, and myelin degradation in the transparent body of the Xenopus laevis tadpole.

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

Monitoring adsorption of gold nanoparticles on gold nanodisk array using dark-field hyperspectral microscopy (Conference Presentation)

NASA Astrophysics Data System (ADS)

Zhao, Fusheng; Zenasni, Oussama; Li, Jingting; Shih, Wei-Chuan

2017-02-01

Localized surface plasmon resonance (LSPR) arises from the interaction of light with noble metal nanoparticles, which induces a collective oscillation in the free electrons. The size and shape of the metallic nanostructure significantly impact LSPR frequency and strength. Nanoplasmonic sensor has become a recent research focus due to its significant signal enhancement and robust signal transduction measured by extinction spectroscopy, fluorescence, Raman scattering, and absorption spectroscopy. Dark-field microscopy, in contrast, reports the scattered photons after light-matter interactions. In this case, the nanoparticles can be understood as dipole radiators whose free electrons oscillate in concert. Coupled with spectroscopy, this platform allows the collection of plasmonically scattered spectra from gold nanoparticles. Plasmonic coupling between electron-beam lithography patterned gold nanodisks (AuND) and colloidal gold nanoparticles (AuNP) can change the plasmonic resonance of the original entities, and can be effectively studied by dark-field hyperspectral microscopy. Typically, a pronounced redshift can be observed when plasmonic coupling occurs. When these nano-entities are functionalized with interactive surface moieties, biochemistry and molecular processes can be studied. In this paper, we will present the capability of assessing the process of immobilizing streptavidin-functionalized AuNPs on an array of biotin-terminated AuNDs. By monitoring changes in the LSPR band of AuNDs, we are able to evaluate similar processes in other molecular systems. In addition, plasmon coupling induced scattering intensity variations can be measured by an electron-multiplied charge-coupled device camera for rapid in situ monitoring. This method can potentially be useful in studying dynamic biophysical and biochemical processes in situ.

Visualizing One-Dimensional Electronic States and their Scattering in Semi-conducting Nanowires

NASA Astrophysics Data System (ADS)

Beidenkopf, Haim; Reiner, Jonathan; Norris, Andrew; Nayak, Abhay Kumar; Avraham, Nurit; Shtrikman, Hadas

One-dimensional electronic systems constitute a fascinating playground for the emergence of exotic electronic effects and phases, within and beyond the Tomonaga-Luttinger liquid paradigm. More recently topological superconductivity and Majorana modes were added to that long list of phenomena. We report scanning tunneling microscopy and spectroscopy measurements conducted on pristine, epitaxialy grown InAs nanowires. We resolve the 1D electronic band structure manifested both via Van-Hove singularities in the local density-of-states, as well as by the quasi-particle interference patterns, induced by scattering from surface impurities. By studying the scattering of the one-dimensional electronic states off various scatterers, including crystallographic defects and the nanowire end, we identify new one-dimensional relaxation regimes and yet unexplored effects of interactions. Some of these may bear implications on the topological superconducting state and Majorana modes therein. The authors acknowledge support from the Israeli Science Foundation (ISF).

Multiscale phase mapping of LiFePO4-based electrodes by transmission electron microscopy and electron forward scattering diffraction.

PubMed

Robert, Donatien; Douillard, Thierry; Boulineau, Adrien; Brunetti, Guillaume; Nowakowski, Pawel; Venet, Denis; Bayle-Guillemaud, Pascale; Cayron, Cyril

2013-12-23

LiFePO4 and FePO4 phase distributions of entire cross-sectioned electrodes with various Li content are investigated from nanoscale to mesoscale, by transmission electron microscopy and by the new electron forward scattering diffraction technique. The distributions of the fully delithiated (FePO4) or lithiated particles (LiFePO4) are mapped on large fields of view (>100 × 100 μm(2)). Heterogeneities in thin and thick electrodes are highlighted at different scales. At the nanoscale, the statistical analysis of 64 000 particles unambiguously shows that the small particles delithiate first. At the mesoscale, the phase maps reveal a core-shell mechanism at the scale of the agglomerates with a preferential pathway along the electrode porosities. At larger scale, lithiation occurs in thick electrodes "stratum by stratum" from the surface in contact with electrolyte toward the current collector.

Determination of the size and phase composition of silver nanoparticles in a gel film of bacterial cellulose by small-angle X-ray scattering, electron diffraction, and electron microscopy

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

Volkov, V. V.; Klechkovskaya, V. V., E-mail: klechvv@ns.crys.ras.ru; Shtykova, E. V.

2009-03-15

The nanoscale structural features in a composite (gel film of Acetobacter Xylinum cellulose with adsorbed silver nanoparticles, stabilized by N-polyvinylpyrrolidone) have been investigated by small-angle X-ray scattering. The size distributions of inhomogeneities in the porous structure of the cellulose matrix and the size distributions of silver nanoparticles in the composite have been determined. It is shown that the sizes of synthesized nanoparticles correlate with the sizes of inhomogeneities in the gel film. Particles of larger size (with radii up to 100 nm) have also been found. Electron microscopy of thin cross sections of a dried composite layer showed that largemore » particles are located on the cellulose layer surface. Electron diffraction revealed a crystal structure of silver nanoparticles in the composite.« less

Electron microscopy localization and characterization of functionalized composite organic-inorganic SERS nanoparticles on leukemia cells.

PubMed

Koh, Ai Leen; Shachaf, Catherine M; Elchuri, Sailaja; Nolan, Garry P; Sinclair, Robert

2008-12-01

We demonstrate the use of electron microscopy as a powerful characterization tool to identify and locate antibody-conjugated composite organic-inorganic nanoparticle (COINs) surface enhanced Raman scattering (SERS) nanoparticles on cells. U937 leukemia cells labeled with antibody CD54-conjugated COINs were characterized in their native, hydrated state using wet scanning electron microscopy (SEM) and in their dehydrated state using high-resolution SEM. In both cases, the backscattered electron (BSE) detector was used to detect and identify the silver constituents in COINs due to its high sensitivity to atomic number variations within a specimen. The imaging and analytical capabilities in the SEM were further complemented by higher resolution transmission electron microscopy (TEM) images and scanning Auger electron spectroscopy (AES) data to give reliable and high-resolution information about nanoparticles and their binding to cell surface antigens.

Understanding electron magnetic circular dichroism in a transition potential approach

NASA Astrophysics Data System (ADS)

Barthel, J.; Mayer, J.; Rusz, J.; Ho, P.-L.; Zhong, X. Y.; Lentzen, M.; Dunin-Borkowski, R. E.; Urban, K. W.; Brown, H. G.; Findlay, S. D.; Allen, L. J.

2018-04-01

This paper introduces an approach based on transition potentials for inelastic scattering to understand the underlying physics of electron magnetic circular dichroism (EMCD). The transition potentials are sufficiently localized to permit atomic-scale EMCD. Two-beam and three-beam systematic row cases are discussed in detail in terms of transition potentials for conventional transmission electron microscopy, and the basic symmetries which arise in the three-beam case are confirmed experimentally. Atomic-scale EMCD in scanning transmission electron microscopy (STEM), using both a standard STEM probe and vortex beams, is discussed.

Molecular Orientation in Dry and Hydrated Cellulose Fibers: A Coherent Anti-Stokes Raman Scattering Microscopy Study

PubMed Central

Zimmerley, Maxwell; Younger, Rebecca; Valenton, Tiffany; Oertel, David C.; Ward, Jimmie L.; Potma, Eric O.

2012-01-01

Coherent anti-Stokes Raman scattering (CARS) microscopy is combined with spontaneous Raman scattering microspectroscopy and second harmonic generation (SHG) microscopy to interrogate the molecular alignment in dry and hydrated cellulose fibers. Two types of cellulose were investigated: natural cellulose I in cotton fibers and regenerated cellulose II in rayon fibers. On the basis of the orientation of the methylene symmetric stretching vibration, the molecular alignment of cellulose microfibrils is found to be conserved on the micrometer scale. Whereas the molecular orientation in cotton shows modest variability along the fiber, the alignment of the cellulose units in rayon is highly consistent throughout the fiber. The ordered alignment is retained upon fiber hydration. Upon hydration of the cellulose fibers, an anisotropic electronic contribution is observed, which indicates an ordered incorporation of water molecules into the fiber structure. The third-order and second-order electronic polarizability of cellulose I are directed along the axis of the polyglucan chain. No second-order optical response is observed in cellulose II, supporting the antiparallel arrangement of the polyglucan chains in regenerated cellulose. PMID:20684644

High-resolution quantitative determination of dielectric function by using scattering scanning near-field optical microscopy

PubMed Central

Tranca, D. E.; Stanciu, S. G.; Hristu, R.; Stoichita, C.; Tofail, S. A. M.; Stanciu, G. A.

2015-01-01

A new method for high-resolution quantitative measurement of the dielectric function by using scattering scanning near-field optical microscopy (s-SNOM) is presented. The method is based on a calibration procedure that uses the s-SNOM oscillating dipole model of the probe-sample interaction and quantitative s-SNOM measurements. The nanoscale capabilities of the method have the potential to enable novel applications in various fields such as nano-electronics, nano-photonics, biology or medicine. PMID:26138665

Electron Diffraction Using Transmission Electron Microscopy

PubMed Central

Bendersky, Leonid A.; Gayle, Frank W.

2001-01-01

Electron diffraction via the transmission electron microscope is a powerful method for characterizing the structure of materials, including perfect crystals and defect structures. The advantages of electron diffraction over other methods, e.g., x-ray or neutron, arise from the extremely short wavelength (≈2 pm), the strong atomic scattering, and the ability to examine tiny volumes of matter (≈10 nm3). The NIST Materials Science and Engineering Laboratory has a history of discovery and characterization of new structures through electron diffraction, alone or in combination with other diffraction methods. This paper provides a survey of some of this work enabled through electron microscopy. PMID:27500060

Diffuse x-ray scattering and transmission electron microscopy study of defects in antimony-implanted silicon

NASA Astrophysics Data System (ADS)

Takamura, Y.; Marshall, A. F.; Mehta, A.; Arthur, J.; Griffin, P. B.; Plummer, J. D.; Patel, J. R.

2004-04-01

Ion implantation followed by laser annealing has been used to create supersaturated and electrically active concentrations of antimony in silicon. Upon subsequent thermal annealing, however, these metastable dopants deactivate towards the equilibrium solubility limit. In this work, the formation of inactive antimony structures has been studied with grazing incidence diffuse x-ray scattering, and transmission electron microscopy, and the results are correlated to previous high-resolution x-ray diffraction data. We find that at a concentration of 6.0×1020 cm-3, small, incoherent clusters of radius 3-4 Å form during annealing at 900 °C. At a higher concentration of 2.2×1021 cm-3, deactivation at 600 °C occurs through the formation of small, antimony aggregates and antimony precipitates. The size of these precipitates from diffuse x-ray scattering is roughly 15 Å in radius for anneal times from 15 to 180 seconds. This value is consistent with the features observed in high-resolution and mass contrast transmission electron microscopy images. The coherent nature of the aggregates and precipitates causes the expansion of the surrounding silicon matrix as the deactivation progresses. In addition, the sensitivity of the diffuse x-ray scattering technique has allowed us to detect the presence of small clusters of radius ˜2 Å in unprocessed Czochralski silicon wafers. These defects are not observed in floating zone silicon wafers, and are tentatively attributed to thermal donors.

Nanometres-resolution Kikuchi patterns from materials science specimens with transmission electron forward scatter diffraction in the scanning electron microscope.

PubMed

Brodusch, N; Demers, H; Gauvin, R

2013-04-01

A charge-coupled device camera of an electron backscattered diffraction system in a scanning electron microscope was positioned below a thin specimen and transmission Kikuchi patterns were collected. Contrary to electron backscattered diffraction, transmission electron forward scatter diffraction provides phase identification and orientation mapping at the nanoscale. The minimum Pd particle size for which a Kikuchi diffraction pattern was detected and indexed reliably was 5.6 nm. An orientation mapping resolution of 5 nm was measured at 30 kV. The resolution obtained with transmission electron forward scatter diffraction was of the same order of magnitude than that reported in electron nanodiffraction in the transmission electron microscope. An energy dispersive spectrometer X-ray map and a transmission electron forward scatter diffraction orientation map were acquired simultaneously. The high-resolution chemical, phase and orientation maps provided at once information on the chemical form, orientation and coherency of precipitates in an aluminium-lithium 2099 alloy. © 2013 The Authors Journal of Microscopy © 2013 Royal Microscopical Society.

Diffraction data of core-shell nanoparticles from an X-ray free electron laser

DOE PAGES

Li, Xuanxuan; Chiu, Chun -Ya; Wang, Hsiang -Ju; ...

2017-04-11

X-ray free-electron lasers provide novel opportunities to conduct single particle analysis on nanoscale particles. Coherent diffractive imaging experiments were performed at the Linac Coherent Light Source (LCLS), SLAC National Laboratory, exposing single inorganic core-shell nanoparticles to femtosecond hard-X-ray pulses. Each facetted nanoparticle consisted of a crystalline gold core and a differently shaped palladium shell. Scattered intensities were observed up to about 7 nm resolution. Analysis of the scattering patterns revealed the size distribution of the samples, which is consistent with that obtained from direct real-space imaging by electron microscopy. Furthermore, scattering patterns resulting from single particles were selected and compiledmore » into a dataset which can be valuable for algorithm developments in single particle scattering research.« less

Electron microscopy approach for the visualization of the epithelial and endothelial glycocalyx.

PubMed

Chevalier, L; Selim, J; Genty, D; Baste, J M; Piton, N; Boukhalfa, I; Hamzaoui, M; Pareige, P; Richard, V

2017-06-01

This study presents a methodological approach for the visualization of the glycocalyx by electron microscopy. The glycocalyx is a three dimensional network mainly composed of glycolipids, glycoproteins and proteoglycans associated with the plasma membrane. Since less than a decade, the epithelial and endothelial glycocalyx proved to play an important role in physiology and pathology, increasing its research interest especially in vascular functions. Therefore, visualization of the glycocalyx requires reliable techniques and its preservation remains challenging due to its fragile and dynamic organization, which is highly sensitive to the different process steps for electron microscopy sampling. In this study, chemical fixation was performed by perfusion as a good alternative to conventional fixation. Additional lanthanum nitrate in the fixative enhances staining of the glycocalyx in transmission electron microscopy bright field and improves its visualization by detecting the elastic scattered electrons, thus providing a chemical contrast. Copyright © 2017 Elsevier Masson SAS. All rights reserved.

Source of coherent short wavelength radiation

DOEpatents

Villa, Francesco

1990-01-01

An apparatus for producing coherent radiation ranging from X-rays to the far ultraviolet (i.e., 1 Kev to 10 eV) utilizing the Compton scattering effect. A photon beam from a laser is scattered on a high energy electron bunch from a pulse power linac. The short wavelength radiation produced by such scattering has sufficient intensity and spatial coherence for use in high resolution applications such as microscopy.

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.

High Dynamic Range Pixel Array Detector for Scanning Transmission Electron Microscopy.

PubMed

Tate, Mark W; Purohit, Prafull; Chamberlain, Darol; Nguyen, Kayla X; Hovden, Robert; Chang, Celesta S; Deb, Pratiti; Turgut, Emrah; Heron, John T; Schlom, Darrell G; Ralph, Daniel C; Fuchs, Gregory D; Shanks, Katherine S; Philipp, Hugh T; Muller, David A; Gruner, Sol M

2016-02-01

We describe a hybrid pixel array detector (electron microscope pixel array detector, or EMPAD) adapted for use in electron microscope applications, especially as a universal detector for scanning transmission electron microscopy. The 128×128 pixel detector consists of a 500 µm thick silicon diode array bump-bonded pixel-by-pixel to an application-specific integrated circuit. The in-pixel circuitry provides a 1,000,000:1 dynamic range within a single frame, allowing the direct electron beam to be imaged while still maintaining single electron sensitivity. A 1.1 kHz framing rate enables rapid data collection and minimizes sample drift distortions while scanning. By capturing the entire unsaturated diffraction pattern in scanning mode, one can simultaneously capture bright field, dark field, and phase contrast information, as well as being able to analyze the full scattering distribution, allowing true center of mass imaging. The scattering is recorded on an absolute scale, so that information such as local sample thickness can be directly determined. This paper describes the detector architecture, data acquisition system, and preliminary results from experiments with 80-200 keV electron beams.

Mechanisms of decoherence in electron microscopy.

PubMed

Howie, A

2011-06-01

The understanding and where possible the minimisation of decoherence mechanisms in electron microscopy were first studied in plasmon loss, diffraction contrast images but are of even more acute relevance in high resolution TEM phase contrast imaging and electron holography. With the development of phase retrieval techniques they merit further attention particularly when their effect cannot be eliminated by currently available energy filters. The roles of electronic excitation, thermal diffuse scattering, transition radiation and bremsstrahlung are examined here not only in the specimen but also in the electron optical column. Terahertz-range aloof beam electronic excitation appears to account satisfactorily for recent observations of decoherence in electron holography. An apparent low frequency divergence can emerge for the calculated classical bremsstrahlung event probability but can be ignored for photon wavelengths exceeding the required coherence distance or path lengths in the equipment. Most bremsstrahlung event probabilities are negligibly important except possibly in large-angle bending magnets or mandolin systems. A more reliable procedure for subtracting thermal diffuse scattering from diffraction pattern intensities is proposed. Copyright © 2010 Elsevier B.V. All rights reserved.

Theory of bright-field scanning transmission electron microscopy for tomography

NASA Astrophysics Data System (ADS)

Levine, Zachary H.

2005-02-01

Radiation transport theory is applied to electron microscopy of samples composed of one or more materials. The theory, originally due to Goudsmit and Saunderson, assumes only elastic scattering and an amorphous medium dominated by atomic interactions. For samples composed of a single material, the theory yields reasonable parameter-free agreement with experimental data taken from the literature for the multiple scattering of 300-keV electrons through aluminum foils up to 25μm thick. For thin films, the theory gives a validity condition for Beer's law. For thick films, a variant of Molière's theory [V. G. Molière, Z. Naturforschg. 3a, 78 (1948)] of multiple scattering leads to a form for the bright-field signal for foils in the multiple-scattering regime. The signal varies as [tln(e1-2γt/τ)]-1 where t is the path length of the beam, τ is the mean free path for elastic scattering, and γ is Euler's constant. The Goudsmit-Saunderson solution interpolates numerically between these two limits. For samples with multiple materials, elemental sensitivity is developed through the angular dependence of the scattering. From the elastic scattering cross sections of the first 92 elements, a singular-value decomposition of a vector space spanned by the elastic scattering cross sections minus a delta function shows that there is a dominant common mode, with composition-dependent corrections of about 2%. A mathematically correct reconstruction procedure beyond 2% accuracy requires the acquisition of the bright-field signal as a function of the scattering angle. Tomographic reconstructions are carried out for three singular vectors of a sample problem with four elements Cr, Cu, Zr, and Te. The three reconstructions are presented jointly as a color image; all four elements are clearly identifiable throughout the image.

Quantum scattering beyond the plane-wave approximation

NASA Astrophysics Data System (ADS)

Karlovets, Dmitry

2017-12-01

While a plane-wave approximation in high-energy physics works well in a majority of practical cases, it becomes inapplicable for scattering of the vortex particles carrying orbital angular momentum, of Airy beams, of the so-called Schrödinger cat states, and their generalizations. Such quantum states of photons, electrons and neutrons have been generated experimentally in recent years, opening up new perspectives in quantum optics, electron microscopy, particle physics, and so forth. Here we discuss the non-plane-wave effects in scattering brought about by the novel quantum numbers of these wave packets. For the well-focused electrons of intermediate energies, already available at electron microscopes, the corresponding contribution can surpass that of the radiative corrections. Moreover, collisions of the cat-like superpositions of such focused beams with atoms allow one to probe effects of the quantum interference, which have never played any role in particle scattering.

Synthesis of gold nanoflowers using deep eutectic solvent with high surface enhanced Raman scattering properties

NASA Astrophysics Data System (ADS)

Aghakhani Mahyari, Farzaneh; Tohidi, Maryam; Safavi, Afsaneh

2016-09-01

A facile, seed-less and one-pot method was developed for synthesis of gold nanoflowers with multiple tips through reduction of HAuCl4 with deep eutectic solvent at room temperature. This solvent is eco-friendly, low-cost, non-toxic and biodegradable and can act as both reducing and shape-controlling agent. In this protocol, highly branched and stable gold nanoflowers were obtained without using any capping agent. The obtained products were characterized by different techniques including, field emission scanning electron microscopy, transmission electron microscopy, x-ray diffraction and UV-vis spectroscopy. The as-prepared gold nanoflowers exhibit efficient surface-enhanced Raman scattering (SERS) properties which can be used as excellent substrates for SERS.

High-quality imaging in environmental scanning electron microscopy--optimizing the pressure limiting system and the secondary electron detection of a commercially available ESEM.

PubMed

Fitzek, H; Schroettner, H; Wagner, J; Hofer, F; Rattenberger, J

2016-04-01

In environmental scanning electron microscopy applications in the kPa regime are of increasing interest for the investigation of wet and biological samples, because neither sample preparation nor extensive cooling are necessary. Unfortunately, the applications are limited by poor image quality. In this work the image quality at high pressures of a FEI Quanta 600 (field emission gun) and a FEI Quanta 200 (thermionic gun) is greatly improved by optimizing the pressure limiting system and the secondary electron (SE) detection system. The scattering of the primary electron beam strongly increases with pressure and thus the image quality vanishes. The key to high-image quality at high pressures is to reduce scattering as far as possible while maintaining ideal operation conditions for the SE-detector. The amount of scattering is reduced by reducing both the additional stagnation gas thickness (aSGT) and the environmental distance (ED). A new aperture holder is presented that significantly reduces the aSGT while maintaining the same field-of-view (FOV) as the original design. With this aperture holder it is also possible to make the aSGT even smaller at the expense of a smaller FOV. A new blade-shaped SE-detector is presented yielding better image quality than usual flat SE-detectors. The electrode of the new SE detector is positioned on the sample table, which allows the SE-detector to operate at ideal conditions regardless of pressure and ED. © 2015 The Authors Journal of Microscopy © 2015 Royal Microscopical Society.

Raman scattering from rapid thermally annealed tungsten silicide

NASA Technical Reports Server (NTRS)

Kumar, Sandeep; Dasgupta, Samhita; Jackson, Howard E.; Boyd, Joseph T.

1987-01-01

Raman scattering as a technique for studying the formation of tungsten silicide is presented. The tungsten silicide films have been formed by rapid thermal annealing of thin tungsten films sputter deposited on silicon substrates. The Raman data are interpreted by using data from resistivity measurements, Auger and Rutherford backscattering measurements, and scanning electron microscopy.

Nano-Se: Cheap and easy-to-obtain novel material for all-dielectric nano-photonics

NASA Astrophysics Data System (ADS)

Ivanova, A. K.; Ionin, A. A.; Khmel'nitskii, R. A.; Klevkov, Yu. K.; Kudryashov, S. I.; Levchenko, A. O.; Mel'nik, N. N.; Nastulyavichus, A. A.; Rudenko, A. A.; Saraeva, I. N.; Smirnov, N. A.; Zayarny, D. A.; Gonchukov, S. A.; Tolordava, E. R.; Baranov, A. N.

2017-09-01

Milligram-per-second production of selenium nanoparticles in water sols was realized through few W, kHz-rate nanosecond laser ablation of a solid selenium pellet. High-yield particle formation mechanism and ultimate mass-removal yield were elucidated by optical profilometry and scanning electron microscopy characterization of crater depths and topographies. Deposited particles were inspected by scanning electron microscopy, while optical transmission Raman and dynamic light scattering spectroscopy characterized their hydrosols.

Materials characterisation by angle-resolved scanning transmission electron microscopy.

PubMed

Müller-Caspary, Knut; Oppermann, Oliver; Grieb, Tim; Krause, Florian F; Rosenauer, Andreas; Schowalter, Marco; Mehrtens, Thorsten; Beyer, Andreas; Volz, Kerstin; Potapov, Pavel

2016-11-16

Solid-state properties such as strain or chemical composition often leave characteristic fingerprints in the angular dependence of electron scattering. Scanning transmission electron microscopy (STEM) is dedicated to probe scattered intensity with atomic resolution, but it drastically lacks angular resolution. Here we report both a setup to exploit the explicit angular dependence of scattered intensity and applications of angle-resolved STEM to semiconductor nanostructures. Our method is applied to measure nitrogen content and specimen thickness in a GaN x As 1-x layer independently at atomic resolution by evaluating two dedicated angular intervals. We demonstrate contrast formation due to strain and composition in a Si- based metal-oxide semiconductor field effect transistor (MOSFET) with Ge x Si 1-x stressors as a function of the angles used for imaging. To shed light on the validity of current theoretical approaches this data is compared with theory, namely the Rutherford approach and contemporary multislice simulations. Inconsistency is found for the Rutherford model in the whole angular range of 16-255 mrad. Contrary, the multislice simulations are applicable for angles larger than 35 mrad whereas a significant mismatch is observed at lower angles. This limitation of established simulations is discussed particularly on the basis of inelastic scattering.

Facing the phase problem in Coherent Diffractive Imaging via Memetic Algorithms.

PubMed

Colombo, Alessandro; Galli, Davide Emilio; De Caro, Liberato; Scattarella, Francesco; Carlino, Elvio

2017-02-09

Coherent Diffractive Imaging is a lensless technique that allows imaging of matter at a spatial resolution not limited by lens aberrations. This technique exploits the measured diffraction pattern of a coherent beam scattered by periodic and non-periodic objects to retrieve spatial information. The diffracted intensity, for weak-scattering objects, is proportional to the modulus of the Fourier Transform of the object scattering function. Any phase information, needed to retrieve its scattering function, has to be retrieved by means of suitable algorithms. Here we present a new approach, based on a memetic algorithm, i.e. a hybrid genetic algorithm, to face the phase problem, which exploits the synergy of deterministic and stochastic optimization methods. The new approach has been tested on simulated data and applied to the phasing of transmission electron microscopy coherent electron diffraction data of a SrTiO 3 sample. We have been able to quantitatively retrieve the projected atomic potential, and also image the oxygen columns, which are not directly visible in the relevant high-resolution transmission electron microscopy images. Our approach proves to be a new powerful tool for the study of matter at atomic resolution and opens new perspectives in those applications in which effective phase retrieval is necessary.

Electron Microscopy Localization and Characterization of Functionalized Composite Organic-Inorganic SERS Nanoparticles on Leukemia Cells

PubMed Central

Koh, Ai Leen; Shachaf, Catherine M.; Elchuri, Sailaja; Nolan, Garry P.; Sinclair, Robert

2008-01-01

We demonstrate the use of electron microscopy as a powerful characterization tool to identify and locate antibody-conjugated composite organic-inorganic (COINs) surface enhanced Raman scattering (SERS) nanoparticles on cells. U937 leukemia cells labeled with antibody CD54-conjugated COINs were characterized in their native, hydrated state using wet Scanning Electron Microscopy (SEM) and in their dehydrated state using high-resolution SEM. In both cases, the backscattered electron detector (BSE) was used to detect and identify the silver constituents in COINs due to its high sensitivity to atomic number variations within a specimen. The imaging and analytical capabilities in the SEM were further complemented by higher resolution Transmission Electron Microscope (TEM) images and Scanning Auger Electron Spectroscopy (AES) data to give reliable and high-resolution information about nanoparticles and their binding to cell surface antigens. PMID:18995965

The spatial coherence function in scanning transmission electron microscopy and spectroscopy.

PubMed

Nguyen, D T; Findlay, S D; Etheridge, J

2014-11-01

We investigate the implications of the form of the spatial coherence function, also referred to as the effective source distribution, for quantitative analysis in scanning transmission electron microscopy, and in particular for interpreting the spatial origin of imaging and spectroscopy signals. These questions are explored using three different source distribution models applied to a GaAs crystal case study. The shape of the effective source distribution was found to have a strong influence not only on the scanning transmission electron microscopy (STEM) image contrast, but also on the distribution of the scattered electron wavefield and hence on the spatial origin of the detected electron intensities. The implications this has for measuring structure, composition and bonding at atomic resolution via annular dark field, X-ray and electron energy loss STEM imaging are discussed. Copyright © 2014 Elsevier B.V. All rights reserved.

Spatial Resolution in Scanning Electron Microscopy and Scanning Transmission Electron Microscopy Without a Specimen Vacuum Chamber.

PubMed

Nguyen, Kayla X; Holtz, Megan E; Richmond-Decker, Justin; Muller, David A

2016-08-01

A long-standing goal of electron microscopy has been the high-resolution characterization of specimens in their native environment. However, electron optics require high vacuum to maintain an unscattered and focused probe, a challenge for specimens requiring atmospheric or liquid environments. Here, we use an electron-transparent window at the base of a scanning electron microscope's objective lens to separate column vacuum from the specimen, enabling imaging under ambient conditions, without a specimen vacuum chamber. We demonstrate in-air imaging of specimens at nanoscale resolution using backscattered scanning electron microscopy (airSEM) and scanning transmission electron microscopy. We explore resolution and contrast using Monte Carlo simulations and analytical models. We find that nanometer-scale resolution can be obtained at gas path lengths up to 400 μm, although contrast drops with increasing gas path length. As the electron-transparent window scatters considerably more than gas at our operating conditions, we observe that the densities and thicknesses of the electron-transparent window are the dominant limiting factors for image contrast at lower operating voltages. By enabling a variety of detector configurations, the airSEM is applicable to a wide range of environmental experiments including the imaging of hydrated biological specimens and in situ chemical and electrochemical processes.

Spatial Resolution in Scanning Electron Microscopy and Scanning Transmission Electron Microscopy Without a Specimen Vacuum Chamber

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

Nguyen, Kayla X.; Holtz, Megan E.; Richmond-Decker, Justin

2016-07-25

Abstract A long-standing goal of electron microscopy has been the high-resolution characterization of specimens in their native environment. However, electron optics require high vacuum to maintain an unscattered and focused probe, a challenge for specimens requiring atmospheric or liquid environments. Here, we use an electron-transparent window at the base of a scanning electron microscope’s objective lens to separate column vacuum from the specimen, enabling imaging under ambient conditions, without a specimen vacuum chamber. We demonstrate in-air imaging of specimens at nanoscale resolution using backscattered scanning electron microscopy (airSEM) and scanning transmission electron microscopy. We explore resolution and contrast using Montemore » Carlo simulations and analytical models. We find that nanometer-scale resolution can be obtained at gas path lengths up to 400μm, although contrast drops with increasing gas path length. As the electron-transparent window scatters considerably more than gas at our operating conditions, we observe that the densities and thicknesses of the electron-transparent window are the dominant limiting factors for image contrast at lower operating voltages. By enabling a variety of detector configurations, the airSEM is applicable to a wide range of environmental experiments including the imaging of hydrated biological specimens andin situchemical and electrochemical processes.« less

The application of polyethylene glycol (PEG) to electron microscopy

PubMed Central

1980-01-01

The cytoplasm of cells from a variety of tissues has been viewed in sections (0.25-1 micrometers) devoid of any embedding resin. Glutaraldehyde- and osmium tetroxide-fixed tissues were infiltrated and embedded in a water-miscible wax, polyethylene glycol (PEG), and subsequently sectioned on dry glass or diamond knives. The PEG matrix was removed and the sections were placed on Formvarcarbon-polylysine- coated grids, dehydrated, dried by the critical-point method, and observed in either the high- or low-voltage electron microscope. Stereoscopic views of cells devoid of embedding resin present an image of cell utrastructure unobscured by electron-scattering resins similar to the image of whole, unembedded critical-point-dried or freeze-dried cultured cells observed by transmission electron microscopy. All organelles, including the cytoskeletal structures, are identified and appear not to have been damaged during processing, although membrane components appear somewhat less distinct. The absence of an embedding matrix eliminates the need for additional staining to increase contrast, unlike the situation with specimens embedded in standard electron-scattering resins. The PEG technique thus appears to be a valuable adjunct to conventional methods for ultrastructural analysis. PMID:7400222

The application of polyethylene glycol (PEG) to electron microscopy.

PubMed

Wolosewick, J J

1980-08-01

The cytoplasm of cells from a variety of tissues has been viewed in sections (0.25-1 micrometers) devoid of any embedding resin. Glutaraldehyde- and osmium tetroxide-fixed tissues were infiltrated and embedded in a water-miscible wax, polyethylene glycol (PEG), and subsequently sectioned on dry glass or diamond knives. The PEG matrix was removed and the sections were placed on Formvarcarbon-polylysine-coated grids, dehydrated, dried by the critical-point method, and observed in either the high- or low-voltage electron microscope. Stereoscopic views of cells devoid of embedding resin present an image of cell utrastructure unobscured by electron-scattering resins similar to the image of whole, unembedded critical-point-dried or freeze-dried cultured cells observed by transmission electron microscopy. All organelles, including the cytoskeletal structures, are identified and appear not to have been damaged during processing, although membrane components appear somewhat less distinct. The absence of an embedding matrix eliminates the need for additional staining to increase contrast, unlike the situation with specimens embedded in standard electron-scattering resins. The PEG technique thus appears to be a valuable adjunct to conventional methods for ultrastructural analysis.

EMRinger: side chain–directed model and map validation for 3D cryo-electron microscopy

DOE PAGES

Barad, Benjamin A.; Echols, Nathaniel; Wang, Ray Yu-Ruei; ...

2015-08-17

Advances in high-resolution cryo-electron microscopy (cryo-EM) require the development of validation metrics to independently assess map quality and model geometry. We report that EMRinger is a tool that assesses the precise fitting of an atomic model into the map during refinement and shows how radiation damage alters scattering from negatively charged amino acids. EMRinger (https://github.com/fraser-lab/EMRinger) will be useful for monitoring progress in resolving and modeling high-resolution features in cryo-EM.

Novel Crystalline SiO2 Nanoparticles via Annelids Bioprocessing of Agro-Industrial Wastes

PubMed Central

2010-01-01

The synthesis of nanoparticles silica oxide from rice husk, sugar cane bagasse and coffee husk, by employing vermicompost with annelids (Eisenia foetida) is reported. The product (humus) is calcinated and extracted to recover the crystalline nanoparticles. X-ray diffraction (XRD), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM) and dynamic light scattering (DLS) show that the biotransformation allows creating specific crystalline phases, since equivalent particles synthesized without biotransformation are bigger and with different crystalline structure. PMID:20802789

Elucidating the Wavelength Dependence of Phonon Scattering in Nanoparticle-Matrix Composites using Phonon Spectroscopy

DTIC Science & Technology

2016-07-11

composites with x - ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), Rutherford backscattering spectroscopy...RBS), particle-induced x - ray emission (PIXE), and energy dispersive x - ray spectroscopy (EDX). This work complements earlier works on CdSe...sample shows only In2Se3 and CdIn2Se4 XRD peaks (Figure 1.4e), it is stoichiometrically   Figure 1.4. X - ray diffraction patterns of (a) γ-In2Se3

X-ray microscopy as an approach to increasing accuracy and efficiency of serial block-face imaging for correlated light and electron microscopy of biological specimens.

PubMed

Bushong, Eric A; Johnson, Donald D; Kim, Keun-Young; Terada, Masako; Hatori, Megumi; Peltier, Steven T; Panda, Satchidananda; Merkle, Arno; Ellisman, Mark H

2015-02-01

The recently developed three-dimensional electron microscopic (EM) method of serial block-face scanning electron microscopy (SBEM) has rapidly established itself as a powerful imaging approach. Volume EM imaging with this scanning electron microscopy (SEM) method requires intense staining of biological specimens with heavy metals to allow sufficient back-scatter electron signal and also to render specimens sufficiently conductive to control charging artifacts. These more extreme heavy metal staining protocols render specimens light opaque and make it much more difficult to track and identify regions of interest (ROIs) for the SBEM imaging process than for a typical thin section transmission electron microscopy correlative light and electron microscopy study. We present a strategy employing X-ray microscopy (XRM) both for tracking ROIs and for increasing the efficiency of the workflow used for typical projects undertaken with SBEM. XRM was found to reveal an impressive level of detail in tissue heavily stained for SBEM imaging, allowing for the identification of tissue landmarks that can be subsequently used to guide data collection in the SEM. Furthermore, specific labeling of individual cells using diaminobenzidine is detectable in XRM volumes. We demonstrate that tungsten carbide particles or upconverting nanophosphor particles can be used as fiducial markers to further increase the precision and efficiency of SBEM imaging.

X-ray Microscopy as an Approach to Increasing Accuracy and Efficiency of Serial Block-face Imaging for Correlated Light and Electron Microscopy of Biological Specimens

PubMed Central

Bushong, Eric A.; Johnson, Donald D.; Kim, Keun-Young; Terada, Masako; Hatori, Megumi; Peltier, Steven T.; Panda, Satchidananda; Merkle, Arno; Ellisman, Mark H.

2015-01-01

The recently developed three-dimensional electron microscopic (EM) method of serial block-face scanning electron microscopy (SBEM) has rapidly established itself as a powerful imaging approach. Volume EM imaging with this scanning electron microscopy (SEM) method requires intense staining of biological specimens with heavy metals to allow sufficient back-scatter electron signal and also to render specimens sufficiently conductive to control charging artifacts. These more extreme heavy metal staining protocols render specimens light opaque and make it much more difficult to track and identify regions of interest (ROIs) for the SBEM imaging process than for a typical thin section transmission electron microscopy correlative light and electron microscopy study. We present a strategy employing X-ray microscopy (XRM) both for tracking ROIs and for increasing the efficiency of the workflow used for typical projects undertaken with SBEM. XRM was found to reveal an impressive level of detail in tissue heavily stained for SBEM imaging, allowing for the identification of tissue landmarks that can be subsequently used to guide data collection in the SEM. Furthermore, specific labeling of individual cells using diaminobenzidine is detectable in XRM volumes. We demonstrate that tungsten carbide particles or upconverting nanophosphor particles can be used as fiducial markers to further increase the precision and efficiency of SBEM imaging. PMID:25392009

Characterization of conductive nanobiomaterials derived from viral assemblies by low-voltage STEM imaging and Raman scattering

NASA Astrophysics Data System (ADS)

Plascencia-Villa, Germán; Carreño-Fuentes, Liliana; Bahena, Daniel; José-Yacamán, Miguel; Palomares, Laura A.; Ramírez, Octavio T.

2014-09-01

New technologies require the development of novel nanomaterials that need to be fully characterized to achieve their potential. High-resolution low-voltage scanning transmission electron microscopy (STEM) has proven to be a very powerful technique in nanotechnology, but its use for the characterization of nanobiomaterials has been limited. Rotavirus VP6 self-assembles into nanotubular assemblies that possess an intrinsic affinity for Au ions. This property was exploited to produce hybrid nanobiomaterials by the in situ functionalization of recombinant VP6 nanotubes with gold nanoparticles. In this work, Raman spectroscopy and advanced analytical electron microscopy imaging with spherical aberration-corrected (Cs) STEM and nanodiffraction at low-voltage doses were employed to characterize nanobiomaterials. STEM imaging revealed the precise structure and arrangement of the protein templates, as well as the nanostructure and atomic arrangement of gold nanoparticles with high spatial sub-Angstrom resolution and avoided radiation damage. The imaging was coupled with backscattered electron imaging, ultra-high resolution scanning electron microscopy and x-ray spectroscopy. The hybrid nanobiomaterials that were obtained showed unique properties as bioelectronic conductive devices and showed enhanced Raman scattering by their precise arrangement into superlattices, displaying the utility of viral assemblies as functional integrative self-assembled nanomaterials for novel applications.

Coupling EELS/EFTEM Imaging with Environmental Fluid Cell Microscopy

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

Unocic, Raymond R; Baggetto, Loic; Veith, Gabriel M

2012-01-01

Insight into dynamically evolving electrochemical reactions and mechanisms encountered in electrical energy storage (EES) and conversion technologies (batteries, fuel cells, and supercapacitors), materials science (corrosion and oxidation), and materials synthesis (electrodeposition) remains limited due to the present lack of in situ high-resolution characterization methodologies. Electrochemical fluid cell microscopy is an emerging in-situ method that allows for the direct, real-time imaging of electrochemical processes within a fluid environment. This technique is facilitated by the use of MEMS-based biasing microchip platforms that serve the purpose of sealing the highly volatile electrolyte between two electron transparent SiNx membranes and interfacing electrodes to anmore » external potentiostat for controlled nanoscale electrochemislly experiments [!]. In order to elucidate both stmctural and chemical changes during such in situ electrochemical experiments, it is impmtant to first improve upon the spatial resolution by utilizing energy-filtered transmission electron microscopy (EFTEM) (to minimize chromatic aben ation), then to detennine the chemical changes via electron energy loss spectroscopy (EELS). This presents a formidable challenge since the overall thickness through which electrons are scattered through the multiple layers of the cell can be on the order of hundreds of nanometers to microns, scattering through which has the deleterious effect of degrading image resolution and decreasing signal-to noise for spectroscopy [2].« less

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.

Salt-induced aggregation and fusion of dioctadecyldimethylammonium chloride and sodium dihexadecylphosphate vesicles.

PubMed Central

Carmona-Ribeiro, A M; Chaimovich, H

1986-01-01

Small dioctadecyldimethylammonium chloride (DODAC) vesicles prepared by sonication fuse upon addition of NaCl as detected by several methods (electron microscopy, trapped volume determinations, temperature-dependent phase transition curves, and osmometer behavior. In contrast, small sodium dihexadecyl phosphate (DHP) vesicles mainly aggregate upon NaCl addition as shown by electron microscopy and the lack of osmometer behavior. Scatter-derived absorbance changes of small and large DODAC or DHP vesicles as a function of time after salt addition were obtained for a range of NaCl or amphiphile concentration. These changes were interpreted in accordance with a phenomenological model based upon fundamental light-scattering laws and simple geometrical considerations. Short-range hydration repulsion between DODAC (or DHP) vesicles is possibly the main energy barrier for the fusion process. Images FIGURE 2 FIGURE 9 PMID:3779002

Quasiparticle scattering in type-II Weyl semimetal MoTe2

NASA Astrophysics Data System (ADS)

Lin, Chun-Liang; Arafune, Ryuichi; Minamitani, Emi; Kawai, Maki; Takagi, Noriaki

2018-03-01

The electronic structure of type-II Weyl semimetal molybdenum ditelluride (MoTe2) is studied by using scanning tunneling microscopy and density functional theory calculations. Through measuring energy-dependent quasiparticle interference (QPI) patterns with a cryogenic scanning tunneling microscope, several characteristic features are found in the QPI patterns. Two of them arise from the Weyl semimetal nature; one is the topological Fermi arc surface state and the other can be assigned to be a Weyl point. The remaining structures are derived from the scatterings relevant to the bulk electronic states. The findings lead to further understanding of the topological electronic structure of type-II Weyl semimetal MoTe2.

Quasiparticle scattering in type-II Weyl semimetal MoTe2.

PubMed

Lin, Chun-Liang; Arafune, Ryuichi; Minamitani, Emi; Kawai, Maki; Takagi, Noriaki

2018-02-15

The electronic structure of type-II Weyl semimetal molybdenum ditelluride (MoTe 2 ) is studied by using scanning tunneling microscopy and density functional theory calculations. Through measuring energy-dependent quasiparticle interference (QPI) patterns with a cryogenic scanning tunneling microscope, several characteristic features are found in the QPI patterns. Two of them arise from the Weyl semimetal nature; one is the topological Fermi arc surface state and the other can be assigned to be a Weyl point. The remaining structures are derived from the scatterings relevant to the bulk electronic states. The findings lead to further understanding of the topological electronic structure of type-II Weyl semimetal MoTe 2 .

Fully nonlocal inelastic scattering computations for spectroscopical transmission electron microscopy methods

NASA Astrophysics Data System (ADS)

Rusz, Ján; Lubk, Axel; Spiegelberg, Jakob; Tyutyunnikov, Dmitry

2017-12-01

The complex interplay of elastic and inelastic scattering amenable to different levels of approximation constitutes the major challenge for the computation and hence interpretation of TEM-based spectroscopical methods. The two major approaches to calculate inelastic scattering cross sections of fast electrons on crystals—Yoshioka-equations-based forward propagation and the reciprocal wave method—are founded in two conceptually differing schemes—a numerical forward integration of each inelastically scattered wave function, yielding the exit density matrix, and a computation of inelastic scattering matrix elements using elastically scattered initial and final states (double channeling). Here, we compare both approaches and show that the latter is computationally competitive to the former by exploiting analytical integration schemes over multiple excited states. Moreover, we show how to include full nonlocality of the inelastic scattering event, neglected in the forward propagation approaches, at no additional computing costs in the reciprocal wave method. Detailed simulations show in some cases significant errors due to the z -locality approximation and hence pitfalls in the interpretation of spectroscopical TEM results.

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

Phosphorus detection in vitrified bacteria by cryo-STEM annular dark-field analysis.

PubMed

Wolf, Sharon Grayer; Rez, Peter; Elbaum, Michael

2015-11-01

Bacterial cells often contain dense granules. Among these, polyphosphate bodies (PPBs) store inorganic phosphate for a variety of essential functions. Identification of PPBs has until now been accomplished by analytical methods that required drying or chemically fixing the cells. These methods entail large electron doses that are incompatible with low-dose imaging of cryogenic specimens. We show here that Scanning Transmission Electron Microscopy (STEM) of fully hydrated, intact, vitrified bacteria provides a simple means for mapping of phosphorus-containing dense granules based on quantitative sensitivity of the electron scattering to atomic number. A coarse resolution of the scattering angles distinguishes phosphorus from the abundant lighter atoms: carbon, nitrogen and oxygen. The theoretical basis is similar to Z contrast of materials science. EDX provides a positive identification of phosphorus, but importantly, the method need not involve a more severe electron dose than that required for imaging. The approach should prove useful in general for mapping of heavy elements in cryopreserved specimens when the element identity is known from the biological context. © 2015 The Authors Journal of Microscopy © 2015 Royal Microscopical Society.

Multimodal Nonlinear Optical Microscopy

PubMed Central

Yue, Shuhua; Slipchenko, Mikhail N.; Cheng, Ji-Xin

2013-01-01

Because each nonlinear optical (NLO) imaging modality is sensitive to specific molecules or structures, multimodal NLO imaging capitalizes the potential of NLO microscopy for studies of complex biological tissues. The coupling of multiphoton fluorescence, second harmonic generation, and coherent anti-Stokes Raman scattering (CARS) has allowed investigation of a broad range of biological questions concerning lipid metabolism, cancer development, cardiovascular disease, and skin biology. Moreover, recent research shows the great potential of using CARS microscope as a platform to develop more advanced NLO modalities such as electronic-resonance-enhanced four-wave mixing, stimulated Raman scattering, and pump-probe microscopy. This article reviews the various approaches developed for realization of multimodal NLO imaging as well as developments of new NLO modalities on a CARS microscope. Applications to various aspects of biological and biomedical research are discussed. PMID:24353747

Simplifying Electron Beam Channeling in Scanning Transmission Electron Microscopy (STEM).

PubMed

Wu, Ryan J; Mittal, Anudha; Odlyzko, Michael L; Mkhoyan, K Andre

2017-08-01

Sub-angstrom scanning transmission electron microscopy (STEM) allows quantitative column-by-column analysis of crystalline specimens via annular dark-field images. The intensity of electrons scattered from a particular location in an atomic column depends on the intensity of the electron probe at that location. Electron beam channeling causes oscillations in the STEM probe intensity during specimen propagation, which leads to differences in the beam intensity incident at different depths. Understanding the parameters that control this complex behavior is critical for interpreting experimental STEM results. In this work, theoretical analysis of the STEM probe intensity reveals that intensity oscillations during specimen propagation are regulated by changes in the beam's angular distribution. Three distinct regimes of channeling behavior are observed: the high-atomic-number (Z) regime, in which atomic scattering leads to significant angular redistribution of the beam; the low-Z regime, in which the probe's initial angular distribution controls intensity oscillations; and the intermediate-Z regime, in which the behavior is mixed. These contrasting regimes are shown to exist for a wide range of probe parameters. These results provide a new understanding of the occurrence and consequences of channeling phenomena and conditions under which their influence is strengthened or weakened by characteristics of the electron probe and sample.

Laser pulse power transmission limits of silica fibers with antireflective coating

NASA Astrophysics Data System (ADS)

Meister, St.; Wosniok, A.; Seewald, G.; Scharfenorth, Ch.; Eichler, H. J.

2005-04-01

Multimode optical fibers are used for the transmission of high power laser pulses and as phase conjugated mirrors by stimulated Brillouin scattering. Both applications are enhanced by antireflection coatings on the fiber end-faces. Fiber transmissions reach more than 99.5% for pulse energies below the threshold of stimulated Brillouin scattering. Laser-induced damage thresholds of the fibers coated with Ta2O5 / SiO2 were measured at 1064 nm and 24 ns pulse duration. A damage threshold of up to 101 J/cm2 could be achieved. The damage morphology was investigated using atomic force microscopy and scanning electron microscopy.

Nano-sized graphene flakes: insights from experimental synthesis and first principles calculations.

PubMed

Lin, Pin-Chun; Chen, Yi-Rui; Hsu, Kuei-Ting; Lin, Tzu-Neng; Tung, Kuo-Lun; Shen, Ji-Lin; Liu, Wei-Ren

2017-03-01

In this study, we proposed a cost-effective method for preparing graphene nano-flakes (GNFs) derived from carbon nanotubes (CNTs) via three steps (pressing, homogenization and sonication exfoliation processes). Scanning electron microscopy (SEM), transmission electron microscopy (TEM), atomic force microscopy (AFM), laser scattering, as well as ultraviolet-visible and photoluminescence (PL) measurements were carried out. The results indicated that the size of as-synthesized GNFs was approximately 40-50 nm. Furthermore, we also used first principles calculations to understand the transformation from CNTs to GNFs from the viewpoints of the edge formation energies of GNFs in different shapes and sizes. The corresponding photoluminescence measurements of GNFs were carried out in this work.

Strategies for Multi-Modal Analysis

NASA Astrophysics Data System (ADS)

Hexemer, Alexander; Wang, Cheng; Pandolfi, Ronald; Kumar, Dinesh; Venkatakrishnan, Singanallur; Sethian, James; Camera Team

This section on soft materials will be dedicated to discuss the extraction of the chemical distribution and spatial arrangement of constituent elements and functional groups at multiple length scales and, thus, the examination of collective dynamics, transport, and electronic ordering phenomena. Traditional measures of structure in soft materials have relied heavily on scattering and imaging based techniques due to their capacity to measure nanoscale dimensions and their capacity to monitor structure under conditions of dynamic stress loading. Special attentions are planned to focus on the application of resonant x-ray scattering, contrast-varied neutron scattering, analytical transmission electron microscopy, and their combinations. This session aims to bring experts in both scattering and electron microscope fields to discuss recent advances in selectively characterizing structural architectures of complex soft materials, which have often multi-components with a wide range of length scales and multiple functionalities, and thus hopes to foster novel ideas to decipher a higher level of structural complexity in soft materials in future. CAMERA, Early Career Award.

A correlative approach to segmenting phases and ferrite morphologies in transformation-induced plasticity steel using electron back-scattering diffraction and energy dispersive X-ray spectroscopy.

PubMed

Gazder, Azdiar A; Al-Harbi, Fayez; Spanke, Hendrik Th; Mitchell, David R G; Pereloma, Elena V

2014-12-01

Using a combination of electron back-scattering diffraction and energy dispersive X-ray spectroscopy data, a segmentation procedure was developed to comprehensively distinguish austenite, martensite, polygonal ferrite, ferrite in granular bainite and bainitic ferrite laths in a thermo-mechanically processed low-Si, high-Al transformation-induced plasticity steel. The efficacy of the ferrite morphologies segmentation procedure was verified by transmission electron microscopy. The variation in carbon content between the ferrite in granular bainite and bainitic ferrite laths was explained on the basis of carbon partitioning during their growth. Copyright © 2014 Elsevier B.V. All rights reserved.

Multifunctional Metallosupramolecular Materials

DTIC Science & Technology

2011-02-28

supramolecular polymers based on 16 and Zn(NTf2)2 using small- angle X - ray scattering (SAXS) and transmission electron microscopy (TEM), carried out by...The SAXS data (Figure 13a) show multiple strong Bragg diffraction maxima at integer multiples of the scattering vector of the primary diffraction ...a minor amount of residual double bonds in the poly(ethylene-co-butylene) core. The metallopolymers 16·[Zn(NTf2)2] x exhibit similar traces, but do

Sub-diffraction-limit localization imaging of a plasmonic nanoparticle pair with wavelength-resolved dark-field microscopy.

PubMed

Wei, Lin; Ma, Yanhong; Zhu, Xupeng; Xu, Jianghong; Wang, Yaxin; Duan, Huigao; Xiao, Lehui

2017-06-29

In this work, with wavelength-resolved dark-field microscopy, the center-of-mass localization information from nanoparticle pairs (i.e., spherical (45 nm in diameter) and rod (45 × 70 nm) shaped gold nanoparticle pairs with different gap distances and orientations) was explored and compared with the results determined by scanning electron microscopy (SEM) measurements. When the gap distance was less than 20 nm, the scattering spectrum of the nanoparticle pair was seriously modulated by the plasmonic coupling effect. The measured coordinate information determined by the optical method (Gaussian fitting) was not consistent with the true results determined by SEM measurement. A good correlation between the optical and SEM measurements was achieved when the gap distance was further increased (e.g., 20, 40 and 60 nm). Under these conditions, well-defined scattering peaks assigned to the corresponding individual nanoparticles could be distinguished from the obtained scattering spectrum. These results would afford valuable information for the studies on single plasmonic nanoparticle imaging applications with the optical microscopy method such as super-localization imaging, high precision single particle tracking in a crowding environment and so on.

Low-voltage electron microscopy of polymer and organic molecular thin films.

PubMed

Drummy, Lawrence F; Yang, Junyan; Martin, David C

2004-06-01

We have demonstrated the capabilities of a novel low-voltage electron microscope (LVEM) for imaging polymer and organic molecular thin films. The LVEM can operate in transmission electron microscopy, scanning transmission electron microscopy, scanning electron microscopy, and electron diffraction modes. The microscope operates at a nominal accelerating voltage of 5 kV and fits on a tabletop. A detailed discussion of the electron-sample interaction processes is presented, and the mean free path for total electron scattering was calculated to be 15 nm for organic samples at 5 kV. The total end point dose for the destruction of crystallinity at 5 kV was estimated at 5 x 10(-4) and 3.5 x 10(-2) C/cm2 for polyethylene and pentacene, respectively. These values are significantly lower than those measured at voltages greater than 100 kV. A defocus series of colloidal gold particles allowed us to estimate the experimental contrast transfer function of the microscope. Images taken of several organic materials have shown high contrast for low atomic number elements and a resolution of 2.5 nm. The materials studied here include thin films of the organic semiconductor pentacene, triblock copolymer films, single-molecule dendrimers, electrospun polymer fibers and gold nanoparticles. Copyright 2004 Elsevier B.V.

Studying aerosol light scattering based on aspect ratio distribution observed by fluorescence microscope.

PubMed

Li, Li; Zheng, Xu; Li, Zhengqiang; Li, Zhanhua; Dubovik, Oleg; Chen, Xingfeng; Wendisch, Manfred

2017-08-07

Particle shape is crucial to the properties of light scattered by atmospheric aerosol particles. A method of fluorescence microscopy direct observation was introduced to determine the aspect ratio distribution of aerosol particles. The result is comparable with that of the electron microscopic analysis. The measured aspect ratio distribution has been successfully applied in modeling light scattering and further in simulation of polarization measurements of the sun/sky radiometer. These efforts are expected to improve shape retrieval from skylight polarization by using directly measured aspect ratio distribution.

Detection of atomic force microscopy cantilever displacement with a transmitted electron beam

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

Wagner, R.; Woehl, T. J.; Keller, R. R.

2016-07-25

The response time of an atomic force microscopy (AFM) cantilever can be decreased by reducing cantilever size; however, the fastest AFM cantilevers are currently nearing the smallest size that can be detected with the conventional optical lever approach. Here, we demonstrate an electron beam detection scheme for measuring AFM cantilever oscillations. The oscillating AFM tip is positioned perpendicular to and in the path of a stationary focused nanometer sized electron beam. As the tip oscillates, the thickness of the material under the electron beam changes, causing a fluctuation in the number of scattered transmitted electrons that are detected. We demonstratemore » detection of sub-nanometer vibration amplitudes with an electron beam, providing a pathway for dynamic AFM with cantilevers that are orders of magnitude smaller and faster than the current state of the art.« less

Scattered electrons in microscopy and microanalysis

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

Ottensmeyer, F.P.

The use of scattered electrons alone for direct imaging of biological specimens makes it possible to obtain structural information at atomic and near-atomic spatial resolutions of 0.3 to 0.5 nanometer. While this is not as good as the resolution possible with x-ray crystallography, such an approach provides structural information rapidly on individual macromolecules that have not been, and possibly cannot be, crystallized. Analysis of the spectrum of energies of scattered electrons and imaging of the latter with characteristic energy bands within the spectrum produces a powerful new technique of atomic microanalysis. This technique, which has a spatial resolution of aboutmore » 0.5 nanometer and a minimum detection sensitivity of about 50 atoms of phosphorus, is especially useful for light atom analysis and appears to have applications in molecular biology, cell biology, histology, pathology, botany, and many other fields.« less

Scattered electrons in microscopy and microanalysis

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

Ottensmeyer, F.P.

The use of scattered electrons alone for direct imaging of biological specimens makes it possible to obtain structural information at atomic and near-atomic spatial resolutions of 0.3 to 0.5 nanometer. While this is not as good as the resolution possible with x-ray crystallography, such an approach provides structural information rapidly on individual macromolecules that have not been, and possibly cannot be, crystallized. Analysis of the spectrum of energies of scattered electrons and imaging of the latter with characteristic energy bands within the spectrum produce a powerful new technique of atomic microanalysis. This technique, which has a spatial resolution of aboutmore » 0.5 nanometer and a minimum detection sensitivity of about 50 atoms of phosphorus, is especially useful for light atom analysis and appears to have applications in molecular biology, cell biology, histology, pathology, botany, and many other fields.« less

Quantitative Imaging of Single Unstained Magnetotactic Bacteria by Coherent X-ray Diffraction Microscopy.

PubMed

Fan, Jiadong; Sun, Zhibin; Zhang, Jian; Huang, Qingjie; Yao, Shengkun; Zong, Yunbing; Kohmura, Yoshiki; Ishikawa, Tetsuya; Liu, Hong; Jiang, Huaidong

2015-06-16

Novel coherent diffraction microscopy provides a powerful lensless imaging method to obtain a better understanding of the microorganism at the nanoscale. Here we demonstrated quantitative imaging of intact unstained magnetotactic bacteria using coherent X-ray diffraction microscopy combined with an iterative phase retrieval algorithm. Although the signal-to-noise ratio of the X-ray diffraction pattern from single magnetotactic bacterium is weak due to low-scattering ability of biomaterials, an 18.6 nm half-period resolution of reconstructed image was achieved by using a hybrid input-output phase retrieval algorithm. On the basis of the quantitative reconstructed images, the morphology and some intracellular structures, such as nucleoid, polyβ-hydroxybutyrate granules, and magnetosomes, were identified, which were also confirmed by scanning electron microscopy and energy dispersive spectroscopy. With the benefit from the quantifiability of coherent diffraction imaging, for the first time to our knowledge, an average density of magnetotactic bacteria was calculated to be ∼1.19 g/cm(3). This technique has a wide range of applications, especially in quantitative imaging of low-scattering biomaterials and multicomponent materials at nanoscale resolution. Combined with the cryogenic technique or X-ray free electron lasers, the method could image cells in a hydrated condition, which helps to maintain their natural structure.

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

Matsutani, Takaomi; Taya, Masaki; Ikuta, Takashi

A parallel image detection system using an annular pupil for electron optics were developed to realize an increase in the depth of focus, aberration-free imaging and separation of amplitude and phase images under scanning transmission electron microscopy (STEM). Apertures for annular pupils able to suppress high-energy electron scattering were developed using a focused ion beam (FIB) technique. The annular apertures were designed with outer diameter of oe 40 {mu}m and inner diameter of oe32 {mu}m. A taper angle varying from 20 deg. to 1 deg. was applied to the slits of the annular apertures to suppress the influence of high-energymore » electron scattering. Each azimuth angle image on scintillator was detected by a multi-anode photomultiplier tube assembly through 40 optical fibers bundled in a ring shape. To focus the image appearing on the scintillator on optical fibers, an optical lens relay system attached with CCD camera was developed. The system enables the taking of 40 images simultaneously from different scattered directions.« less

Characterization of magnetic nanoparticle by dynamic light scattering

PubMed Central

2013-01-01

Here we provide a complete review on the use of dynamic light scattering (DLS) to study the size distribution and colloidal stability of magnetic nanoparticles (MNPs). The mathematical analysis involved in obtaining size information from the correlation function and the calculation of Z-average are introduced. Contributions from various variables, such as surface coating, size differences, and concentration of particles, are elaborated within the context of measurement data. Comparison with other sizing techniques, such as transmission electron microscopy and dark-field microscopy, revealed both the advantages and disadvantages of DLS in measuring the size of magnetic nanoparticles. The self-assembly process of MNP with anisotropic structure can also be monitored effectively by DLS. PMID:24011350

Viewing Integrated-Circuit Interconnections By SEM

NASA Technical Reports Server (NTRS)

Lawton, Russel A.; Gauldin, Robert E.; Ruiz, Ronald P.

1990-01-01

Back-scattering of energetic electrons reveals hidden metal layers. Experiment shows that with suitable operating adjustments, scanning electron microscopy (SEM) used to look for defects in aluminum interconnections in integrated circuits. Enables monitoring, in situ, of changes in defects caused by changes in temperature. Gives truer picture of defects, as etching can change stress field of metal-and-passivation pattern, causing changes in defects.

Bandgap Inhomogeneity of a PbSe Quantum Dot Ensemble from Two-Dimensional Spectroscopy and Comparison to Size Inhomogeneity from Electron Microscopy

DOE PAGES

Park, Samuel D.; Baranov, Dmitry; Ryu, Jisu; ...

2017-01-03

Femtosecond two-dimensional Fourier transform spectroscopy is used to determine the static bandgap inhomogeneity of a colloidal quantum dot ensemble. The excited states of quantum dots absorb light, so their absorptive two-dimensional (2D) spectra will typically have positive and negative peaks. We show that the absorption bandgap inhomogeneity is robustly determined by the slope of the nodal line separating positive and negative peaks in the 2D spectrum around the bandgap transition; this nodal line slope is independent of excited state parameters not known from the absorption and emission spectra. The absorption bandgap inhomogeneity is compared to a size and shape distributionmore » determined by electron microscopy. The electron microscopy images are analyzed using new 2D histograms that correlate major and minor image projections to reveal elongated nanocrystals, a conclusion supported by grazing incidence small-angle X-ray scattering and high-resolution transmission electron microscopy. Lastly, the absorption bandgap inhomogeneity quantitatively agrees with the bandgap variations calculated from the size and shape distribution, placing upper bounds on any surface contributions.« less

Probing Dirac fermion dynamics in topological insulator Bi2Se3 films with a scanning tunneling microscope.

PubMed

Song, Can-Li; Wang, Lili; He, Ke; Ji, Shuai-Hua; Chen, Xi; Ma, Xu-Cun; Xue, Qi-Kun

2015-05-01

Scanning tunneling microscopy and spectroscopy have been used to investigate the femtosecond dynamics of Dirac fermions in the topological insulator Bi2Se3 ultrathin films. At the two-dimensional limit, bulk electrons become quantized and the quantization can be controlled by the film thickness at a single quintuple layer level. By studying the spatial decay of standing waves (quasiparticle interference patterns) off steps, we measure directly the energy and film thickness dependence of the phase relaxation length lϕ and inelastic scattering lifetime τ of topological surface-state electrons. We find that τ exhibits a remarkable (E - EF)(-2) energy dependence and increases with film thickness. We show that the features revealed are typical for electron-electron scattering between surface and bulk states.

Thin-Film Phase Plates for Transmission Electron Microscopy Fabricated from Metallic Glasses.

PubMed

Dries, Manuel; Hettler, Simon; Schulze, Tina; Send, Winfried; Müller, Erich; Schneider, Reinhard; Gerthsen, Dagmar; Luo, Yuansu; Samwer, Konrad

2016-10-01

Thin-film phase plates (PPs) have become an interesting tool to enhance the contrast of weak-phase objects in transmission electron microscopy (TEM). The thin film usually consists of amorphous carbon, which suffers from quick degeneration under the intense electron-beam illumination. Recent investigations have focused on the search for alternative materials with an improved material stability. This work presents thin-film PPs fabricated from metallic glass alloys, which are characterized by a high electrical conductivity and an amorphous structure. Thin films of the zirconium-based alloy Zr65.0Al7.5Cu27.5 (ZAC) were fabricated and their phase-shifting properties were evaluated. The ZAC film was investigated by different TEM techniques, which reveal beneficial properties compared with amorphous carbon PPs. Particularly favorable is the small probability for inelastic plasmon scattering, which results from the combined effect of a moderate inelastic mean free path and a reduced film thickness due to a high mean inner potential. Small probability plasmon scattering improves contrast transfer at high spatial frequencies, which makes the ZAC alloy a promising material for PP fabrication.

Relative merits and limiting factors for x-ray and electron microscopy of thick, hydrated organic materials

DOE PAGES

Du, Ming; Jacobsen, Chris

2017-10-07

Electron and x-ray microscopes allow one to image the entire, unlabeled structure of hydrated materials at a resolution well beyond what visible light microscopes can achieve. However, both approaches involve ionizing radiation, so that radiation damage must be considered as one of the limits to imaging. Drawing upon earlier work, we describe here a unified approach to estimating the image contrast (and thus the required exposure and corresponding radiation dose) in both x-ray and electron microscopy. This approach accounts for factors such as plural and inelastic scattering, and (in electron microscopy) the use of energy filters to obtain so-called "zeromore » loss" images. As expected, it shows that electron microscopy offers lower dose for specimens thinner than about 1 mu m (such as for studies of macromolecules, viruses, bacteria and archaebacteria, and thin sectioned material), while x-ray microscopy offers superior characteristics for imaging thicker specimen such as whole eukaryotic cells, thick-sectioned tissues, and organs. The required radiation dose scales strongly as a function of the desired spatial resolution, allowing one to understand the limits of live and frozen hydrated specimen imaging. Lastly, we consider the factors limiting x-ray microscopy of thicker materials, suggesting that specimens as thick as a whole mouse brain can be imaged with x-ray microscopes without significant image degradation should appropriate image reconstruction methods be identified.« less

Relative merits and limiting factors for x-ray and electron microscopy of thick, hydrated organic materials

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

Du, Ming; Jacobsen, Chris

Electron and x-ray microscopes allow one to image the entire, unlabeled structure of hydrated materials at a resolution well beyond what visible light microscopes can achieve. However, both approaches involve ionizing radiation, so that radiation damage must be considered as one of the limits to imaging. Drawing upon earlier work, we describe here a unified approach to estimating the image contrast (and thus the required exposure and corresponding radiation dose) in both x-ray and electron microscopy. This approach accounts for factors such as plural and inelastic scattering, and (in electron microscopy) the use of energy filters to obtain so-called "zeromore » loss" images. As expected, it shows that electron microscopy offers lower dose for specimens thinner than about 1 mu m (such as for studies of macromolecules, viruses, bacteria and archaebacteria, and thin sectioned material), while x-ray microscopy offers superior characteristics for imaging thicker specimen such as whole eukaryotic cells, thick-sectioned tissues, and organs. The required radiation dose scales strongly as a function of the desired spatial resolution, allowing one to understand the limits of live and frozen hydrated specimen imaging. Lastly, we consider the factors limiting x-ray microscopy of thicker materials, suggesting that specimens as thick as a whole mouse brain can be imaged with x-ray microscopes without significant image degradation should appropriate image reconstruction methods be identified.« less

Milligram-per-second femtosecond laser production of Se nanoparticle inks and ink-jet printing of nanophotonic 2D-patterns

NASA Astrophysics Data System (ADS)

Ionin, Andrey; Ivanova, Anastasia; Khmel'nitskii, Roman; Klevkov, Yury; Kudryashov, Sergey; Mel'nik, Nikolay; Nastulyavichus, Alena; Rudenko, Andrey; Saraeva, Irina; Smirnov, Nikita; Zayarny, Dmitry; Baranov, Anatoly; Kirilenko, Demid; Brunkov, Pavel; Shakhmin, Alexander

2018-04-01

Milligram-per-second production of selenium nanoparticles in water sols was realized through 7-W, 2 MHz-rate femtosecond laser ablation of a crystalline trigonal selenium pellet. High-yield particle formation mechanism and ultimate mass-removal yield were elucidated by optical profilometry and scanning electron microscopy characterization of the corresponding crater depths and topographies. Deposited selenium particles were inspected by scanning and transmission electron microscopy, while their hydrosols (nanoinks) were characterized by optical transmission, Raman and dynamic light scattering spectroscopy. 2D patterns and coatings were ink-jet printed on thin supported silver films and their bare silica glass substrates, as well as on IR-transparent CaF2 substrates, and characterized by electron microscopy, energy-dispersive x-ray spectroscopy, and broadband (vis-mid IR) transmission spectroscopy, exhibiting crystalline selenium nanoparticles with high refractive index as promising all-dielectric sensing building nanoblocks in nanophotonics.

Scanning Tunneling Microscopy Observation of Phonon Condensate

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

Altfeder, Igor; Balatsky, Alexander V.; Voevodin, Andrey A.

Using quantum tunneling of electrons into vibrating surface atoms, phonon oscillations can be observed on the atomic scale. Phonon interference patterns with unusually large signal amplitudes have been revealed by scanning tunneling microscopy in intercalated van der Waals heterostructures. Our results show that the effective radius of these phonon quasi-bound states, the real-space distribution of phonon standing wave amplitudes, the scattering phase shifts, and the nonlinear intermode coupling strongly depend on the presence of defect-induced scattering resonance. The observed coherence of these quasi-bound states most likely arises from phase- and frequency-synchronized dynamics of all phonon modes, and indicates the formationmore » of many-body condensate of optical phonons around resonant defects. We found that increasing the strength of the scattering resonance causes the increase of the condensate droplet radius without affecting the condensate fraction inside it. The condensate can be observed at room temperature.« less

Scanning Tunneling Microscopy Observation of Phonon Condensate

PubMed Central

Altfeder, Igor; Voevodin, Andrey A.; Check, Michael H.; Eichfeld, Sarah M.; Robinson, Joshua A.; Balatsky, Alexander V.

2017-01-01

Using quantum tunneling of electrons into vibrating surface atoms, phonon oscillations can be observed on the atomic scale. Phonon interference patterns with unusually large signal amplitudes have been revealed by scanning tunneling microscopy in intercalated van der Waals heterostructures. Our results show that the effective radius of these phonon quasi-bound states, the real-space distribution of phonon standing wave amplitudes, the scattering phase shifts, and the nonlinear intermode coupling strongly depend on the presence of defect-induced scattering resonance. The observed coherence of these quasi-bound states most likely arises from phase- and frequency-synchronized dynamics of all phonon modes, and indicates the formation of many-body condensate of optical phonons around resonant defects. We found that increasing the strength of the scattering resonance causes the increase of the condensate droplet radius without affecting the condensate fraction inside it. The condensate can be observed at room temperature. PMID:28225066

Scanning Tunneling Microscopy Observation of Phonon Condensate

DOE PAGES

Altfeder, Igor; Balatsky, Alexander V.; Voevodin, Andrey A.; ...

2017-02-22

Using quantum tunneling of electrons into vibrating surface atoms, phonon oscillations can be observed on the atomic scale. Phonon interference patterns with unusually large signal amplitudes have been revealed by scanning tunneling microscopy in intercalated van der Waals heterostructures. Our results show that the effective radius of these phonon quasi-bound states, the real-space distribution of phonon standing wave amplitudes, the scattering phase shifts, and the nonlinear intermode coupling strongly depend on the presence of defect-induced scattering resonance. The observed coherence of these quasi-bound states most likely arises from phase- and frequency-synchronized dynamics of all phonon modes, and indicates the formationmore » of many-body condensate of optical phonons around resonant defects. We found that increasing the strength of the scattering resonance causes the increase of the condensate droplet radius without affecting the condensate fraction inside it. The condensate can be observed at room temperature.« less

A streaming multi-GPU implementation of image simulation algorithms for scanning transmission electron microscopy

DOE PAGES

Pryor, Alan; Ophus, Colin; Miao, Jianwei

2017-10-25

Simulation of atomic-resolution image formation in scanning transmission electron microscopy can require significant computation times using traditional methods. A recently developed method, termed plane-wave reciprocal-space interpolated scattering matrix (PRISM), demonstrates potential for significant acceleration of such simulations with negligible loss of accuracy. In this paper, we present a software package called Prismatic for parallelized simulation of image formation in scanning transmission electron microscopy (STEM) using both the PRISM and multislice methods. By distributing the workload between multiple CUDA-enabled GPUs and multicore processors, accelerations as high as 1000 × for PRISM and 15 × for multislice are achieved relative to traditionalmore » multislice implementations using a single 4-GPU machine. We demonstrate a potentially important application of Prismatic, using it to compute images for atomic electron tomography at sufficient speeds to include in the reconstruction pipeline. Prismatic is freely available both as an open-source CUDA/C++ package with a graphical user interface and as a Python package, PyPrismatic.« less

A streaming multi-GPU implementation of image simulation algorithms for scanning transmission electron microscopy.

PubMed

Pryor, Alan; Ophus, Colin; Miao, Jianwei

2017-01-01

Simulation of atomic-resolution image formation in scanning transmission electron microscopy can require significant computation times using traditional methods. A recently developed method, termed plane-wave reciprocal-space interpolated scattering matrix (PRISM), demonstrates potential for significant acceleration of such simulations with negligible loss of accuracy. Here, we present a software package called Prismatic for parallelized simulation of image formation in scanning transmission electron microscopy (STEM) using both the PRISM and multislice methods. By distributing the workload between multiple CUDA-enabled GPUs and multicore processors, accelerations as high as 1000 × for PRISM and 15 × for multislice are achieved relative to traditional multislice implementations using a single 4-GPU machine. We demonstrate a potentially important application of Prismatic , using it to compute images for atomic electron tomography at sufficient speeds to include in the reconstruction pipeline. Prismatic is freely available both as an open-source CUDA/C++ package with a graphical user interface and as a Python package, PyPrismatic .

Time dependent changes in Schottky barrier mapping of the W/Si(001) interface utilizing ballistic electron emission microscopy

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

Durcan, Chris A.; Balsano, Robert; LaBella, Vincent P., E-mail: vlabella@albany.edu

2015-06-28

The W/Si(001) Schottky barrier height is mapped to nanoscale dimensions using ballistic electron emission microscopy (BEEM) over a period of 21 days to observe changes in the interface electrostatics. Initially, the average spectrum is fit to a Schottky barrier height of 0.71 eV, and the map is uniform with 98% of the spectra able to be fit. After 21 days, the average spectrum is fit to a Schottky barrier height of 0.62 eV, and the spatial map changes dramatically with only 27% of the spectra able to be fit. Transmission electron microscopy shows the formation of an ultra-thin tungsten silicide at themore » interface, which increases in thickness over the 21 days. This increase is attributed to an increase in electron scattering and the changes are observed in the BEEM measurements. Interestingly, little to no change is observed in the I-V measurements throughout the 21 day period.« less

A streaming multi-GPU implementation of image simulation algorithms for scanning transmission electron microscopy

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

Pryor, Alan; Ophus, Colin; Miao, Jianwei

Simulation of atomic-resolution image formation in scanning transmission electron microscopy can require significant computation times using traditional methods. A recently developed method, termed plane-wave reciprocal-space interpolated scattering matrix (PRISM), demonstrates potential for significant acceleration of such simulations with negligible loss of accuracy. In this paper, we present a software package called Prismatic for parallelized simulation of image formation in scanning transmission electron microscopy (STEM) using both the PRISM and multislice methods. By distributing the workload between multiple CUDA-enabled GPUs and multicore processors, accelerations as high as 1000 × for PRISM and 15 × for multislice are achieved relative to traditionalmore » multislice implementations using a single 4-GPU machine. We demonstrate a potentially important application of Prismatic, using it to compute images for atomic electron tomography at sufficient speeds to include in the reconstruction pipeline. Prismatic is freely available both as an open-source CUDA/C++ package with a graphical user interface and as a Python package, PyPrismatic.« less

Precipitation and Phase Transformations in 2101 Lean Duplex Stainless Steel During Isothermal Aging

NASA Astrophysics Data System (ADS)

Maetz, Jean-Yves; Cazottes, Sophie; Verdu, Catherine; Kleber, Xavier

2016-01-01

The effect of isothermal aging at 963 K (690 °C) on the microstructure of a 2101 lean duplex stainless steel, with the composition Fe-21.5Cr-5Mn-1.6Ni-0.22N-0.3Mo, was investigated using a multi-technique and multi-scale approach. The kinetics of phase transformation and precipitation was followed from a few minutes to thousands of hours using thermoelectric power measurements; based on these results, certain aging states were selected for electron microscopy characterization. Scanning electron microscopy, electron back-scattered diffraction, and transmission electron microscopy were used to quantitatively describe the microstructural evolution through crystallographic analysis, chemical analysis, and volume fraction measurements from the macroscopic scale down to the nanometric scale. During aging, the precipitation of M23C6 carbides, Cr2N nitrides, and σ phase as well as the transformation of ferrite into austenite and austenite into martensite was observed. These complex microstructural changes are controlled by Cr volume diffusion. The precipitation and phase transformation mechanisms are described.

Possibility to Probe Negative Values of a Wigner Function in Scattering of a Coherent Superposition of Electronic Wave Packets by Atoms.

PubMed

Karlovets, Dmitry V; Serbo, Valeriy G

2017-10-27

Within a plane-wave approximation in scattering, an incoming wave packet's Wigner function stays positive everywhere, which obscures such purely quantum phenomena as nonlocality and entanglement. With the advent of the electron microscopes with subnanometer-sized beams, one can enter a genuinely quantum regime where the latter effects become only moderately attenuated. Here we show how to probe negative values of the Wigner function in scattering of a coherent superposition of two Gaussian packets with a nonvanishing impact parameter between them (a Schrödinger's cat state) by atomic targets. For hydrogen in the ground 1s state, a small parameter of the problem, a ratio a/σ_{⊥} of the Bohr radius a to the beam width σ_{⊥}, is no longer vanishing. We predict an azimuthal asymmetry of the scattered electrons, which is found to be up to 10%, and argue that it can be reliably detected. The production of beams with the not-everywhere-positive Wigner functions and the probing of such quantum effects can open new perspectives for noninvasive electron microscopy, quantum tomography, particle physics, and so forth.

An inexpensive approach for bright-field and dark-field imaging by scanning transmission electron microscopy in scanning electron microscopy.

PubMed

Patel, Binay; Watanabe, Masashi

2014-02-01

Scanning transmission electron microscopy in scanning electron microscopy (STEM-in-SEM) is a convenient technique for soft materials characterization. Various specimen-holder geometries and detector arrangements have been used for bright-field (BF) STEM-in-SEM imaging. In this study, to further the characterization potential of STEM-IN-SEM, a new specimen holder has been developed to facilitate direct detection of BF signals and indirect detection of dark-field (DF) signals without the need for substantial instrument modification. DF imaging is conducted with the use of a gold (Au)-coated copper (Cu) plate attached to the specimen holder which directs highly scattered transmitted electrons to an off-axis yttrium-aluminum-garnet (YAG) detector. A hole in the copper plate allows for BF imaging with a transmission electron (TE) detector. The inclusion of an Au-coated Cu plate enhanced DF signal intensity. Experiments validating the acquisition of true DF signals revealed that atomic number (Z) contrast may be achieved for materials with large lattice spacing. However, materials with small lattice spacing still exhibit diffraction contrast effects in this approach. The calculated theoretical fine probe size is 1.8 nm. At 30 kV, in this indirect approach, DF spatial resolution is limited to 3.2 nm as confirmed experimentally.

Gaps analysis for CD metrology beyond the 22nm node

NASA Astrophysics Data System (ADS)

Bunday, Benjamin; Germer, Thomas A.; Vartanian, Victor; Cordes, Aaron; Cepler, Aron; Settens, Charles

2013-04-01

This paper will examine the future for critical dimension (CD) metrology. First, we will present the extensive list of applications for which CD metrology solutions are needed, showing commonalities and differences among the various applications. We will then report on the expected technical limits of the metrology solutions currently being investigated by SEMATECH and others in the industry to address the metrology challenges of future nodes, including conventional CD scanning electron microscopy (CD-SEM) and optical critical dimension (OCD) metrology and new potential solutions such as He-ion microscopy (HeIM, sometimes elsewhere referred to as HIM), CD atomic force microscopy (CD-AFM), CD small-angle x-ray scattering (CD-SAXS), high-voltage scanning electron microscopy (HV-SEM), and other types. A technical gap analysis matrix will then be demonstrated, showing the current state of understanding of the future of the CD metrology space.

Evidence for novel age-dependent network structures as a putative primo vascular network in the dura mater of the rat brain

PubMed Central

Lee, Ho-Sung; Kang, Dai-In; Yoon, Seung Zhoo; Ryu, Yeon Hee; Lee, Inhyung; Kim, Hoon-Gi; Lee, Byung-Cheon; Lee, Ki Bog

2015-01-01

With chromium-hematoxylin staining, we found evidence for the existence of novel age-dependent network structures in the dura mater of rat brains. Under stereomicroscopy, we noticed that chromium-hematoxylin-stained threadlike structures, which were barely observable in 1-week-old rats, were networked in specific areas of the brain, for example, the lateral lobes and the cerebella, in 4-week-old rats. In 7-week-old rats, those structures were found to have become larger and better networked. With phase contrast microscopy, we found that in 1-week-old rats, chromium-hematoxylin-stained granules were scattered in the same areas of the brain in which the network structures would later be observed in the 4- and 7-week-old rats. Such age-dependent network structures were examined by using optical and transmission electron microscopy, and the following results were obtained. The scattered granules fused into networks with increasing age. Cross-sections of the age-dependent network structures demonstrated heavily-stained basophilic substructures. Transmission electron microscopy revealed the basophilic substructures to be clusters with high electron densities consisting of nanosized particles. We report these data as evidence for the existence of age-dependent network structures in the dura mater, we discuss their putative functions of age-dependent network structures beyond the general concept of the dura mater as a supporting matrix. PMID:26330833

Spin-orbit scattering visualized in quasiparticle interference

NASA Astrophysics Data System (ADS)

Kohsaka, Y.; Machida, T.; Iwaya, K.; Kanou, M.; Hanaguri, T.; Sasagawa, T.

2017-03-01

In the presence of spin-orbit coupling, electron scattering off impurities depends on both spin and orbital angular momentum of electrons—spin-orbit scattering. Although some transport properties are subject to spin-orbit scattering, experimental techniques directly accessible to this effect are limited. Here we show that a signature of spin-orbit scattering manifests itself in quasiparticle interference (QPI) imaged by spectroscopic-imaging scanning tunneling microscopy. The experimental data of a polar semiconductor BiTeI are well reproduced by numerical simulations with the T -matrix formalism that include not only scalar scattering normally adopted but also spin-orbit scattering stronger than scalar scattering. To accelerate the simulations, we extend the standard efficient method of QPI calculation for momentum-independent scattering to be applicable even for spin-orbit scattering. We further identify a selection rule that makes spin-orbit scattering visible in the QPI pattern. These results demonstrate that spin-orbit scattering can exert predominant influence on QPI patterns and thus suggest that QPI measurement is available to detect spin-orbit scattering.

Structure of biodiesel based bicontinuous microemulsions for environmentally compatible decontamination: A small angle neutron scattering and freeze fracture electron microscopy study.

PubMed

Wellert, S; Karg, M; Imhof, H; Steppin, A; Altmann, H-J; Dolle, M; Richardt, A; Tiersch, B; Koetz, J; Lapp, A; Hellweg, T

2008-09-01

Most toxic industrial chemicals and chemical warfare agents are hydrophobic and can only be solubilized in organic solvents. However, most reagents employed for the degradation of these toxic compounds can only be dissolved in water. Hence, microemulsions are auspicious media for the decontamination of a variety of chemical warfare agents and pesticides. They allow for the solubilization of both the lipophilic toxics and the hydrophilic reagent. Alkyl oligoglucosides and plant derived solvents like rapeseed methyl ester enable the formulation of environmentally compatible bicontinuous microemulsions. In the present article the phase behavior of such a microemulsion is studied and the bicontinuous phase is identified. Small angle neutron scattering (SANS) and freeze fracture electron microscopy (FFEM) measurements are used to characterize the structure of the bicontinuous phase and allow for an estimation of the total internal interface. Moreover, also the influence of the co-surfactant (1-pentanol) on the structural parameters of the bicontinuous phase is studied with SANS.

An analysis of FtsZ assembly using small angle X-ray scattering and electron microscopy.

PubMed

Kuchibhatla, Anuradha; Abdul Rasheed, A S; Narayanan, Janaky; Bellare, Jayesh; Panda, Dulal

2009-04-09

Small angle X-ray scattering (SAXS) was used for the first time to study the self-assembly of the bacterial cell division protein, FtsZ, with three different additives: calcium chloride, monosodium glutamate and DEAE-dextran hydrochloride in solution. The SAXS data were analyzed assuming a model form factor and also by a model-independent analysis using the pair distance distribution function. Transmission electron microscopy (TEM) was used for direct observation of the FtsZ filaments. By sectioning and negative staining with glow discharged grids, very high bundling as well as low bundling polymers were observed under different assembly conditions. FtsZ polymers formed different structures in the presence of different additives and these additives were found to increase the bundling of FtsZ protofilaments by different mechanisms. The combined use of SAXS and TEM provided us a significant insight of the assembly of FtsZ and microstructures of the assembled FtsZ polymers.

Whole-cell imaging of the budding yeast Saccharomyces cerevisiae by high-voltage scanning transmission electron tomography.

PubMed

Murata, Kazuyoshi; Esaki, Masatoshi; Ogura, Teru; Arai, Shigeo; Yamamoto, Yuta; Tanaka, Nobuo

2014-11-01

Electron tomography using a high-voltage electron microscope (HVEM) provides three-dimensional information about cellular components in sections thicker than 1 μm, although in bright-field mode image degradation caused by multiple inelastic scattering of transmitted electrons limit the attainable resolution. Scanning transmission electron microscopy (STEM) is believed to give enhanced contrast and resolution compared to conventional transmission electron microscopy (CTEM). Samples up to 1 μm in thickness have been analyzed with an intermediate-voltage electron microscope because inelastic scattering is not a critical limitation, and probe broadening can be minimized. Here, we employed STEM at 1 MeV high-voltage to extend the useful specimen thickness for electron tomography, which we demonstrate by a seamless tomographic reconstruction of a whole, budding Saccharomyces cerevisiae yeast cell, which is ~3 μm in thickness. High-voltage STEM tomography, especially in the bright-field mode, demonstrated sufficiently enhanced contrast and intensity, compared to CTEM tomography, to permit segmentation of major organelles in the whole cell. STEM imaging also reduced specimen shrinkage during tilt-series acquisition. The fidelity of structural preservation was limited by cytoplasmic extraction, and the spatial resolution was limited by the relatively large convergence angle of the scanning probe. However, the new technique has potential to solve longstanding problems of image blurring in biological specimens beyond 1 μm in thickness, and may facilitate new research in cellular structural biology. Copyright © 2014 Elsevier B.V. All rights reserved.

SRS in the single molecule limit (Conference Presentation)

NASA Astrophysics Data System (ADS)

Potma, Eric O.; Crampton, Kevin T.; Fast, Alexander; Apkarian, Vartkess A.

2017-02-01

We present combined surface-enhanced stimulated Raman scattering (SE-SRS) and surface-enhanced coherent anti-Stokes Raman scattering (SE-CARS) measurements on individual plasmonic antennas dressed with bipyridyl-ethylene molecules. By carefully optimizing the conditions for performing SE-SRS experiments, we have obtained stable and reproducible molecular surface-enhanced SRS spectra from single nano-antennas. Using surface-enhanced Raman scattering (SERS) and transmission electron microscopy of the same antennas, we confirm that the observed SE-SRS signals originate from only one or a few molecules. We highlight the physics of surface enhancement in the context of coherent Raman scattering and derive sensitivity parameters under the relevant conditions. The implications of single molecule SRS measurements are discussed.

Relative merits and limiting factors for x-ray and electron microscopy of thick, hydrated organic materials.

PubMed

Du, Ming; Jacobsen, Chris

2018-01-01

Electron and x-ray microscopes allow one to image the entire, unlabeled structure of hydrated materials at a resolution well beyond what visible light microscopes can achieve. However, both approaches involve ionizing radiation, so that radiation damage must be considered as one of the limits to imaging. Drawing upon earlier work, we describe here a unified approach to estimating the image contrast (and thus the required exposure and corresponding radiation dose) in both x-ray and electron microscopy. This approach accounts for factors such as plural and inelastic scattering, and (in electron microscopy) the use of energy filters to obtain so-called "zero loss" images. As expected, it shows that electron microscopy offers lower dose for specimens thinner than about 1 µm (such as for studies of macromolecules, viruses, bacteria and archaebacteria, and thin sectioned material), while x-ray microscopy offers superior characteristics for imaging thicker specimen such as whole eukaryotic cells, thick-sectioned tissues, and organs. The required radiation dose scales strongly as a function of the desired spatial resolution, allowing one to understand the limits of live and frozen hydrated specimen imaging. Finally, we consider the factors limiting x-ray microscopy of thicker materials, suggesting that specimens as thick as a whole mouse brain can be imaged with x-ray microscopes without significant image degradation should appropriate image reconstruction methods be identified. Copyright © 2017 Elsevier B.V. All rights reserved.

Quasiparticle Scattering in Type-II Weyl semimetal MoTe₂.

PubMed

Lin, Chun-Liang; Arafune, Ryuichi; Minamitani, Emi; Kawai, Maki; Takagi, Noriaki

2018-01-30

The electronic structure of type-II Weyl semimetal molybdenum ditelluride (MoTe₂) is studied by using scanning tunneling microscopy and density functional theory calculations. Through measuring energy-dependent quasiparticle interference (QPI) patterns with a cryogenic scanning tunneling microscope, several characteristic features are found in the QPI patterns. Two of them arise from the Weyl semimetal nature; one is the topological Fermi arc surface state and the other can be assigned to be a Weyl point. The remaining structures are derived from the scatterings relevant to the bulk electronic states. The findings lead to thorough understanding of the topological electronic structure of type-II Weyl semimetal MoTe₂. © 2018 IOP Publishing Ltd.

Fine structure characterization of martensite/austenite constituent in low-carbon low-alloy steel by transmission electron forward scatter diffraction.

PubMed

Li, C W; Han, L Z; Luo, X M; Liu, Q D; Gu, J F

2016-11-01

Transmission electron forward scatter diffraction and other characterization techniques were used to investigate the fine structure and the variant relationship of the martensite/austenite (M/A) constituent of the granular bainite in low-carbon low-alloy steel. The results demonstrated that the M/A constituents were distributed in clusters throughout the bainitic ferrite. Lath martensite was the main component of the M/A constituent, where the relationship between the martensite variants was consistent with the Nishiyama-Wassermann orientation relationship and only three variants were found in the M/A constituent, suggesting that the variants had formed in the M/A constituent according to a specific mechanism. Furthermore, the Σ3 boundaries in the M/A constituent were much longer than their counterparts in the bainitic ferrite region. The results indicate that transmission electron forward scatter diffraction is an effective method of crystallographic analysis for nanolaths in M/A constituents. © 2016 The Authors Journal of Microscopy © 2016 Royal Microscopical Society.

Structures of Astromaterials Revealed by EBSD

NASA Technical Reports Server (NTRS)

Zolensky, M.

2018-01-01

Groups at the Johnson Space Center and the University of Tokyo have been using electron back-scattered diffraction (EBSD) to reveal the crystal structures of extraterrestrial minerals for many years. Even though we also routinely use transmission electron microscopy, synchrotron X-ray diffraction (SXRD), and conventional electron diffraction, we find that EBSD is the most powerful technique for crystal structure elucidation in many instances. In this talk I describe a few of the cases where we have found EBSD to provide crucial, unique information. See attachment.

Dynamic light scattering study on vesicles of Netaine-Cholesterol system

NASA Astrophysics Data System (ADS)

Alenaizi, R.; Radiman, S.; Mohamed, F.; Rahman, I. Abdul

2014-09-01

The morphology of vesicles system with defined particle size and shape is one of interest in our technical applications. Here we have used dynamic light scattering technique and transmission electron microscopy for structural characterization of N-dimethylglycine Betaine with 5-cholesten-3β-ol vesicles in aqueous solutions. An isotropic one phase region is found in the very diluted regions depending on Betaine/Cholesterol ratio. The isotropic region was stable for more than 3 months at room temperature, with monodispersed unilamellar vesicles ˜ 300nm.

Probing mesoscopic crystals with electrons: One-step simultaneous inelastic and elastic scattering theory

NASA Astrophysics Data System (ADS)

Nazarov, Vladimir U.; Silkin, Vyacheslav M.; Krasovskii, Eugene E.

2017-12-01

Inelastic scattering of the medium-energy (˜10 -100 eV) electrons underlies the method of the high-resolution electron energy-loss spectroscopy (HREELS), which has been successfully used for decades to characterize pure and adsorbate-covered surfaces of solids. With the emergence of graphene and other quasi-two-dimensional (Q2D) crystals, HREELS could be expected to become the major experimental tool to study this class of materials. We, however, identify a critical flaw in the theoretical picture of the HREELS of Q2D crystals in the context of the inelastic scattering only ("energy-loss functions" formalism), in contrast to its justifiable use for bulk solids and surfaces. The shortcoming is the neglect of the elastic scattering, which we show is inseparable from the inelastic one, and which, affecting the spectra dramatically, must be taken into account for the meaningful interpretation of the experiment. With this motivation, using the time-dependent density functional theory for excitations, we build a theory of the simultaneous inelastic and elastic electron scattering at Q2D crystals. We apply this theory to HREELS of graphene, revealing an effect of the strongly coupled excitation of the π +σ plasmon and elastic diffraction resonances. Our results open a path to the theoretically interpretable study of the excitation processes in crystalline mesoscopic materials by means of HREELS, with its supreme resolution on the meV energy scale, which is far beyond the capacity of the now overwhelmingly used EELS in transmission electron microscopy.

Three-dimensional imaging of individual point defects using selective detection angles in annular dark field scanning transmission electron microscopy.

PubMed

Johnson, Jared M; Im, Soohyun; Windl, Wolfgang; Hwang, Jinwoo

2017-01-01

We propose a new scanning transmission electron microscopy (STEM) technique that can realize the three-dimensional (3D) characterization of vacancies, lighter and heavier dopants with high precision. Using multislice STEM imaging and diffraction simulations of β-Ga 2 O 3 and SrTiO 3 , we show that selecting a small range of low scattering angles can make the contrast of the defect-containing atomic columns substantially more depth-dependent. The origin of the depth-dependence is the de-channeling of electrons due to the existence of a point defect in the atomic column, which creates extra "ripples" at low scattering angles. The highest contrast of the point defect can be achieved when the de-channeling signal is captured using the 20-40mrad detection angle range. The effect of sample thickness, crystal orientation, local strain, probe convergence angle, and experimental uncertainty to the depth-dependent contrast of the point defect will also be discussed. The proposed technique therefore opens new possibilities for highly precise 3D structural characterization of individual point defects in functional materials. Copyright © 2016 Elsevier B.V. All rights reserved.

Synthesis and characterization of metal-dielectric composites with copper nanoparticles embedded in a glass matrix: A multitechnique approach

NASA Astrophysics Data System (ADS)

Lipinska-Kalita, Kristina E.; Krol, Denise M.; Hemley, Russell J.; Mariotto, Gino; Kalita, Patricia E.; Ohki, Yoshimichi

2005-09-01

The precipitation and growth of copper nanoparticles in an optically transparent aluminosilicate glass matrix was investigated. The size of particles in this heterophase glass-based composite was modified in a controlled manner by isothermal heat treatments. A multitechnique approach, consisting of Raman scattering spectroscopy, high-resolution transmission electron microscopy, x-ray diffraction technique, and optical absorption spectroscopy, has been used to study the nucleation and crystallization processes. Optical absorption spectroscopy revealed the presence of intense absorption bands attributed to oscillations of free electrons, known as the surface-plasmon resonance band of copper particles, and confirmed a gradual increase of the particles' mean size and density with annealing time. The Raman scattering on acoustical phonons from Cu quantum dots in the glass matrix measured for off-resonance conditions demonstrated the presence of intense, inhomogeneously broadened peaks that have been assigned to the confined acoustic eigenmodes of copper nanoparticles. The particle-size dependence of the acoustic peak energies and the relation between the size distribution and bandwidths of these peaks were derived. High-resolution transmission electron microscopy was used to monitor the nucleation of the nanoparticles and to estimate their mean size.

Electron Microscope Studies of Cadmium Mercury Telluride

NASA Astrophysics Data System (ADS)

Lyster, Martin

Available from UMI in association with The British Library. Requires signed TDF. Epitaxial layers of Cd_{x }Hg_{(1-x)}Te grown on various substrates by liquid phase epitaxy and metallo-organic vapour phase epitaxy have been studied using transmission and scanning electron microscopy, in a variety of contrast modes. Wavelength-dispersive X-ray microanalysis has been used to study interfaces in epitaxial specimens, and the results are used to derive diffusion coefficients for a range of values of x in Cd_ {x}Hg_{(1-x)} Te. Extensive use has been made of back-scattered electron contrast in the SEM as a means of compositional mapping, and defect structures are imaged by this technique. The back-scattered electron contrast at interfaces has been studied in detail and is modelled using the Monte Carlo approach. The modelling is combined with calculations and practical measurements of the probe size in the SEM instrument used in the work, to arrive at a quantitative explanation of this contrast. The SEM and scintillator detector used allow a spatial resolution of better than 1000A, but it is shown that improvements in this are possible with present technology. Scanning infra-red microscopy (SIRM) and high -resolution transmission electron microscopy (HREM) have been applied to the study of CdTe. SIRM images reveal information about Te precipitation, including particle size and density. HREM images provide results concerning dislocation structures in CdTe. Selected-area diffraction contrast TEM results are presented which illustrate the microstructure of LPE and MOVPE material; and TEM foil preparation techniques are discussed, including the choice of ion species for milling cross-sectional specimens. In view of the results obtained, suggestions are made for future work in this field.

Competitive Self-Assembly Manifests Supramolecular Darwinism in Soft-Oxometalates

NASA Astrophysics Data System (ADS)

Das, Santu; Kumar, Saurabh; Mallick, Apabrita; Roy, Soumyajit

2015-09-01

Topological transformation manifested in inorganic materials shows manifold possibilities. In our present work, we show a clear topological transformation in a soft-oxometalate (SOM) system which was formed from its polyoxometalate (POM) precursor [PMo12@Mo72Fe30]. This topological transformation was observed due to time dependent competitive self-assembly of two different length scale soft-oxometalate moieties formed from this two-component host-guest reaction. We characterized different morphologies by scanning electron microscopy, electron dispersive scattering spectroscopy, dynamic light scattering, horizontal attenuated total reflection-infrared spectroscopy and Raman spectroscopy. The predominant structure is selected by its size in a sort of supramolecular Darwinian competition in this process and is described here.

Water without windows: Evaluating the performance of open cell transmission electron microscopy under saturated water vapor conditions, and assessing its potential for microscopy of hydrated biological specimens.

PubMed

Cassidy, Cathal; Yamashita, Masao; Cheung, Martin; Kalale, Chola; Adaniya, Hidehito; Kuwahara, Ryusuke; Shintake, Tsumoru

2017-01-01

We have performed open cell transmission electron microscopy experiments through pure water vapor in the saturation pressure regime (>0.6 kPa), in a modern microscope capable of sub-Å resolution. We have systematically studied achievable pressure levels, stability and gas purity, effective thickness of the water vapor column and associated electron scattering processes, and the effect of gas pressure on electron optical resolution and image contrast. For example, for 1.3 kPa pure water vapor and 300kV electrons, we report pressure stability of ± 20 Pa over tens of minutes, effective thickness of 0.57 inelastic mean free paths, lattice resolution of 0.14 nm on a reference Au specimen, and no significant degradation in contrast or stability of a biological specimen (M13 virus, with 6 nm body diameter). We have also done some brief experiments to confirm feasibility of loading specimens into an in situ water vapor ambient without exposure to intermediate desiccating conditions. Finally, we have also checked if water experiments had any discernible impact on the microscope performance, and report pertinent vacuum and electron optical data, for reference purposes.

Direct observation and analysis of york-shell materials using low-voltage high-resolution scanning electron microscopy: Nanometal-particles encapsulated in metal-oxide, carbon, and polymer

NASA Astrophysics Data System (ADS)

Asahina, Shunsuke; Suga, Mitsuo; Takahashi, Hideyuki; Young Jeong, Hu; Galeano, Carolina; Schüth, Ferdi; Terasaki, Osamu

2014-11-01

Nanometal particles show characteristic features in chemical and physical properties depending on their sizes and shapes. For keeping and further enhancing their features, the particles should be protected from coalescence or degradation. One approach is to encapsulate the nanometal particles inside pores with chemically inert or functional materials, such as carbon, polymer, and metal oxides, which contain mesopores to allow permeation of only chemicals not the nanometal particles. Recently developed low-voltage high-resolution scanning electron microscopy was applied to the study of structural, chemical, and electron state of both nanometal particles and encapsulating materials in yolk-shell materials of Au@C, Ru/Pt@C, Au@TiO2, and Pt@Polymer. Progresses in the following categories were shown for the yolk-shell materials: (i) resolution of topographic image contrast by secondary electrons, of atomic-number contrast by back-scattered electrons, and of elemental mapping by X-ray energy dispersive spectroscopy; (ii) sample preparation for observing internal structures; and (iii) X-ray spectroscopy such as soft X-ray emission spectroscopy. Transmission electron microscopy was also used for characterization of Au@C.

Using Asymmetric Flow Field-Flow Fractionation (AF4) to Determine C60 Colloidal Size Distributions

EPA Science Inventory

The formation of aqueous fullerene suspensions by solvent exchange, sonication, or extended mixing in water is widely reported. Commonly used methods for determining the size of these aggregates rely on static and dynamic light scattering, electron microscopy (EM), or atomic forc...

The refractive index in electron microscopy and the errors of its approximations.

PubMed

Lentzen, M

2017-05-01

In numerical calculations for electron diffraction often a simplified form of the electron-optical refractive index, linear in the electric potential, is used. In recent years improved calculation schemes have been proposed, aiming at higher accuracy by including higher-order terms of the electric potential. These schemes start from the relativistically corrected Schrödinger equation, and use a second simplified form, now for the refractive index squared, being linear in the electric potential. The second and higher-order corrections thus determined have, however, a large error, compared to those derived from the relativistically correct refractive index. The impact of the two simplifications on electron diffraction calculations is assessed through numerical comparison of the refractive index at high-angle Coulomb scattering and of cross-sections for a wide range of scattering angles, kinetic energies, and atomic numbers. Copyright © 2016 Elsevier B.V. All rights reserved.

Coherent nonlinear optical imaging: beyond fluorescence microscopy.

PubMed

Min, Wei; Freudiger, Christian W; Lu, Sijia; Xie, X Sunney

2011-01-01

The quest for ultrahigh detection sensitivity with spectroscopic contrasts other than fluorescence has led to various novel approaches to optical microscopy of biological systems. Coherent nonlinear optical imaging, especially the recently developed nonlinear dissipation microscopy (including stimulated Raman scattering and two-photon absorption) and pump-probe microscopy (including excited-state absorption, stimulated emission, and ground-state depletion), provides new image contrasts for nonfluorescent species. Thanks to the high-frequency modulation transfer scheme, these imaging techniques exhibit superb detection sensitivity. By directly interrogating vibrational and/or electronic energy levels of molecules, they offer high molecular specificity. Here we review the underlying principles and excitation and detection schemes, as well as exemplary biomedical applications of this emerging class of molecular imaging techniques.

Assembly of Ring-Shaped Phosphorus within Carbon Nanotube Nanoreactors.

PubMed

Zhang, Jinying; Zhao, Dan; Xiao, Dingbin; Ma, Chuansheng; Du, Hongchu; Li, Xin; Zhang, Lihui; Huang, Jialiang; Huang, Hongyang; Jia, Chun-Lin; Tománek, David; Niu, Chunming

2017-02-06

A phosphorus allotrope that has not been observed so far, ring-shaped phosphorus consisting of alternate P 8 and P 2 structural units, has been assembled inside multi-walled carbon nanotube nanoreactors with inner diameters of 5-8 nm by a chemical vapor transport and reaction of red phosphorus at 500 °C. The ring-shaped nanostructures with surrounding graphene walls are stable under ambient conditions. The nanostructures were characterized by high-resolution transmission electron microscopy, scanning transmission electron microscopy, energy-dispersive X-ray spectroscopy, Raman scattering, attenuated total reflectance Fourier transform infrared spectroscopy, and X-ray photoelectron spectroscopy. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

Li, Shuning; Roy, Amitava; Lichtenberg, Henning

The micro-segmented flow technique was applied for continuous synthesis of ZnO micro- and nanoparticles with short residence times of 9.4 s and 21.4 s, respectively. The obtained particles were characterized by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Small angle X-ray scattering (SAXS) and photoluminescence spectroscopy were used to determine the size and optical properties of ZnO nanoparticles. In addition, extended X-ray absorption fine structure (EXAFS) spectroscopy was employed to investigate local structural properties. The EXAFS measurements reveal a larger degree of structural disorder in the nanoparticles than the microparticles. These structural changes should be taken into considerationmore » while evaluating the size-dependent visible emission of ZnO nanoparticles.« less

Characterization of contaminant removal by an optical strip material

NASA Astrophysics Data System (ADS)

Hamilton, James P.; Frigo, S. P.; Caroll, Brenden J.; Assoufidyen, L.; Lewis, Matthew S.; Cook, Russell E.; de Carlo, F.

2001-03-01

Department of Chemistry and Engineering Physics, University of Wisconsin-Platteville, Platteville, WI 53818 Advanced Photon Source, X-Ray Facilities Division, Argonne National Laboratory, Advanced Photon Source, User Program Division, Argonne National Laboratory, *Electron Microscopy Center, Materials Science Division, Argonne National Laboratory, Argonne National Laboratory, 9700 S. Cass Ave., Argonne IL 60439-4856 USA A novel optical strip coating material, Opticlean, has been shown to safely remove fingerprints, particles and contamination from a variety of optical surfaces including coated glass, Si and first surface mirrors. Contaminant removal was monitored by Nomarski, Atomic Force and Scanning Electron Microscopy. Sub-micron features on diffraction gratings and silicon wafers were also cleaned without leaving light scattering particles on the surface. **This work was supported in part by the U.S. Department of Energy, Basic Energy Sciences-Materials Sciences, under contract no. W-31-109-ENG-38. The authors acknowledge the support and facilities provided by the Advanced Photon Source and the Electron Microscopy Center at Argonne National Laboratory.

Cryogenic coherent X-ray diffraction imaging of biological samples at SACLA: a correlative approach with cryo-electron and light microscopy.

PubMed

Takayama, Yuki; Yonekura, Koji

2016-03-01

Coherent X-ray diffraction imaging at cryogenic temperature (cryo-CXDI) allows the analysis of internal structures of unstained, non-crystalline, whole biological samples in micrometre to sub-micrometre dimensions. Targets include cells and cell organelles. This approach involves preparing frozen-hydrated samples under controlled humidity, transferring the samples to a cryo-stage inside a vacuum chamber of a diffractometer, and then exposing the samples to coherent X-rays. Since 2012, cryo-coherent diffraction imaging (CDI) experiments have been carried out with the X-ray free-electron laser (XFEL) at the SPring-8 Ångstrom Compact free-electron LAser (SACLA) facility in Japan. Complementary use of cryo-electron microscopy and/or light microscopy is highly beneficial for both pre-checking samples and studying the integrity or nature of the sample. This article reports the authors' experience in cryo-XFEL-CDI of biological cells and organelles at SACLA, and describes an attempt towards reliable and higher-resolution reconstructions, including signal enhancement with strong scatterers and Patterson-search phasing.

Chemo-spectroscopic sensor for carboxyl terminus overexpressed in carcinoma cell membrane.

PubMed

Stanca, Sarmiza E; Matthäus, Christian; Neugebauer, Ute; Nietzsche, Sandor; Fritzsche, Wolfgang; Dellith, Jan; Heintzmann, Rainer; Weber, Karina; Deckert, Volker; Krafft, Christoph; Popp, Jürgen

2015-10-01

Certain carboxyl groups of the plasma membrane are involved in tumorgenesis processes. A gold core-hydroxyapatite shell (AuHA) nanocomposite is introduced as chemo-spectroscopic sensor to monitor these carboxyl groups of the cell membrane. Hydroxyapatite (HA) plays the role both of a chemical detector and of a biocompatible Raman marker. The principle of detection is based on chemical interaction between the hydroxyl groups of the HA and the carboxyl terminus of the proteins. The AuHA exhibits a surface enhanced Raman scattering (SERS) signal at 954 cm(-1) which can be used for its localization. The bio-sensing capacity of AuHA towards human skin epidermoid carcinoma (A431) and Chinese hamster ovary (CHO) cell lines is investigated using Raman microspectroscopic imaging. The localization of AuHA on cells is correlated with scanning electron microscopy, transmission electron microscopy and structured illumination fluorescence microscopy. This qualitative approach is a step towards a quantitative study of the proteins terminus. This method would enable further studies on the molecular profiling of the plasma membrane, in an attempt to provide accurate cell identification. Using a gold core-hydroxyapatite shell (AuHA) nanocomposite, the authors in this paper showed the feasibility of detecting and differentiating cell surface molecules by surface enhanced Raman scattering. Copyright © 2015 Elsevier Inc. All rights reserved.

Functionalization of a nanostructured hydroxyapatite with Cu(II) compounds as a pesticide: in situ transmission electron microscopy and environmental scanning electron microscopy observations of treated Vitis vinifera L. leaves.

PubMed

Battiston, Enrico; Salvatici, Maria C; Lavacchi, Alessandro; Gatti, Antonietta; Di Marco, Stefano; Mugnai, Laura

2018-02-19

The present study evaluated a biocompatible material for plant protection with the aim of reducing the amount of active substance applied. We used a synthetic hydroxyapatite (HA) that has been studied extensively as a consequence of its bioactivity and biocompatibility. An aggregation between HA nanoparticles and four Cu(II) compounds applied to Vitis vinifera L. leaves as a pesticide was studied. Formulations were characterized by X-ray diffraction (XRD), dynamic light scattering (DLS) and electron microscopy and applied in planta to verify particle aggregation and efficiency in controlling the pathogen Plasmopara viticola. The XRD patterns showed different crystalline phases dependig on the Cu(II) compound formulated with HA particles, DLS showed that nanostructured particles are stable as aggregates out of the nanometer range and, in all formulations, transmission electron microscopy (TEM) and environmental scanning electron microscopy (ESEM) microscopy showed large aggregates which were partially nanostructured and were recognized as stable in their micrometric dimensions. Such particles did not show phytotoxic effects after their application in planta. A formulation based on HA and a soluble Cu(II) compound showed promising results in the control of the fungal pathogen, confirming the potential role of HA as an innovative delivery system of Cu(II) ions. The present work indicates the possibility of improving the biological activity of a bioactive substance by modifying its structure through an achievable formulation with a biocompatible material. © 2018 Society of Chemical Industry. © 2018 Society of Chemical Industry.

Wide-field optical detection of nanoparticles using on-chip microscopy and self-assembled nanolenses

NASA Astrophysics Data System (ADS)

Mudanyali, Onur; McLeod, Euan; Luo, Wei; Greenbaum, Alon; Coskun, Ahmet F.; Hennequin, Yves; Allier, Cédric P.; Ozcan, Aydogan

2013-03-01

The direct observation of nanoscale objects is a challenging task for optical microscopy because the scattering from an individual nanoparticle is typically weak at optical wavelengths. Electron microscopy therefore remains one of the gold standard visualization methods for nanoparticles, despite its high cost, limited throughput and restricted field-of-view. Here, we describe a high-throughput, on-chip detection scheme that uses biocompatible wetting films to self-assemble aspheric liquid nanolenses around individual nanoparticles to enhance the contrast between the scattered and background light. We model the effect of the nanolens as a spatial phase mask centred on the particle and show that the holographic diffraction pattern of this effective phase mask allows detection of sub-100 nm particles across a large field-of-view of >20 mm2. As a proof-of-concept demonstration, we report on-chip detection of individual polystyrene nanoparticles, adenoviruses and influenza A (H1N1) viral particles.

Label-free volumetric optical imaging of intact murine brains

NASA Astrophysics Data System (ADS)

Ren, Jian; Choi, Heejin; Chung, Kwanghun; Bouma, Brett E.

2017-04-01

A central effort of today’s neuroscience is to study the brain’s ’wiring diagram’. The nervous system is believed to be a network of neurons interacting with each other through synaptic connection between axons and dendrites, therefore the neuronal connectivity map not only depicts the underlying anatomy, but also has important behavioral implications. Different approaches have been utilized to decipher neuronal circuits, including electron microscopy (EM) and light microscopy (LM). However, these approaches typically demand extensive sectioning and reconstruction for a brain sample. Recently, tissue clearing methods have enabled the investigation of a fully assembled biological system with greatly improved light penetration. Yet, most of these implementations, still require either genetic or exogenous contrast labeling for light microscopy. Here we demonstrate a high-speed approach, termed as Clearing Assisted Scattering Tomography (CAST), where intact brains can be imaged at optical resolution without labeling by leveraging tissue clearing and the scattering contrast of optical frequency domain imaging (OFDI).

Wide-field optical detection of nanoparticles using on-chip microscopy and self-assembled nanolenses

PubMed Central

Mudanyali, Onur; McLeod, Euan; Luo, Wei; Greenbaum, Alon; Coskun, Ahmet F.; Hennequin, Yves; Allier, Cédric P.; Ozcan, Aydogan

2013-01-01

The direct observation of nanoscale objects is a challenging task for optical microscopy because the scattering from an individual nanoparticle is typically weak at optical wavelengths. Electron microscopy therefore remains one of the gold standard visualization methods for nanoparticles, despite its high cost, limited throughput and restricted field-of-view. Here, we describe a high-throughput, on-chip detection scheme that uses biocompatible wetting films to self-assemble aspheric liquid nanolenses around individual nanoparticles to enhance the contrast between the scattered and background light. We model the effect of the nanolens as a spatial phase mask centred on the particle and show that the holographic diffraction pattern of this effective phase mask allows detection of sub-100 nm particles across a large field-of-view of >20 mm2. As a proof-of-concept demonstration, we report on-chip detection of individual polystyrene nanoparticles, adenoviruses and influenza A (H1N1) viral particles. PMID:24358054

Electron-beam broadening in amorphous carbon films in low-energy scanning transmission electron microscopy.

PubMed

Drees, H; Müller, E; Dries, M; Gerthsen, D

2018-02-01

Resolution in scanning transmission electron microscopy (STEM) is ultimately limited by the diameter of the electron beam. The electron beam diameter is not only determined by the properties of the condenser lens system but also by electron scattering in the specimen which leads to electron-beam broadening and degradation of the resolution with increasing specimen thickness. In this work we introduce a new method to measure electron-beam broadening which is based on STEM imaging with a multi-segmented STEM detector. We focus on STEM at low electron energies between 10 and 30 keV and use an amorphous carbon film with known thickness as test object. The experimental results are compared with calculated beam diameters using different analytical models and Monte-Carlo simulations. We find excellent agreement of the experimental data with the recently published model by Gauvin and Rudinsky [1] for small t/λ el (thickness to elastic mean free path) values which are considered in our study. Copyright © 2017 Elsevier B.V. All rights reserved.

Quasiparticle interference in ZrSiS: Strongly band-selective scattering depending on impurity lattice site

NASA Astrophysics Data System (ADS)

Butler, Christopher J.; Wu, Yu-Mi; Hsing, Cheng-Rong; Tseng, Yi; Sankar, Raman; Wei, Ching-Ming; Chou, Fang-Cheng; Lin, Minn-Tsong

2017-11-01

Scanning tunneling microscopy visualizations of quasiparticle interference (QPI) enable powerful insights into the k -space properties of superconducting, topological, Rashba, and other exotic electronic phases, but their reliance on impurities acting as scattering centers is rarely scrutinized. Here, we investigate QPI at the vacuum-cleaved (001) surface of the Dirac semimetal ZrSiS. We find that interference patterns around impurities located on the Zr and S lattice sites appear very different, and can be ascribed to selective scattering of different subsets of the predominantly Zr 4 d -derived band structure, namely, the m =0 and ±1 components. We show that the selectivity of scattering channels requires an explanation beyond the different bands' orbital characteristics and their respective charge density distributions over Zr and S lattice sites. Importantly, this result shows that the usual assumption of generic scattering centers allowing observations of quasiparticle interference to shed light indiscriminately and isotropically upon the q space of scattering events does not hold, and that the scope and interpretation of QPI observations can therefore be be strongly contingent on the material defect chemistry. This finding promises to spur new investigations into the quasiparticle scattering process itself, to inform future interpretations of quasiparticle interference observations, and ultimately to aid the understanding and engineering of quantum electronic transport properties.

Delaminated graphene at silicon carbide facets: atomic scale imaging and spectroscopy.

PubMed

Nicotra, Giuseppe; Ramasse, Quentin M; Deretzis, Ioannis; La Magna, Antonino; Spinella, Corrado; Giannazzo, Filippo

2013-04-23

Atomic-resolution structural and spectroscopic characterization techniques (scanning transmission electron microscopy and electron energy loss spectroscopy) are combined with nanoscale electrical measurements (conductive atomic force microscopy) to study at the atomic scale the properties of graphene grown epitaxially through the controlled graphitization of a hexagonal SiC(0001) substrate by high temperature annealing. This growth technique is known to result in a pronounced electron-doping (∼10(13) cm(-2)) of graphene, which is thought to originate from an interface carbon buffer layer strongly bound to the substrate. The scanning transmission electron microscopy analysis, carried out at an energy below the knock-on threshold for carbon to ensure no damage is imparted to the film by the electron beam, demonstrates that the buffer layer present on the planar SiC(0001) face delaminates from it on the (112n) facets of SiC surface steps. In addition, electron energy loss spectroscopy reveals that the delaminated layer has a similar electronic configuration to purely sp2-hybridized graphene. These observations are used to explain the local increase of the graphene sheet resistance measured around the surface steps by conductive atomic force microscopy, which we suggest is due to significantly lower substrate-induced doping and a resonant scattering mechanism at the step regions. A first-principles-calibrated theoretical model is proposed to explain the structural instability of the buffer layer on the SiC facets and the resulting delamination.

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

Sornadurai, D.; Ravindran, T. R.; Paul, V. Thomas

Synthesis parameters are optimized in order to grow single crystals of multiferroic BiFeO{sub 3}. 2 to 3 mm size pyramid (tetrahedron) shaped single crystals were successfully obtained by solvothermal method. Scanning electron microscopy with EDAX confirmed the phase formation. Raman scattering spectra of bulk BiFeO3 single crystals have been measured which match well with reported spectra.

Tailored Rh surface facilitates, enhancement of Raman scattering in trimetallic AuPt core/Rh shell composites: Experimental and theoretical evidences

NASA Astrophysics Data System (ADS)

Loganathan, B.; Chandraboss, V. L.; Senthilvelan, S.; Karthikeyan, B.

2016-01-01

We present a detailed analysis of surface-enhanced Raman scattering of 7-azaindole and L-cysteine adsorbed on a tailored Rh surface by using experimental and density functional theoretical (DFT) calculations. DFT with the B3LYP/Lanl2DZ basis set was used for the optimization of the ground state geometries and simulation of the surface-enhanced Raman spectrum of probe molecules adsorbed on Rh6 cluster. 7-azaindole and L-cysteine adsorption at the shell interface was ascertained from first-principles. In addition, characterization of synthesized trimetallic AuPt core/Rh shell colloidal nanocomposites has been analyzed by UV-visible spectroscopy, high-resolution transmission and scanning electron microscopy, selected area electron diffraction pattern analysis, energy-dispersive X-ray spectroscopy, atomic force, confocal Raman microscopy, FT-Raman and surface-enhanced Raman spectroscopic analysis. This analysis serves as the first step in gaining an accurate understanding of specific interactions at the interface of organic and biomolecules and to gain knowledge on the surface composition of trimetallic Au/Pt/Rh colloidal nanocomposites.

Synthesis of polymer-stabilized monometallic Cu and bimetallic Cu/Ag nanoparticles and their surface-enhanced Raman scattering properties

NASA Astrophysics Data System (ADS)

Zhang, Danhui; Liu, Xiaoheng

2013-03-01

The present study demonstrates a facile process for the production of spherical-shaped Cu and Ag nanoparticles synthesized and stabilized by hydrazine and gelatin, respectively. Advantages of the synthetic method include its production of water dispersible copper and copper/silver nanoparticles at room temperature under no inert atmosphere. The resulting nanoparticles (copper or copper/silver) are investigated by X-ray diffraction (XRD), UV-vis spectroscopy, and transmission electron microscopy (TEM). The nanometallic dispersions were characterized by surface plasmon absorbance measuring at 420 and 572 nm for Ag and Cu nanoparticles, respectively. Transmission electron microscopy showed the formation of nanoparticles in the range of ˜10 nm (silver), and ˜30 nm (copper). The results also demonstrate that the reducing order of Cu2+/Ag+ is important for the formation of the bimetallic nanoparticles. The surface-enhanced Raman scattering effects of copper and copper/silver nanoparticles were also displayed. It was found that the enhancement ability of copper/silver nanoparticles was little higher than the copper nanoparticles.

Formation of silver nanoparticle at phospholipid template using Langmuir-Blodgett technique and its Surface-enhanced Raman Spectroscopy application

NASA Astrophysics Data System (ADS)

Mahato, M.; Sarkar, R.; Pal, P.; Talapatra, G. B.

2015-10-01

The biosynthesis of metal nanoparticle and their suitable assembly has recently gained tremendous interest for its application in biomedical arena such as substrates for surface-enhanced Raman scattering and others. In this article, an easy, low-cost, fast, bio-friendly and toxic-reducing agent free protocol has been described for the preparation of silver nanoparticle film using biocompatible 1,2-dipalmitoyl-sn-glycero-3-phosphocholine phospholipid Langmuir monolayer template. Interactions, docking and attachment of silver ions to the above-mentioned phospholipid monolayer have been studied by surface pressure-area isotherm and compressibility analysis at the air-water interface. We have deposited the Langmuir-Blodgett monolayer/multilayer containing silver nanoparticle onto glass/SiO2/quartz substrates. The formation of phospholipid-silver nanoparticle complex in Langmuir-Blodgett film has been characterized by field emission-scanning electron microscopy and high-resolution tunneling electron microscopy images. We have applied this deposited film as a substrate for surface-enhanced Raman scattering application using rhodamine 123 to understand the existence of the surface plasmon activity of silver nanoparticle.

Structural Studies of Amorphous Materials by Fluctuation Electron Microscopy

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

Treacy, Michael M. J.

Fluctuation Electron Microscopy (FEM) is a technique that examines the fluctuations in electron scattering across a uniformly thin amorphous sample. The statistics of the intensity fluctuations, mean and variance, reveal any underlying medium-range order present in the structure. The goals of this project were: (1) To determine the fundamentals of the scattering physics that gives rise to the variance signal in fluctuation electron microscopy (FEM); (2) To use these discoveries to find ways to quantify FEM; (3) To apply the FEM method to interesting and technologically important families of amorphous materials, particularly those with important applications in energy-related processes. Excellent progress was made in items (1) and (2). In stage (3) we did not examine the metamict zircons, as proposed. Instead, we examined films of polycrystalline and amorphous semi-conducting diamond. Significant accomplishments are: (1) A Reverse Monte Carlo procedure was successfully implemented to invert FEM data into a structural model. This is computer-intensive, but it demonstrated that diffraction and FEM data from amorphous silicon are most consistent with a paracrystallite model. This means that there is more diamond-like topology present in amorphous silicon than is predicted by the continuous random network model. (2) There is significant displacement decoherence arising in diffraction from amorphous silicon and carbon. The samples are being bombarded by the electron beam and atoms do not stay still while being irradiated – much more than was formerly understood. The atom motions cause the destructive and constructive interferences in the diffraction pattern to fluctuate with time, and it is the time-averaged speckle that is being measured. The variance is reduced by a factor m, 4 ≤ m ≤ 1000, relative to that predicted by kinematical scattering theory. (3) Speckle intensity obeys a gamma distribution, where the mean intensitymore » $$ \\overline{I}\\ $$ and m are the two parameters governing the shape of the gamma distribution profile. m is determined by the illumination spatial coherence, which is normally very high, and mostly by the displacement decoherence within the sample. (4) Amorphous materials are more affected by the electron beam than are crystalline materials. Different samples exhibit different disruptibility, as measured by the effective values of m that fit the data. (5) Understanding the origin of the displacement decoherence better should lead to efficient methods for computing the observed variance from amorphous materials.« less

Electron scattering in graphene with adsorbed NaCl nanoparticles

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

Drabińska, Aneta, E-mail: Aneta.Drabinska@fuw.edu.pl; Kaźmierczak, Piotr; Bożek, Rafał

2015-01-07

In this work, the results of contactless magnetoconductance and Raman spectroscopy measurements performed for a graphene sample after its immersion in NaCl solution were presented. The properties of the immersed sample were compared with those of a non-immersed reference sample. Atomic force microscopy and electron spin resonance experiments confirmed the deposition of NaCl nanoparticles on the graphene surface. A weak localization signal observed using contactless magnetoconductance showed the reduction of the coherence length after NaCl treatment of graphene. Temperature dependence of the coherence length indicated a change from ballistic to diffusive regime in electron transport after NaCl treatment. The mainmore » inelastic scattering process was of the electron-electron type but the major reason for the reduction of the coherence length at low temperatures was additional, temperature independent, inelastic scattering. We associate it with spin flip scattering, caused by NaCl nanoparticles present on the graphene surface. Raman spectroscopy showed an increase in the D and D′ bands intensities for graphene after its immersion in NaCl solution. An analysis of the D, D′, and G bands intensities proved that this additional scattering is related to the decoration of vacancies and grain boundaries with NaCl nanoparticles, as well as generation of new on-site defects as a result of the decoration of the graphene surface with NaCl nanoparticles. The observed energy shifts of 2D and G bands indicated that NaCl deposition on the graphene surface did not change carrier concentration, but reduced compressive biaxial strain in the graphene layer.« less

Active pixel sensor array as a detector for electron microscopy.

PubMed

Milazzo, Anna-Clare; Leblanc, Philippe; Duttweiler, Fred; Jin, Liang; Bouwer, James C; Peltier, Steve; Ellisman, Mark; Bieser, Fred; Matis, Howard S; Wieman, Howard; Denes, Peter; Kleinfelder, Stuart; Xuong, Nguyen-Huu

2005-09-01

A new high-resolution recording device for transmission electron microscopy (TEM) is urgently needed. Neither film nor CCD cameras are systems that allow for efficient 3-D high-resolution particle reconstruction. We tested an active pixel sensor (APS) array as a replacement device at 200, 300, and 400 keV using a JEOL JEM-2000 FX II and a JEM-4000 EX electron microscope. For this experiment, we used an APS prototype with an area of 64 x 64 pixels of 20 microm x 20 microm pixel pitch. Single-electron events were measured by using very low beam intensity. The histogram of the incident electron energy deposited in the sensor shows a Landau distribution at low energies, as well as unexpected events at higher absorbed energies. After careful study, we concluded that backscattering in the silicon substrate and re-entering the sensitive epitaxial layer a second time with much lower speed caused the unexpected events. Exhaustive simulation experiments confirmed the existence of these back-scattered electrons. For the APS to be usable, the back-scattered electron events must be eliminated, perhaps by thinning the substrate to less than 30 microm. By using experimental data taken with an APS chip with a standard silicon substrate (300 microm) and adjusting the results to take into account the effect of a thinned silicon substrate (30 microm), we found an estimate of the signal-to-noise ratio for a back-thinned detector in the energy range of 200-400 keV was about 10:1 and an estimate for the spatial resolution was about 10 microm.

Limiting factors in atomic resolution cryo electron microscopy: No simple tricks

PubMed Central

Zhang, Xing; Zhou, Z. Hong

2013-01-01

To bring cryo electron microscopy (cryoEM) of large biological complexes to atomic resolution, several factors – in both cryoEM image acquisition and 3D reconstruction – that may be neglected at low resolution become significantly limiting. Here we present thorough analyses of four limiting factors: (a) electron-beam tilt, (b) inaccurate determination of defocus values, (c) focus gradient through particles, and (d) particularly for large particles, dynamic (multiple) scattering of electrons. We also propose strategies to cope with these factors: (a) the divergence and direction tilt components of electron-beam tilt could be reduced by maintaining parallel illumination and by using a coma-free alignment procedure, respectively. Moreover, the effect of all beam tilt components, including spiral tilt, could be eliminated by use of a spherical aberration corrector. (b) More accurate measurement of defocus value could be obtained by imaging areas adjacent to the target area at high electron dose and by measuring the image shift induced by tilting the electron beam. (c) Each known Fourier coefficient in the Fourier transform of a cryoEM image is the sum of two Fourier coefficients of the 3D structure, one on each of two curved ‘characteristic surfaces’ in 3D Fourier space. We describe a simple model-based iterative method that could recover these two Fourier coefficients on the two characteristic surfaces. (d) The effect of dynamic scattering could be corrected by deconvolution of a transfer function. These analyses and our proposed strategies offer useful guidance for future experimental designs targeting atomic resolution cryoEM reconstruction. PMID:21627992

Nonformity of the electron density in amorphous silicon films

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

Ionova, E.N.; Cheremskoi, P.G.; Fedorenko, A.I.

1985-12-01

The authors study the nonuniformity of a-Si:H films obtained by the method of vacuum condensation, with the help of x-ray small-angle scattering (SLS) and transmission electron microscopy. Films of hydrogenated amorphous silicon are greatest interest, because the electronic properties of this material can be controlled by doping. As a result of the compensation of the ruptured bonds, and possibly, effects of melting, the properties of such films are analogous to those of singlecrystalline silicon. XLS enables a quantitative determination of the prameters of the regions of low electron density (RLD) in such objects.

Energy dispersive X-ray analysis on an absolute scale in scanning transmission electron microscopy.

PubMed

Chen, Z; D'Alfonso, A J; Weyland, M; Taplin, D J; Allen, L J; Findlay, S D

2015-10-01

We demonstrate absolute scale agreement between the number of X-ray counts in energy dispersive X-ray spectroscopy using an atomic-scale coherent electron probe and first-principles simulations. Scan-averaged spectra were collected across a range of thicknesses with precisely determined and controlled microscope parameters. Ionization cross-sections were calculated using the quantum excitation of phonons model, incorporating dynamical (multiple) electron scattering, which is seen to be important even for very thin specimens. Copyright © 2015 Elsevier B.V. All rights reserved.

Phase-contrast scanning transmission electron microscopy.

PubMed

Minoda, Hiroki; Tamai, Takayuki; Iijima, Hirofumi; Hosokawa, Fumio; Kondo, Yukihito

2015-06-01

This report introduces the first results obtained using phase-contrast scanning transmission electron microscopy (P-STEM). A carbon-film phase plate (PP) with a small center hole is placed in the condenser aperture plane so that a phase shift is introduced in the incident electron waves except those passing through the center hole. A cosine-type phase-contrast transfer function emerges when the phase-shifted scattered waves interfere with the non-phase-shifted unscattered waves, which passed through the center hole before incidence onto the specimen. The phase contrast resulting in P-STEM is optically identical to that in phase-contrast transmission electron microscopy that is used to provide high contrast for weak phase objects. Therefore, the use of PPs can enhance the phase contrast of the STEM images of specimens in principle. The phase shift resulting from the PP, whose thickness corresponds to a phase shift of π, has been confirmed using interference fringes displayed in the Ronchigram of a silicon single crystal specimen. The interference fringes were found to abruptly shift at the edge of the PP hole by π. © The Author 2015. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

In-situ small-angle x-ray scattering study of nanoparticles in the plasma plume induced by pulsed laser irradiation of metallic targets

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

Lavisse, L.; Jouvard, J.-M.; Girault, M.

2012-04-16

Small angle x-ray scattering was used to probe in-situ the formation of nanoparticles in the plasma plume generated by pulsed laser irradiation of a titanium metal surface under atmospheric conditions. The size and morphology of the nanoparticles were characterized as function of laser irradiance. Two families of nanoparticles were identified with sizes on the order of 10 and 70 nm, respectively. These results were confirmed by ex-situ transmission electron microscopy experiments.

Synthesis and Raman scattering of GaN nanorings, nanoribbons and nanowires

NASA Astrophysics Data System (ADS)

Li, Z. J.; Chen, X. L.; Li, H. J.; Tu, Q. Y.; Yang, Z.; Xu, Y. P.; Hu, B. Q.

Low-dimensional GaN materials, including nanorings, nanoribbons and smooth nanowires have been synthesized by reacting gallium and ammonia using Ag particles as a catalyst on the substrate of MgO single crystals. They were characterized by field emission scanning electron microscopy (FE-SEM), energy dispersive X-ray spectroscopy (EDX) and X-ray diffraction (XRD). EDX, XRD indicated that the low-dimensional nanomaterials were wurtzite GaN. New features are found in Raman scatterings for these low-dimensional GaN materials, which are different from the previous observations of GaN materials.

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%).

Unusual inhomogeneous microstructures in charge glass state of PbCrO3

NASA Astrophysics Data System (ADS)

Kurushima, Kosuke; Tsukasaki, Hirofumi; Ogata, Takahiro; Sakai, Yuki; Azuma, Masaki; Ishii, Yui; Mori, Shigeo

2018-05-01

We investigated the microstructures and local structures of perovskite PbCrO3, which shows a metal-to-insulator transition and a 9.8% volume collapse, by electron diffraction, high-resolution transmission electron microscopy (TEM), and high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM). It is revealed that the charge glass state is characterized by the unique coexistence of the crystalline state with a cubic symmetry on average and the noncrystalline state. HAADF-STEM observation at atomic resolution revealed that Pb ions were displaced from the ideal A site position of the cubic perovskite structure, which gives rise to characteristic diffuse scatterings around the fundamental Bragg reflections. These structural inhomogeneities are crucial to the understanding of the unique physical properties in the charge glass state of PbCrO3.

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.

Biophysical interpretation and ex-vivo characterization of scattered light from tumor-associated breast stroma

NASA Astrophysics Data System (ADS)

Laughney, Ashley; Krishnaswamy, Venkat; Schwab, Mary; Wells, Wendy A.; Paulsen, Keith D.; Pogue, Brian W.

2009-02-01

The purpose of this study was to extract scatter parameters related to tissue ultra-structures from freshly excised breast tissue and to assess whether evident changes in scatter across diagnostic categories is primarily influenced by variation in the composition of each tissues subtypes or by physical remodeling of the extra-cellular environment. Pathologists easily distinguish between epithelium, stroma and adipose tissues, so this classification was adopted for macroscopic subtype classification. Micro-sampling reflectance spectroscopy was used to characterize single-backscattered photons from fresh, excised tumors and normal reduction specimens with sub-millimeter resolution. Phase contrast microscopy (sub-micron resolution) was used to characterize forward-scattered light through frozen tissue from the DHMC Tissue Bank, representing normal, benign and malignant breast tissue, sectioned at 10 microns. The packing density and orientation of collagen fibers in the extracellular matrix (ECM) associated with invasive, normal and benign epithelium was evaluated using transmission electron microscopy (TEM). Regions of interest (ROIs) in the H&E stained tissues were identified for analysis, as outlined by a pathologist as the gold standard. We conclude that the scatter parameters associated with tumor specimens (Npatients=6, Nspecimens=13) significantly differs from that of normal reductions (Npatients=6, Nspecimens=10). Further, tissue subtypes may be identified by their scatter spectra at sub-micron resolution. Stromal tissue scatters significantly more than the epithelial cells embedded in its ECM and adipose tissue scatters much less. However, the scatter signature of the stroma at the sub-micron level is not particularly differentiating in terms of a diagnosis.

Symposium U: Thermoelectric Power Generation. Held in Boston, Massachusetts on November 26-29, 2007

DTIC Science & Technology

2008-04-01

including X - ray /electron diffraction, TGA analysis, Raman / Fourier Transform Infrared Spectroscopy, electron microscopy, Rutherford back-scattering and...Energy dispersive X - ray analysis were performed on the treated sample. The results revealed that a surface layer (from 10 nm to up to micron in...nanoparticles into a matrix of bulk Bi2Te 3 material via a hot pressing process. These nanocomposites have been examined by SEM and X - ray powder

You can't measure what you can't see - detectors for microscopies

NASA Astrophysics Data System (ADS)

Denes, Peter

For centuries, the human eye has been the imaging detector of choice thanks to its high sensitivity, wide dynamic range, and direct connection to a built-in data recording and analysis system. The eye, however, is limited to visible light, which excludes microscopies with electrons and X-rays, and the built-in recording system stores archival information at very low rates. The former limitation has been overcome by ``indirect'' detectors, which convert probe particles to visible light, and the latter by a variety of recording techniques, from photographic film to semiconductor-based imagers. Semiconductor imagers have been used for decades as ``direct'' detectors in particle physics, and almost as long for hard X-rays. For soft X-ray microscopy, the challenge has been the small signal levels - plus getting the X-rays into the detector itself, given how quickly they are absorbed in inert layers. For electron microscopy, the challenge has been reconciling detector spatial resolution and pixel count with the large multiple scattering of electrons with energies used for microscopy. Further, a high recording rate (``movies'' rather than ``snapshots'') enables time-resolved studies, time-dependent corrections, shot-by-shot experiments and scanning techniques - at the expense of creating large data volumes. This talk will discuss solutions to these challenges, as well as an outlook towards future developments.

Alignment error envelopes for single particle analysis.

PubMed

Jensen, G J

2001-01-01

To determine the structure of a biological particle to high resolution by electron microscopy, image averaging is required to combine information from different views and to increase the signal-to-noise ratio. Starting from the number of noiseless views necessary to resolve features of a given size, four general factors are considered that increase the number of images actually needed: (1) the physics of electron scattering introduces shot noise, (2) thermal motion and particle inhomogeneity cause the scattered electrons to describe a mixture of structures, (3) the microscope system fails to usefully record all the information carried by the scattered electrons, and (4) image misalignment leads to information loss through incoherent averaging. The compound effect of factors 2-4 is approximated by the product of envelope functions. The problem of incoherent image averaging is developed in detail through derivation of five envelope functions that account for small errors in 11 "alignment" parameters describing particle location, orientation, defocus, magnification, and beam tilt. The analysis provides target error tolerances for single particle analysis to near-atomic (3.5 A) resolution, and this prospect is shown to depend critically on image quality, defocus determination, and microscope alignment. Copyright 2001 Academic Press.

Water without windows: Evaluating the performance of open cell transmission electron microscopy under saturated water vapor conditions, and assessing its potential for microscopy of hydrated biological specimens

PubMed Central

Yamashita, Masao; Cheung, Martin; Kalale, Chola; Adaniya, Hidehito; Kuwahara, Ryusuke; Shintake, Tsumoru

2017-01-01

We have performed open cell transmission electron microscopy experiments through pure water vapor in the saturation pressure regime (>0.6 kPa), in a modern microscope capable of sub-Å resolution. We have systematically studied achievable pressure levels, stability and gas purity, effective thickness of the water vapor column and associated electron scattering processes, and the effect of gas pressure on electron optical resolution and image contrast. For example, for 1.3 kPa pure water vapor and 300kV electrons, we report pressure stability of ± 20 Pa over tens of minutes, effective thickness of 0.57 inelastic mean free paths, lattice resolution of 0.14 nm on a reference Au specimen, and no significant degradation in contrast or stability of a biological specimen (M13 virus, with 6 nm body diameter). We have also done some brief experiments to confirm feasibility of loading specimens into an in situ water vapor ambient without exposure to intermediate desiccating conditions. Finally, we have also checked if water experiments had any discernible impact on the microscope performance, and report pertinent vacuum and electron optical data, for reference purposes. PMID:29099843

Efficiency enhancement in dye sensitized solar cells using dual function mesoporous silica as scatterer and back recombination inhibitor

NASA Astrophysics Data System (ADS)

Tanvi; Mahajan, Aman; Bedi, R. K.; Kumar, Subodh; Saxena, Vibha; Aswal, D. K.

2016-08-01

In the present work, we report the usage of mesoporous silica for improving light harvesting as well as for suppression of back recombination without affecting the extent of dye loading on TiO2 films. Synthesized mesoporous SiO2 was characterized by X-ray photoelectron spectroscopy, X-ray diffraction, Brunauer Emmett and Teller measurement, Scanning electron microscopy and Transmission electron microscopy. DSSCs were fabricated by incorporating different wt% of mesoporous SiO2 in TiO2 paste. An improvement of 50% was observed for devices fabricated using 0.75 wt% of mesoporous SiO2. The mechanism behind the improvement was investigated using electrochemical impedance spectroscopy and UV-Vis spectroscopy.

Preparation of silver nanoparticles loaded graphene oxide nanosheets for antibacterial activity

NASA Astrophysics Data System (ADS)

T, T. T., Vi; Lue, S. J.

2016-11-01

A simple, facile method to fabricate successfully silver nanoparticle (AgNPs) decorated on graphene oxide (GO) layers via grafted thiol groups. Samples were prepared with different concentrations of AgNO3. Resulting AgNPs were quasi-spherical in shape and attached on the layers of GO. Physical properties were confirmed by X-ray diffraction (XRD), zeta potential, dynamic light scattering (DLS), Fourier transform infrared (FTIR) spectra, thermogravimetric analyzer (TGA), transmission electron microscopy (TEM) and field emission scanning electron microscopy (FE-SEM). Antimicrobial test was effectively showed using MRSA (Staphylococcus areus). The GO-Ag NPs with appropriate Ag NPs content of 0.2 M AgNO3 exhibited the strongest antibacterial activity at 48.77% inhibition after 4 hours incubation.

Research on the Ordered Mesoporous Silica for Tobacco Harm Reduction

NASA Astrophysics Data System (ADS)

Wang, Y.; Y Li, Z.; Ding, J. X.; Hu, Z. J.; Liu, Z.; Zhou, G.; Huang, T. H.

2017-12-01

For reducting tobacco harm, this paper prepared an ordered mesoporous silica by using triblock copolymer Pluronic P123 as template. The property of this material was characterized by the X-ray scattering spectrum(XRD), Transmission electron microscopy(TEM), Scanning electron microscopy (SEM) and Nitrogen adsorption/desorption. Then this ordered mesoporous silica was added into the cigarette filter in order to researching its effect of cigarette harm index. The result shows that the feature of SBA-15 was grain morphology, ordered arrangement, tubular porous 2-D hexagonal structure. The application of SBA-15 in cigarette filter can selectively reduce harmful components in cigarette smoke such as crotonaldehyde, hydrogen cyanide, benzo pyrene and tar. The synthesized SBA-15 could properly reduce cigarette harm index.

Scaffolded DNA origami of a DNA tetrahedron molecular container.

PubMed

Ke, Yonggang; Sharma, Jaswinder; Liu, Minghui; Jahn, Kasper; Liu, Yan; Yan, Hao

2009-06-01

We describe a strategy of scaffolded DNA origami to design and construct 3D molecular cages of tetrahedron geometry with inside volume closed by triangular faces. Each edge of the triangular face is approximately 54 nm in dimension. The estimated total external volume and the internal cavity of the triangular pyramid are about 1.8 x 10(-23) and 1.5 x 10(-23) m(3), respectively. Correct formation of the tetrahedron DNA cage was verified by gel electrophoresis, atomic force microscopy, transmission electron microscopy, and dynamic light scattering techniques.

Combining gas-phase electrophoretic mobility molecular analysis (GEMMA), light scattering, field flow fractionation and cryo electron microscopy in a multidimensional approach to characterize liposomal carrier vesicles

PubMed Central

Gondikas, Andreas; von der Kammer, Frank; Hofmann, Thilo; Marchetti-Deschmann, Martina; Allmaier, Günter; Marko-Varga, György; Andersson, Roland

2017-01-01

For drug delivery, characterization of liposomes regarding size, particle number concentrations, occurrence of low-sized liposome artefacts and drug encapsulation are of importance to understand their pharmacodynamic properties. In our study, we aimed to demonstrate the applicability of nano Electrospray Gas-Phase Electrophoretic Mobility Molecular Analyser (nES GEMMA) as a suitable technique for analyzing these parameters. We measured number-based particle concentrations, identified differences in size between nominally identical liposomal samples, and detected the presence of low-diameter material which yielded bimodal particle size distributions. Subsequently, we compared these findings to dynamic light scattering (DLS) data and results from light scattering experiments coupled to Asymmetric Flow-Field Flow Fractionation (AF4), the latter improving the detectability of smaller particles in polydisperse samples due to a size separation step prior detection. However, the bimodal size distribution could not be detected due to method inherent limitations. In contrast, cryo transmission electron microscopy corroborated nES GEMMA results. Hence, gas-phase electrophoresis proved to be a versatile tool for liposome characterization as it could analyze both vesicle size and size distribution. Finally, a correlation of nES GEMMA results with cell viability experiments was carried out to demonstrate the importance of liposome batch-to-batch control as low-sized sample components possibly impact cell viability. PMID:27639623

Electron Microscopy and Analytical X-ray Characterization of Compositional and Nanoscale Structural Changes in Fossil Bone

NASA Astrophysics Data System (ADS)

Boatman, Elizabeth Marie

The nanoscale structure of compact bone contains several features that are direct indicators of bulk tissue mechanical properties. Fossil bone tissues represent unique opportunities to understand the compact bone structure/property relationships from a deep time perspective, offering a possible array of new insights into bone diseases, biomimicry of composite materials, and basic knowledge of bioapatite composition and nanoscale bone structure. To date, most work with fossil bone has employed microscale techniques and has counter-indicated the survival of bioapatite and other nanoscale structural features. The obvious disconnect between the use of microscale techniques and the discernment of nanoscale structure has prompted this work. The goal of this study was to characterize the nanoscale constituents of fossil compact bone by applying a suite of diffraction, microscopy, and spectrometry techniques, representing the highest levels of spatial and energy resolution available today, and capable of complementary structural and compositional characterization from the micro- to the nanoscale. Fossil dinosaur and crocodile long bone specimens, as well as modern ratite and crocodile femurs, were acquired from the UC Museum of Paleontology. Preserved physiological features of significance were documented with scanning electron microscopy back-scattered imaging. Electron microprobe wavelength-dispersive X-ray spectroscopy (WDS) revealed fossil bone compositions enriched in fluorine with a complementary loss of oxygen. X-ray diffraction analyses demonstrated that all specimens were composed of apatite. Transmission electron microscopy (TEM) imaging revealed preserved nanocrystallinity in the fossil bones and electron diffraction studies further identified these nanocrystallites as apatite. Tomographic analyses of nanoscale elements imaged by TEM and small angle X-ray scattering were performed, with the results of each analysis further indicating that nanoscale structure is highly conserved in these four fossil specimens. Finally, the results of this study indicate that bioapatite can be preserved in even the most ancient vertebrate specimens, further supporting the idea that fossilization is a preservational process. This work also underlines the importance of using appropriately selected characterization and analytical techniques for the study of fossil bone, especially from the perspective of spatial resolution and the scale of the bone structural features in question.

Experimental evaluation of environmental scanning electron microscopes at high chamber pressure.

PubMed

Fitzek, H; Schroettner, H; Wagner, J; Hofer, F; Rattenberger, J

2015-11-01

In environmental scanning electron microscopy (ESEM) high pressure applications have become increasingly important. Wet or biological samples can be investigated without time-consuming sample preparation and potential artefacts from this preparation can be neglected. Unfortunately, the signal-to-noise ratio strongly decreases with increasing chamber pressure. To evaluate the high pressure performance of ESEM and to compare different electron microscopes, information about spatial resolution and detector type is not enough. On the one hand, the scattering of the primary electron beam increases, which vanishes the contrast in images; and on the other hand, the secondary electrons (SE) signal amplification decreases. The stagnation gas thickness (effective distance the beam has to travel through the imaging gas) as well as the SE detection system depend on the microscope and for a complete and serious evaluation of an ESEM or low vacuum SEM it is necessary to specify these two parameters. A method is presented to determine the fraction of scattered and unscattered electrons and to calculate the stagnation gas thickness (θ). To evaluate the high pressure performance of the SE detection system, a method is presented that allows for an analysis of a single image and the calculation of the signal-to-noise ratio of this image. All investigations are performed on an FEI ESEM Quanta 600 (field emission gun) and an FEI ESEM Quanta 200 (thermionic gun). These methods and measurements should represent opportunities for evaluating the high pressure performance of an ESEM. © 2015 The Authors Journal of Microscopy © 2015 Royal Microscopical Society.

Scanned gate microscopy of inter-edge channel scattering in the quantum Hall regime

NASA Astrophysics Data System (ADS)

Woodside, Michael T.; Vale, Chris; McEuen, Paul L.; Kadow, C.; Maranowski, K. D.; Gossard, A. C.

2000-03-01

Novel scanned probe techniques have recently been used to study in detail the microscopic properties of 2D electron gases in the quantum Hall regime [1]. We report local measurements of the scattering between edge states in a quantum Hall conductor with non-equilibrium edge state populations. Using an atomic force microscope (AFM) tip as a local gate to perturb the edge states, we find that the scattering is dominated by individual, microscopic scattering sites, which we directly image and characterise. The dependence of the scattering on the AFM tip voltage reveals that it involves tunneling both through quasi-bound impurity states and through disorder-induced weak links between the edge states. [1] S. H. Tessmer et al., Nature 392, 51 (1998); K. L. McCormick et al., Phys. Rev. B 59, 4654 (1999); A. Yacoby et al., Solid State Comm. 111, 1 (1999).

Possible superconductivity in Sr₂IrO₄ probed by quasiparticle interference.

PubMed

Gao, Yi; Zhou, Tao; Huang, Huaixiang; Wang, Qiang-Hua

2015-03-18

Based on the possible superconducting (SC) pairing symmetries recently proposed, the quasiparticle interference (QPI) patterns in electron- and hole-doped Sr₂IrO₄ are theoretically investigated. In the electron-doped case, the QPI spectra can be explained based on a model similar to the octet model of the cuprates while in the hole-doped case, both the Fermi surface topology and the sign of the SC order parameter resemble those of the iron pnictides and there exists a QPI vector resulting from the interpocket scattering between the electron and hole pockets. In both cases, the evolution of the QPI vectors with energy and their behaviors in the nonmagnetic and magnetic impurity scattering cases can well be explained based on the evolution of the constant-energy contours and the sign structure of the SC order parameter. The QPI spectra presented in this paper can be compared with future scanning tunneling microscopy experiments to test whether there are SC phases in electron- and hole-doped Sr₂IrO₄ and what the pairing symmetry is.

Crystal defect studies using x-ray diffuse scattering

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

Larson, B.C.

1980-01-01

Microscopic lattice defects such as point (single atom) defects, dislocation loops, and solute precipitates are characterized by local electronic density changes at the defect sites and by distortions of the lattice structure surrounding the defects. The effect of these interruptions of the crystal lattice on the scattering of x-rays is considered in this paper, and examples are presented of the use of the diffuse scattering to study the defects. X-ray studies of self-interstitials in electron irradiated aluminum and copper are discussed in terms of the identification of the interstitial configuration. Methods for detecting the onset of point defect aggregation intomore » dislocation loops are considered and new techniques for the determination of separate size distributions for vacancy loops and interstitial loops are presented. Direct comparisons of dislocation loop measurements by x-rays with existing electron microscopy studies of dislocation loops indicate agreement for larger size loops, but x-ray measurements report higher concentrations in the smaller loop range. Methods for distinguishing between loops and three-dimensional precipitates are discussed and possibilities for detailed studies considered. A comparison of dislocation loop size distributions obtained from integral diffuse scattering measurements with those from TEM show a discrepancy in the smaller sizes similar to that described above.« less

Facile preparation of dendritic Ag-Pd bimetallic nanostructures on the surface of Cu foil for application as a SERS-substrate

NASA Astrophysics Data System (ADS)

Yi, Zao; Tan, Xiulan; Niu, Gao; Xu, Xibin; Li, Xibo; Ye, Xin; Luo, Jiangshan; Luo, Binchi; Wu, Weidong; Tang, Yongjian; Yi, Yougen

2012-05-01

Dendritic Ag-Pd bimetallic nanostructures have been synthesized on the surface of Cu foil via a multi-stage galvanic replacement reaction (MGRR) of Ag dendrites in a Na2PdCl4 solution. After five stages of replacement reaction, one obtained structures with protruding Ag-Pd flakes; these will mature into many porous structures with a few Ag atoms that are left over dendrites. The dendritic Ag-Pd bimetallic nanostructures were characterized by transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), field emission scanning electron microscopy (FESEM), energy-dispersive X-ray (EDX), selected area electron diffraction (SAED) and X-ray photoelectron spectroscopy (XPS). The morphology of the products strongly depended on the stage of galvanic replacement reaction and reaction temperature. The morphology and composition-dependent surface-enhanced Raman scattering (SERS) of the as-synthesized Ag-Pd bimetallic nanostructures were investigated. The effectiveness of these dendritic Ag-Pd bimetallic nanostructures on the surface of Cu foil as substrates toward SERS detection was evaluated by using rhodamine 6G (R6G) as a probe molecule. The results indicate that as-synthesized dendritic Ag-Pd bimetallic nanostructures are good candidates for SERS spectroscopy.

Magnetic effects in the paraxial regime of elastic electron scattering

NASA Astrophysics Data System (ADS)

Edström, Alexander; Lubk, Axel; Rusz, Ján

2016-11-01

Motivated by a recent claim [Phys. Rev. Lett. 116, 127203 (2016), 10.1103/PhysRevLett.116.127203] that electron vortex beams can be used to image magnetism at the nanoscale in elastic scattering experiments, using transmission electron microscopy, a comprehensive computational study is performed to study magnetic effects in the paraxial regime of elastic electron scattering in magnetic solids. Magnetic interactions from electron vortex beams, spin polarized electron beams, and beams with phase aberrations are considered, as they pass through ferromagnetic FePt or antiferromagnetic LaMnAsO. The magnetic signals are obtained by comparing the intensity over a disk in the diffraction plane for beams with opposite angular momentum or aberrations. The strongest magnetic signals are obtained from vortex beams with large orbital angular momentum, where relative magnetic signals above 10-3 are indicated for 10 ℏ orbital angular momentum, meaning that relative signals of one percent could be expected with the even larger orbital angular momenta, which have been produced in experimental setups. All results indicate that beams with low acceleration voltage and small convergence angles yield stronger magnetic signals, which is unfortunately problematic for the possibility of high spatial resolution imaging. Nevertheless, under atomic resolution conditions, relative magnetic signals in the order of 10-4 are demonstrated, corresponding to an increase with one order of magnitude compared to previous work.

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

Chen, Limiao, E-mail: chenlimiao@csu.edu.cn; Jing, Qifeng; Chen, Jun

Silver nanostructures with dendritic, flower-like and irregular morphologies were controllably deposited on a silicon substrate in an aqueous hydrogen fluoride solution at room temperature. The morphology of the Ag nanostructures changed from dendritic to urchin-like, flowerlike and pinecone-like with increasing the concentration of polyvinyl pyrrolidone (MW = 55,000) from 2 to 10 mM. The Ag nanostructures were characterized by transmission electron microscopy, high-resolution transmission electron microscopy, scanning electron microscopy, energy-dispersive X-ray, and X-ray diffraction. Through a series of time-dependent morphological evolution studies, the growth processes of Ag nanostructures have been systematically investigated and the corresponding growth mechanisms have been discussed.more » In addition, the morphology-dependent surface-enhanced Raman scattering of as-synthesized Ag nanostructures were investigated. The results indicated that flower-like Ag nanostructure had the highest activity than the other Ag nanostructures for Rhodamine 6G probe molecules. Highlights: • A simple method was developed to prepare dendritic and flower-like Ag nanostructures. • The flower-like Ag nanoparticles exhibit highest SERS activity. • The SERS substrate based on flower-like Ag particles can be used to detect melamine.« less

Characterization of new DOPC/DHPC platform for dermal applications.

PubMed

Rodríguez, Gelen; Rubio, Laia; Barba, Clara; López-Iglesias, Carmen; de la Maza, Alfons; López, Olga; Cócera, Mercedes

2013-05-01

Systems formed by mixtures of the phospholipids dioleoylphosphatidylcholine (DOPC) and dihexanoylphosphatidylcholine (DHPC) were characterized by use of differential scanning calorimetry, small angle X-ray scattering and two electron-microscopy techniques, freeze fracture electron microscopy and cryogenic transmission electron microscopy. These techniques allowed for the determination of the size, morphology, structural topology, self-assembly and thermotropic behavior of the nanostructures present in the mixtures. The interaction between the two phospholipids provides curvatures, irregularities and the increase of thickness and flexibility in the membrane. These effects led to the formation of different aggregates with a differential distribution of both phospholipids. The effect of these systems on the skin in vivo was evaluated by measurement of the biophysical skin parameters. Our results show that the DOPC/DHPC application induces a decrease in the permeability and in the hydration of the tissue. These effects in vivo are related to different microstructural changes promoted by these systems in the skin in vitro, published in a recent work. The fundamental biophysical analyses of DOPC/DHPC systems contribute to our understanding of the mechanisms that govern their interaction with the skin.

Self-assembly approach toward magnetic silica-type nanoparticles of different shapes from reverse block copolymer mesophases.

PubMed

Garcia, Carlos B W; Zhang, Yuanming; Mahajan, Surbhi; DiSalvo, Francis; Wiesner, Ulrich

2003-11-05

In the present study poly(isoprene-block-ethylene oxide), PI-b-PEO, block copolymers are used to structure iron oxide and silica precursors into reverse mesophases, which upon dissolution of the organic matrix lead to well-defined nanoparticles of spheres, cylinders, and plates based on the original structure of the mesophase prepared. The hybrid mesophases with sphere, cylinder, and lamellar morphologies containing the inorganic components in the minority phases are characterized through a combination of small-angle X-ray scattering (SAXS), transmission electron microscopy (TEM), scanning transmission electron microscopy (STEM), and electron energy loss spectroscopy (EELS). After heat treatments the respective nanoparticles on mica surfaces are characterized by scanning force microscopy (SFM). X-ray diffraction (XRD) and superconducting quantum interference device (SQUID) magnetometer measurements are performed to demonstrate that the heat treatment leads to the formation of a magnetic gamma-Fe2O3 crystalline phase within the amorphous aluminosilicate. The results pave the way to functional, i.e., magnetic nanoparticles where the size, shape, and iron oxide concentration can be controlled opening a range of possible applications.

Visualization of carrier dynamics in p(n)-type GaAs by scanning ultrafast electron microscopy

PubMed Central

Cho, Jongweon; Hwang, Taek Yong; Zewail, Ahmed H.

2014-01-01

Four-dimensional scanning ultrafast electron microscopy is used to investigate doping- and carrier-concentration-dependent ultrafast carrier dynamics of the in situ cleaved single-crystalline GaAs(110) substrates. We observed marked changes in the measured time-resolved secondary electrons depending on the induced alterations in the electronic structure. The enhancement of secondary electrons at positive times, when the electron pulse follows the optical pulse, is primarily due to an energy gain involving the photoexcited charge carriers that are transiently populated in the conduction band and further promoted by the electron pulse, consistent with a band structure that is dependent on chemical doping and carrier concentration. When electrons undergo sufficient energy loss on their journey to the surface, dark contrast becomes dominant in the image. At negative times, however, when the electron pulse precedes the optical pulse (electron impact), the dynamical behavior of carriers manifests itself in a dark contrast which indicates the suppression of secondary electrons upon the arrival of the optical pulse. In this case, the loss of energy of material’s electrons is by collisions with the excited carriers. These results for carrier dynamics in GaAs(110) suggest strong carrier–carrier scatterings which are mirrored in the energy of material’s secondary electrons during their migration to the surface. The approach presented here provides a fundamental understanding of materials probed by four-dimensional scanning ultrafast electron microscopy, and offers possibilities for use of this imaging technique in the study of ultrafast charge carrier dynamics in heterogeneously patterned micro- and nanostructured material surfaces and interfaces. PMID:24469803

Visualization of carrier dynamics in p(n)-type GaAs by scanning ultrafast electron microscopy.

PubMed

Cho, Jongweon; Hwang, Taek Yong; Zewail, Ahmed H

2014-02-11

Four-dimensional scanning ultrafast electron microscopy is used to investigate doping- and carrier-concentration-dependent ultrafast carrier dynamics of the in situ cleaved single-crystalline GaAs(110) substrates. We observed marked changes in the measured time-resolved secondary electrons depending on the induced alterations in the electronic structure. The enhancement of secondary electrons at positive times, when the electron pulse follows the optical pulse, is primarily due to an energy gain involving the photoexcited charge carriers that are transiently populated in the conduction band and further promoted by the electron pulse, consistent with a band structure that is dependent on chemical doping and carrier concentration. When electrons undergo sufficient energy loss on their journey to the surface, dark contrast becomes dominant in the image. At negative times, however, when the electron pulse precedes the optical pulse (electron impact), the dynamical behavior of carriers manifests itself in a dark contrast which indicates the suppression of secondary electrons upon the arrival of the optical pulse. In this case, the loss of energy of material's electrons is by collisions with the excited carriers. These results for carrier dynamics in GaAs(110) suggest strong carrier-carrier scatterings which are mirrored in the energy of material's secondary electrons during their migration to the surface. The approach presented here provides a fundamental understanding of materials probed by four-dimensional scanning ultrafast electron microscopy, and offers possibilities for use of this imaging technique in the study of ultrafast charge carrier dynamics in heterogeneously patterned micro- and nanostructured material surfaces and interfaces.

Back-scattered electron imaging of a non-vertebral case of hypervitaminosis A in a cat.

PubMed

Franch, J; Pastor, J; Franch, B; Durall, I; Manzanares, M C

2000-03-01

We describe a clinical case of hypervitaminosis A in a cat. The main lesions were bony fusions of both the hip and stifle joints, without spinal involvement. A post-mortem study using back-scattered scanning electron microscopy (BEI-SEM) revealed that exostoses had formed around the joints without articular surface involvement. The more recently formed areas of bony proliferation were composed mainly of chondroid tissue surrounded by different degrees of woven bone. As the bony reaction occurred, remodelling of the trabeculae was observed which lead to progressive substitution of chondroid tissue by woven bone surrounded by apposition of lamellar bone. No traces of calcified cartilage were observed in any of the bone sections evaluated. Copyright 2000 European Society of Feline Medicine.

Microstructures and magnetic properties of Co-Al-O granular thin films

NASA Astrophysics Data System (ADS)

Ohnuma, M.; Hono, K.; Onodera, H.; Ohnuma, S.; Fujimori, H.; Pedersen, J. S.

2000-01-01

The microstructures of Co-Al-O thin films of wide varieties of compositions are studied by transmission electron microscopy and small angle x-ray scattering (SAXS). In the superparamagnetic specimens, high resolution electron microscope images reveal that isolated spherical Co particles are surrounded by an amorphous aluminum oxide matrix. However, in the soft ferromagnetic films, the shape of the Co particles is prolate ellipsoidal. SAXS intensities from the soft magnetic specimens decrease inversely with the wave vector, q, in a low wave-vector region, while an interparticle interference peak is observed for the superparamagnetic specimens. The scattering profiles of the soft magnetic films imply that the Co particles have a cylindrical shape and are randomly oriented. The correlation between the magnetic properties and the microstructures is discussed.

Analyzing indirect secondary electron contrast of unstained bacteriophage T4 based on SEM images and Monte Carlo simulations

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

Ogura, Toshihiko, E-mail: t-ogura@aist.go.jp

2009-03-06

The indirect secondary electron contrast (ISEC) condition of the scanning electron microscopy (SEM) produces high contrast detection with minimal damage of unstained biological samples mounted under a thin carbon film. The high contrast image is created by a secondary electron signal produced under the carbon film by a low acceleration voltage. Here, we show that ISEC condition is clearly able to detect unstained bacteriophage T4 under a thin carbon film (10-15 nm) by using high-resolution field emission (FE) SEM. The results show that FE-SEM provides higher resolution than thermionic emission SEM. Furthermore, we investigated the scattered electron area within themore » carbon film under ISEC conditions using Monte Carlo simulation. The simulations indicated that the image resolution difference is related to the scattering width in the carbon film and the electron beam spot size. Using ISEC conditions on unstained virus samples would produce low electronic damage, because the electron beam does not directly irradiate the sample. In addition to the routine analysis, this method can be utilized for structural analysis of various biological samples like viruses, bacteria, and protein complexes.« less

Angularly-selective transmission imaging in a scanning electron microscope.

PubMed

Holm, Jason; Keller, Robert R

2016-08-01

This work presents recent advances in transmission scanning electron microscopy (t-SEM) imaging control capabilities. A modular aperture system and a cantilever-style sample holder that enable comprehensive angular selectivity of forward-scattered electrons are described. When combined with a commercially available solid-state transmission detector having only basic bright-field and dark-field imaging capabilities, the advances described here enable numerous transmission imaging modes. Several examples are provided that demonstrate how contrast arising from diffraction to mass-thickness can be obtained. Unanticipated image contrast at some imaging conditions is also observed and addressed. Published by Elsevier B.V.

Time-resolved scanning electron microscopy with polarization analysis

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

Frömter, Robert, E-mail: rfroemte@physik.uni-hamburg.de; Oepen, Hans Peter; The Hamburg Centre for Ultrafast Imaging, Luruper Chaussee 149, 22761 Hamburg

2016-04-04

We demonstrate the feasibility of investigating periodically driven magnetization dynamics in a scanning electron microscope with polarization analysis based on spin-polarized low-energy electron diffraction. With the present setup, analyzing the time structure of the scattering events, we obtain a temporal resolution of 700 ps, which is demonstrated by means of imaging the field-driven 100 MHz gyration of the vortex in a soft-magnetic FeCoSiB square. Owing to the efficient intrinsic timing scheme, high-quality movies, giving two components of the magnetization simultaneously, can be recorded on the time scale of hours.

Measuring nanometre-scale electric fields in scanning transmission electron microscopy using segmented detectors.

PubMed

Brown, H G; Shibata, N; Sasaki, H; Petersen, T C; Paganin, D M; Morgan, M J; Findlay, S D

2017-11-01

Electric field mapping using segmented detectors in the scanning transmission electron microscope has recently been achieved at the nanometre scale. However, converting these results to quantitative field measurements involves assumptions whose validity is unclear for thick specimens. We consider three approaches to quantitative reconstruction of the projected electric potential using segmented detectors: a segmented detector approximation to differential phase contrast and two variants on ptychographical reconstruction. Limitations to these approaches are also studied, particularly errors arising from detector segment size, inelastic scattering, and non-periodic boundary conditions. A simple calibration experiment is described which corrects the differential phase contrast reconstruction to give reliable quantitative results despite the finite detector segment size and the effects of plasmon scattering in thick specimens. A plasmon scattering correction to the segmented detector ptychography approaches is also given. Avoiding the imposition of periodic boundary conditions on the reconstructed projected electric potential leads to more realistic reconstructions. Copyright © 2017 Elsevier B.V. All rights reserved.

Nanostructural reorganization of bacterial cellulose by ultrasonic treatment.

PubMed

Tischer, Paula C S Faria; Sierakowski, Maria Rita; Westfahl, Harry; Tischer, Cesar Augusto

2010-05-10

In this work, bacterial cellulose was subjected to a high-power ultrasonic treatment for different time intervals. The morphological analysis, scanning electron microscopy, and atomic force microscopy revealed that this treatment changed the width and height of the microfibrillar ribbons and roughness of their surface, originating films with new nanostructures. Differential thermal analysis showed a higher thermal stability for ultrasonicated samples with a pyrolysis onset temperature of 208 degrees C for native bacterial cellulose and 250 and 268 degrees C for the modified samples. The small-angle X-ray scattering experiments demonstrated that the treatment with ultrasound increased the thickness of the ribbons, while wide-angle X-ray scattering experiments demonstrated that the average crystallite dimension and the degree of crystallinity also increased. A model is proposed where the thicker ribbons and crystallites result from the fusion of neighboring ribbons due to cavitation effects.

Coherent anti-Stokes Raman scattering microscopy of single nanodiamonds

NASA Astrophysics Data System (ADS)

Pope, Iestyn; Payne, Lukas; Zoriniants, George; Thomas, Evan; Williams, Oliver; Watson, Peter; Langbein, Wolfgang; Borri, Paola

2014-11-01

Nanoparticles have attracted enormous attention for biomedical applications as optical labels, drug-delivery vehicles and contrast agents in vivo. In the quest for superior photostability and biocompatibility, nanodiamonds are considered one of the best choices due to their unique structural, chemical, mechanical and optical properties. So far, mainly fluorescent nanodiamonds have been utilized for cell imaging. However, their use is limited by the efficiency and costs in reliably producing fluorescent defect centres with stable optical properties. Here, we show that single non-fluorescing nanodiamonds exhibit strong coherent anti-Stokes Raman scattering (CARS) at the sp3 vibrational resonance of diamond. Using correlative light and electron microscopy, the relationship between CARS signal strength and nanodiamond size is quantified. The calibrated CARS signal in turn enables the analysis of the number and size of nanodiamonds internalized in living cells in situ, which opens the exciting prospect of following complex cellular trafficking pathways quantitatively.

Coherent anti-Stokes Raman scattering microscopy of single nanodiamonds

PubMed Central

Pope, Iestyn; Payne, Lukas; Zoriniants, George; Thomas, Evan; Williams, Oliver; Watson, Peter; Langbein, Wolfgang; Borri, Paola

2016-01-01

Nanoparticles have attracted enormous attention for biomedical applications as optical labels, drug delivery vehicles, and contrast agents in vivo. In the quest for superior photostability and bio-compatibility, nanodiamonds (NDs) are considered one of the best choices due to their unique structural, chemical, mechanical, and optical properties. So far, mainly fluorescent NDs have been utilized for cell imaging. However, their use is limited by the efficiency and costs in reliably producing fluorescent defect centers with stable optical properties. Here, we show that single non-fluorescing NDs exhibit strong coherent anti-Stokes Raman scattering (CARS) at the sp3 vibrational resonance of diamond. Using correlative light and electron microscopy, the relationship between CARS signal strength and ND size is quantified. The calibrated CARS signal in turn enables the analysis of the number and size of NDs internalized in living cells in situ, which opens the exciting prospect of following complex cellular trafficking pathways quantitatively. PMID:25305746

Coherent anti-Stokes Raman scattering microscopy of single nanodiamonds.

PubMed

Pope, Iestyn; Payne, Lukas; Zoriniants, George; Thomas, Evan; Williams, Oliver; Watson, Peter; Langbein, Wolfgang; Borri, Paola

2014-11-01

Nanoparticles have attracted enormous attention for biomedical applications as optical labels, drug-delivery vehicles and contrast agents in vivo. In the quest for superior photostability and biocompatibility, nanodiamonds are considered one of the best choices due to their unique structural, chemical, mechanical and optical properties. So far, mainly fluorescent nanodiamonds have been utilized for cell imaging. However, their use is limited by the efficiency and costs in reliably producing fluorescent defect centres with stable optical properties. Here, we show that single non-fluorescing nanodiamonds exhibit strong coherent anti-Stokes Raman scattering (CARS) at the sp(3) vibrational resonance of diamond. Using correlative light and electron microscopy, the relationship between CARS signal strength and nanodiamond size is quantified. The calibrated CARS signal in turn enables the analysis of the number and size of nanodiamonds internalized in living cells in situ, which opens the exciting prospect of following complex cellular trafficking pathways quantitatively.

Atomic scale imaging of magnetic circular dichroism by achromatic electron microscopy.

PubMed

Wang, Zechao; Tavabi, Amir H; Jin, Lei; Rusz, Ján; Tyutyunnikov, Dmitry; Jiang, Hanbo; Moritomo, Yutaka; Mayer, Joachim; Dunin-Borkowski, Rafal E; Yu, Rong; Zhu, Jing; Zhong, Xiaoyan

2018-03-01

In order to obtain a fundamental understanding of the interplay between charge, spin, orbital and lattice degrees of freedom in magnetic materials and to predict and control their physical properties 1-3 , experimental techniques are required that are capable of accessing local magnetic information with atomic-scale spatial resolution. Here, we show that a combination of electron energy-loss magnetic chiral dichroism 4 and chromatic-aberration-corrected transmission electron microscopy, which reduces the focal spread of inelastically scattered electrons by orders of magnitude when compared with the use of spherical aberration correction alone, can achieve atomic-scale imaging of magnetic circular dichroism and provide element-selective orbital and spin magnetic moments atomic plane by atomic plane. This unique capability, which we demonstrate for Sr 2 FeMoO 6 , opens the door to local atomic-level studies of spin configurations in a multitude of materials that exhibit different types of magnetic coupling, thereby contributing to a detailed understanding of the physical origins of magnetic properties of materials at the highest spatial resolution.

Hollow Cone Electron Imaging for Single Particle 3D Reconstruction of Proteins

PubMed Central

Tsai, Chun-Ying; Chang, Yuan-Chih; Lobato, Ivan; Van Dyck, Dirk; Chen, Fu-Rong

2016-01-01

The main bottlenecks for high-resolution biological imaging in electron microscopy are radiation sensitivity and low contrast. The phase contrast at low spatial frequencies can be enhanced by using a large defocus but this strongly reduces the resolution. Recently, phase plates have been developed to enhance the contrast at small defocus but electrical charging remains a problem. Single particle cryo-electron microscopy is mostly used to minimize the radiation damage and to enhance the resolution of the 3D reconstructions but it requires averaging images of a massive number of individual particles. Here we present a new route to achieve the same goals by hollow cone dark field imaging using thermal diffuse scattered electrons giving about a 4 times contrast increase as compared to bright field imaging. We demonstrate the 3D reconstruction of a stained GroEL particle can yield about 13.5 Å resolution but using a strongly reduced number of images. PMID:27292544

Applications and limitations of electron correlation microscopy to study relaxation dynamics in supercooled liquids

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

Zhang, Pei; He, Li; Besser, Matthew F.

Here, electron correlation microscopy (ECM) is a way to measure structural relaxation times, τ, of liquids with nanometer-scale spatial resolution using coherent electron scattering equivalent of photon correlation spectroscopy. We have applied ECM with a 3.5 nm diameter probe to Pt 57.5Cu 14.7Ni 5.3P 22.5 amorphous nanorods and Pd 40Ni 40P 20 bulk metallic glass (BMG) heated inside the STEM into the supercooled liquid region. These data demonstrate that the ECM technique is limited by the characteristics of the time series, which must be at least 40τ to obtain a well-converged correlation function g 2(t), and the time per frame,more » which must be less than 0.1τ to obtain sufficient sampling. A high-speed direct electron camera enables fast acquisition and affords reliable g 2(t) data even with low signal per frame.« less

Applications and limitations of electron correlation microscopy to study relaxation dynamics in supercooled liquids

DOE PAGES

Zhang, Pei; He, Li; Besser, Matthew F.; ...

2016-09-08

Here, electron correlation microscopy (ECM) is a way to measure structural relaxation times, τ, of liquids with nanometer-scale spatial resolution using coherent electron scattering equivalent of photon correlation spectroscopy. We have applied ECM with a 3.5 nm diameter probe to Pt 57.5Cu 14.7Ni 5.3P 22.5 amorphous nanorods and Pd 40Ni 40P 20 bulk metallic glass (BMG) heated inside the STEM into the supercooled liquid region. These data demonstrate that the ECM technique is limited by the characteristics of the time series, which must be at least 40τ to obtain a well-converged correlation function g 2(t), and the time per frame,more » which must be less than 0.1τ to obtain sufficient sampling. A high-speed direct electron camera enables fast acquisition and affords reliable g 2(t) data even with low signal per frame.« less

Size-dependent surface-enhanced Raman scattering of sodium benzoate on Silver nanoparticles

NASA Astrophysics Data System (ADS)

Badr, Y.; Mahmoud, M. A.

2005-07-01

The absorption spectrum of silver nanoparticles (Ag NPs) with different size and the transmission electron microscopy (TEM) was recorded. Surface-enhanced Raman scattering (SERS) spectra of Sodium Benzoate (SB) adsorbed on Ag NPs with different particle size were studied. The carboxylic group bands were enhanced as the particle size decreases due to the chemisorption of SB on the Ag NPs through it in which the carboxyl group was perpendicular to the surface and the benzene ring parallel to the surface; the SB bands were enhanced as the coverage density of Ag NPs increased.

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.

Characteristics of angular cross correlations studied by light scattering from two-dimensional microsphere films

NASA Astrophysics Data System (ADS)

Schroer, M. A.; Gutt, C.; Grübel, G.

2014-07-01

Recently the analysis of scattering patterns by angular cross-correlation analysis (CCA) was introduced to reveal the orientational order in disordered samples with special focus to future applications on x-ray free-electron laser facilities. We apply this CCA approach to ultra-small-angle light-scattering data obtained from two-dimensional monolayers of microspheres. The films were studied in addition by optical microscopy. This combined approach allows to calculate the cross-correlations of the scattering patterns, characterized by the orientational correlation function Ψl(q), as well as to obtain the real-space structure of the monolayers. We show that CCA is sensitive to the orientational order of monolayers formed by the microspheres which are not directly visible from the scattering patterns. By mixing microspheres of different radii the sizes of ordered monolayer domains is reduced. For these samples it is shown that Ψl(q) quantitatively describes the degree of hexagonal order of the two-dimensional films. The experimental CCA results are compared with calculations based on the microscopy images. Both techniques show qualitatively similar features. Differences can be attributed to the wave-front distortion of the laser beam in the experiment. This effect is discussed by investigating the effect of different wave fronts on the cross-correlation analysis results. The so-determined characteristics of the cross-correlation analysis will be also relevant for future x-ray-based studies.

Three-dimensional nanoscale imaging by plasmonic Brownian microscopy

NASA Astrophysics Data System (ADS)

Labno, Anna; Gladden, Christopher; Kim, Jeongmin; Lu, Dylan; Yin, Xiaobo; Wang, Yuan; Liu, Zhaowei; Zhang, Xiang

2017-12-01

Three-dimensional (3D) imaging at the nanoscale is a key to understanding of nanomaterials and complex systems. While scanning probe microscopy (SPM) has been the workhorse of nanoscale metrology, its slow scanning speed by a single probe tip can limit the application of SPM to wide-field imaging of 3D complex nanostructures. Both electron microscopy and optical tomography allow 3D imaging, but are limited to the use in vacuum environment due to electron scattering and to optical resolution in micron scales, respectively. Here we demonstrate plasmonic Brownian microscopy (PBM) as a way to improve the imaging speed of SPM. Unlike photonic force microscopy where a single trapped particle is used for a serial scanning, PBM utilizes a massive number of plasmonic nanoparticles (NPs) under Brownian diffusion in solution to scan in parallel around the unlabeled sample object. The motion of NPs under an evanescent field is three-dimensionally localized to reconstruct the super-resolution topology of 3D dielectric objects. Our method allows high throughput imaging of complex 3D structures over a large field of view, even with internal structures such as cavities that cannot be accessed by conventional mechanical tips in SPM.

Extremely strong self-assembly of a bimetallic salen complex visualized at the single-molecule level.

PubMed

Salassa, Giovanni; Coenen, Michiel J J; Wezenberg, Sander J; Hendriksen, Bas L M; Speller, Sylvia; Elemans, Johannes A A W; Kleij, Arjan W

2012-04-25

A bis-Zn(salphen) structure shows extremely strong self-assembly both in solution as well as at the solid-liquid interface as evidenced by scanning tunneling microscopy, competitive UV-vis and fluorescence titrations, dynamic light scattering, and transmission electron microscopy. Density functional theory analysis on the Zn(2) complex rationalizes the very high stability of the self-assembled structures provoked by unusual oligomeric (Zn-O)(n) coordination motifs within the assembly. This coordination mode is strikingly different when compared with mononuclear Zn(salphen) analogues that form dimeric structures having a typical Zn(2)O(2) central unit. The high stability of the multinuclear structure therefore holds great promise for the development of stable self-assembled monolayers with potential for new opto-electronic materials.

Thermoelectric properties of Co4Sb12 with Bi2Te3 nanoinclusions

NASA Astrophysics Data System (ADS)

Ghosh, Sanyukta; Bisht, Anuj; Karati, Anirudha; Rogl, Gerda; Rogl, Peter; Murty, B. S.; Suwas, Satyam; Mallik, Ramesh Chandra

2018-03-01

The figure of merit (zT) of a thermoelectric material can be enhanced by incorporation of nanoinclusions into bulk material. The presence of bismuth telluride (Bi2Te3) nanoinclusions in Co4Sb12 leads to lower phonon thermal conductivity by introducing interfaces and defects; it enhances the average zT between 300-700 K. In the current study, Bi2Te3 nanoparticles were dispersed into bulk Co4Sb12 by ball-milling. The bulk was fabricated by spark plasma sintering. The presence of Bi2Te3 dispersion in Co4Sb12 was confirmed by x-ray diffraction, scanning electron microscopy, transmission electron microscopy and electron back scattered diffraction technique. Energy dispersive spectroscopy showed antimony (Sb) as an impurity phase for higher contents of Bi2Te3 in the sample. The Seebeck coefficient (S) and electrical conductivity (σ) were measured in the temperature range of 350-673 K. The negative value of S indicates that most of the charge carriers were electrons. A decrease in S and increase in σ with Bi2Te3 content are due to the increased carrier concentration, as confirmed by Hall measurement. The thermal conductivity, measured between 423-673 K, decreased due to the increased phonon scattering at interfaces. A maximum zT of 0.17 was achieved at 523 K and it did not vary much throughout the temperature range. The experimental results of composites were compared by using effective medium theories.

Thermoelectric properties of Co4Sb12 with Bi2Te3 nanoinclusions.

PubMed

Ghosh, Sanyukta; Bisht, Anuj; Karati, Anirudha; Rogl, Gerda; Rogl, Peter; Murty, B S; Suwas, Satyam; Mallik, Ramesh Chandra

2018-02-12

The figure of merit (zT) of a thermoelectric material can be enhanced by incorporation of nanoinclusions into bulk material. The presence of bismuth telluride (Bi 2 Te 3 ) nanoinclusions in Co 4 Sb 12 leads to lower phonon thermal conductivity by introducing interfaces and defects; it enhances the average zT between 300-700 K. In the current study, Bi 2 Te 3 nanoparticles were dispersed into bulk Co 4 Sb 12 by ball-milling. The bulk was fabricated by spark plasma sintering. The presence of Bi 2 Te 3 dispersion in Co 4 Sb 12 was confirmed by x-ray diffraction, scanning electron microscopy, transmission electron microscopy and electron back scattered diffraction technique. Energy dispersive spectroscopy showed antimony (Sb) as an impurity phase for higher contents of Bi 2 Te 3 in the sample. The Seebeck coefficient (S) and electrical conductivity (σ) were measured in the temperature range of 350-673 K. The negative value of S indicates that most of the charge carriers were electrons. A decrease in S and increase in σ with Bi 2 Te 3 content are due to the increased carrier concentration, as confirmed by Hall measurement. The thermal conductivity, measured between 423-673 K, decreased due to the increased phonon scattering at interfaces. A maximum zT of 0.17 was achieved at 523 K and it did not vary much throughout the temperature range. The experimental results of composites were compared by using effective medium theories.

Photoisomerisation and light-induced morphological switching of a polyoxometalate-azobenzene hybrid.

PubMed

Markiewicz, Grzegorz; Pakulski, Dawid; Galanti, Agostino; Patroniak, Violetta; Ciesielski, Artur; Stefankiewicz, Artur R; Samorì, Paolo

2017-06-29

The functionalization of a spherical Keplerate-type polyoxometalate {Mo 72 V 30 } with a cationic azobenzene surfactant has been achieved through ionic self-assembly. The photoisomerisation reaction of this complex, which emerges in a light-triggered aggregation-disaggregation process, has been followed by 1 H NMR spectroscopy, dynamic light scattering, absorption spectroscopy and scanning electron microscopy analyses.

Conventions and workflows for using Situs

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

Wriggers, Willy, E-mail: wriggers@biomachina.org

2012-04-01

Recent developments of the Situs software suite for multi-scale modeling are reviewed. Typical workflows and conventions encountered during processing of biophysical data from electron microscopy, tomography or small-angle X-ray scattering are described. Situs is a modular program package for the multi-scale modeling of atomic resolution structures and low-resolution biophysical data from electron microscopy, tomography or small-angle X-ray scattering. This article provides an overview of recent developments in the Situs package, with an emphasis on workflows and conventions that are important for practical applications. The modular design of the programs facilitates scripting in the bash shell that allows specific programs tomore » be combined in creative ways that go beyond the original intent of the developers. Several scripting-enabled functionalities, such as flexible transformations of data type, the use of symmetry constraints or the creation of two-dimensional projection images, are described. The processing of low-resolution biophysical maps in such workflows follows not only first principles but often relies on implicit conventions. Situs conventions related to map formats, resolution, correlation functions and feature detection are reviewed and summarized. The compatibility of the Situs workflow with CCP4 conventions and programs is discussed.« less

StatSTEM: An efficient approach for accurate and precise model-based quantification of atomic resolution electron microscopy images.

PubMed

De Backer, A; van den Bos, K H W; Van den Broek, W; Sijbers, J; Van Aert, S

2016-12-01

An efficient model-based estimation algorithm is introduced to quantify the atomic column positions and intensities from atomic resolution (scanning) transmission electron microscopy ((S)TEM) images. This algorithm uses the least squares estimator on image segments containing individual columns fully accounting for overlap between neighbouring columns, enabling the analysis of a large field of view. For this algorithm, the accuracy and precision with which measurements for the atomic column positions and scattering cross-sections from annular dark field (ADF) STEM images can be estimated, has been investigated. The highest attainable precision is reached even for low dose images. Furthermore, the advantages of the model-based approach taking into account overlap between neighbouring columns are highlighted. This is done for the estimation of the distance between two neighbouring columns as a function of their distance and for the estimation of the scattering cross-section which is compared to the integrated intensity from a Voronoi cell. To provide end-users this well-established quantification method, a user friendly program, StatSTEM, is developed which is freely available under a GNU public license. Copyright © 2016 Elsevier B.V. All rights reserved.

Atomically Thin Graphene Windows That Enable High Contrast Electron Microscopy without a Specimen Vacuum Chamber.

PubMed

Han, Yimo; Nguyen, Kayla X; Ogawa, Yui; Park, Jiwoong; Muller, David A

2016-12-14

Scanning electron microscopes (SEMs) require a high vacuum environment to generate and shape an electron beam for imaging; however, the vacuum conditions greatly limit the nature of specimens that can be examined. From a purely scattering physics perspective, it is not necessary to place the specimen inside the vacuum chamber-the mean free paths (MFPs) for electron scattering in air at typical SEM beam voltages are 50-100 μm. This is the idea behind the airSEM, which removes the specimen vacuum chamber from the SEM and places the sample in air. The thickness of the gas layer is less than a MFP from an electron-transparent window to preserve the shape and resolution of the incident beam, resulting in comparable imaging quality to an all-vacuum SEM. Present silicon nitride windows scatter far more strongly than the air gap and are currently the contrast and resolution limiting factor in the airSEM. Graphene windows have been used previously to wrap or seal samples in vacuum for imaging. Here we demonstrate the use of a robust bilayer graphene window for sealing the electron optics from the room environment, providing an electron transparent window with only a 2% drop in contrast. There is a 5-fold-increase in signal/noise ratio for imaging compared to multi-MFP-thick silicon nitride windows, enabling high contrast in backscattered, transmission, and surface imaging modes for the new airSEM geometry.

Microstructural features of carious human enamel imaged with back-scattered electrons.

PubMed

Pearce, E I; Nelson, D G

1989-02-01

We have used back-scattered electrons (BE) in the scanning electron microscope to produce mineral density images of enamel. Flat surfaces of artificially-carious enamel, softened in an intra-oral experiment, and naturally-carious (white spot) enamel were polished to a high gloss with diamond lapping compound, rendering them almost featureless by secondary electron scanning electron microscopy. They were then examined at 10 to 30 kV in a Philips 505 instrument fitted with a 4-quadrant BE detector. Study of surfaces prepared approximately parallel to the natural surface showed that mineral was lost from both prism core and the interprismatic region, leaving a thin mineral-rich rim at the prism periphery. The same lesions viewed longitudinally on a surface prepared perpendicular to the natural surface showed mineral-rich bands at the prism margins in the outer enamel. Near the advancing front of the lesion, the prism junctions were widened and the prism cores sometimes hypermineralized. Natural lesions sectioned in the prism long axis showed features previously seen with other techniques, e.g., cross-striations and striae of Retzius, but in much greater detail. Mineral enrichment at the prism periphery in the lesion body and a widening of the prism junction at the advancing fronts of lesions in permanent teeth were most obvious. Calculations showed that with an accelerating voltage of 30 kV, the images reflected mineral density up to 4 microns beneath the surface. BE microscopy produces a high-resolution image of mineral loss or gain in carious enamel, with relatively easy sample preparation.

Effect of void shape in Czochralski-Si wafers on the intensity of laser-scattering

NASA Astrophysics Data System (ADS)

Takahashi, J.; Kawakami, K.; Nakai, K.

2001-06-01

The shape effect of anisotropic-shaped microvoid defects in Czochralski-grown silicon wafers on the intensity of laser scattering has been investigated. The size and shape of the defects were examined by means of transmission electron microscopy. Octahedral voids in conventional (nitrogen-undoped) wafers showed an almost isotropic scattering property under the incident condition of a p-polarization beam. On the other hand, parallelepiped-plate-shaped voids in nitrogen-doped wafers showed an anisotropic scattering property on both p- and s-polarized components of scattered light, depending strongly on the incident laser direction. The measured results were explained not by scattering calculation using Born approximation but by calculation based on Rayleigh scattering. It was found that the s component is explained by an inclination of a dipole moment induced on a defect from the scattering plane. Furthermore, using numerical electromagnetic analysis it was shown that the asymmetric behavior of the s component on the parallelepiped-plate voids is ascribed to the parallelepiped shape effect. These results suggest that correction of the scattering intensity is necessary to evaluate the size and volume of anisotropic-shaped defects from the scattered intensity.

Polymeric capsule-cushioned leukocyte cell membrane vesicles as a biomimetic delivery platform

NASA Astrophysics Data System (ADS)

Gao, Changyong; Wu, Zhiguang; Lin, Zhihua; Lin, Xiankun; He, Qiang

2016-02-01

We report a biomimetic delivery of microsized capsule-cushioned leukocyte membrane vesicles (CLMVs) through the conversion of freshly reassembled leukocyte membrane vesicles (LMVs), including membrane lipids and membrane-bound proteins onto the surface of layer-by-layer assembled polymeric multilayer microcapsules. The leukocyte membrane coating was verified by using electron microscopy, a quartz crystal microbalance, dynamic light scattering, and confocal laser scanning microscopy. The resulting CLMVs have the ability to effectively evade clearance by the immune system and thus prolong the circulation time in mice. Moreover, we also show that the right-side-out leukocyte membrane coating can distinctly improve the accumulation of capsules in tumor sites through the molecular recognition of membrane-bound proteins of CLMVs with those of tumor cells in vitro and in vivo. The natural cell membrane camouflaged polymeric multilayer capsules with the immunosuppressive and tumor-recognition functionalities of natural leukocytes provide a new biomimetic delivery platform for disease therapy.We report a biomimetic delivery of microsized capsule-cushioned leukocyte membrane vesicles (CLMVs) through the conversion of freshly reassembled leukocyte membrane vesicles (LMVs), including membrane lipids and membrane-bound proteins onto the surface of layer-by-layer assembled polymeric multilayer microcapsules. The leukocyte membrane coating was verified by using electron microscopy, a quartz crystal microbalance, dynamic light scattering, and confocal laser scanning microscopy. The resulting CLMVs have the ability to effectively evade clearance by the immune system and thus prolong the circulation time in mice. Moreover, we also show that the right-side-out leukocyte membrane coating can distinctly improve the accumulation of capsules in tumor sites through the molecular recognition of membrane-bound proteins of CLMVs with those of tumor cells in vitro and in vivo. The natural cell membrane camouflaged polymeric multilayer capsules with the immunosuppressive and tumor-recognition functionalities of natural leukocytes provide a new biomimetic delivery platform for disease therapy. Electronic supplementary information (ESI) available. See DOI: 10.1039/c5nr08407e

Deep Tissue Fluorescent Imaging in Scattering Specimens Using Confocal Microscopy

PubMed Central

Clendenon, Sherry G.; Young, Pamela A.; Ferkowicz, Michael; Phillips, Carrie; Dunn, Kenneth W.

2015-01-01

In scattering specimens, multiphoton excitation and nondescanned detection improve imaging depth by a factor of 2 or more over confocal microscopy; however, imaging depth is still limited by scattering. We applied the concept of clearing to deep tissue imaging of highly scattering specimens. Clearing is a remarkably effective approach to improving image quality at depth using either confocal or multiphoton microscopy. Tissue clearing appears to eliminate the need for multiphoton excitation for deep tissue imaging. PMID:21729357

Phase behaviors of binary mixtures composed of electron-rich and electron-poor triphenylene discotic liquid crystals

NASA Astrophysics Data System (ADS)

An, Lingling; Jing, Min; Xiao, Bo; Bai, Xiao-Yan; Zeng, Qing-Dao; Zhao, Ke-Qing

2016-09-01

Disk-like liquid crystals (DLCs) can self-assemble to ordered columnar mesophases and are intriguing one-dimensional organic semiconductors with high charge carrier mobility. To improve their applicable property of mesomorphic temperature ranges, we exploit the binary mixtures of electronic donor-acceptor DLC materials. The electron-rich 2,3,6,7,10,11-hexakis(alkoxy)triphenylenes (C4, C6, C8, C10, C12) and an electron-deficient tetrapentyl triphenylene-2,3,6,10-tetracarboxylate have been prepared and their binary mixtures have been investigated. The mesomorphism of the 1:1 (molar ratio) mixtures has been characterized by polarizing optical microscopy (POM), differential scanning calorimetry (DSC), and small angel x-ray scattering (SAXS). The self-assembled monolayer structure of a discogen on a solid-liquid interface has been imaged by the high resolution scanning tunneling microscopy (STM). The match of peripheral chain length has important influence on the mesomorphism of the binary mixtures. Project supported by the National Natural Science Foundation of China (Grant Nos. 51273133 and 51443004).

Effect of Cooling Rates on γ → α Transformation and Metastable States in Fe-Cu Alloys with Addition of Ni

NASA Astrophysics Data System (ADS)

Crozet, C.; Verdier, M.; Lay, S.; Antoni-Zdziobek, A.

2018-07-01

α/γ phase transformations occurring in Fe-10Cu-xNi alloys (0 ≤ x ≤ 15 in mass%) were studied using X-ray diffraction, scanning electron microscopy, electron back scattered diffraction, transmission electron microscopy and chemical analysis, combining X-ray microanalysis with energy dispersive spectrometry in the scanning electron microscope and electron microprobe analysis with wavelength dispersive spectrometry. The influence of cooling rate on the microstructure was investigated using ice-brine quenching and 2 °C/min slow cooling rate performed with dilatometry. Ni addition induces metastable transformations on cooling: massive and bainitic ferrite are formed depending on the alloy composition and cooling rate. Moreover, most of the Cu phase precipitates on cooling giving rise to a fine distribution of Cu particles in the ferrite grains. For both cooling conditions, the hardness increases with increasing Ni content and a higher hardness is obtained in the quenched alloy for each composition. The change in hardness is correlated to the effect of Ni solid solution, transformation structure and size of Cu particles.

Green synthesis and characterization of alginate nanoparticles and its role as a biosorbent for Cr(VI) ions

NASA Astrophysics Data System (ADS)

Geetha, P.; Latha, M. S.; Pillai, Saumya S.; Deepa, B.; Santhosh Kumar, K.; Koshy, Mathew

2016-02-01

Green synthesis of nanoparticles has attained considerable attention in recent years because of its myriad of applications including drug delivery, tissue engineering and water purification. In the present study, alginate nanoparticles stabilized by honey were prepared by cross-linking aqueous solution of alginate with calcium ions. Honey mediated synthesis has been reported earlier for the production of metal nanoparticles. However no literature is available on the use of this technique for polymeric nanoparticles. Highly stable nanoparticles of 10-100 nm size were generated by this technique. The synthesised nanoparticles were characterized by transmission electron microscopy, scanning electron microscopy, atomic force microscopy, dynamic light scattering and Fourier transform infrared spectroscopic techniques. Potential of using these nanoparticles for heavy metal removal was studied by using Cr(VI) from aqueous solution, where a maximum removal efficiency of 93.5% was obtained. This method was also successfully employed for the production of other polymeric nanoparticles like casein, chitosan and albumin.

Worming Their Way into Shape: Toroidal Formations in Micellar Solutions

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

Cardiel Rivera, Joshua J.; Tonggu, Lige; Dohnalkova, Alice

2013-11-01

We report the formation of nanostructured toroidal micellar bundles (nTMB) from a semidilute wormlike micellar solution, evidenced by both cryogenicelectron microscopy and transmission electron microscopy images. Our strategy for creating nTMB involves a two-step protocol consisting of a simple prestraining process followed by flow through a microfluidic device containing an array of microposts, producing strain rates in the wormlike micelles on the order of 105 s^1. In combination with microfluidic confinement, these unusually large strain rates allow for the formation of stable nTMB. Electron microscopy images reveal a variety of nTMB morphologies and provide the size distribution of the nTMB.more » Small-angle neutron scattering indicates the underlying microstructural transition from wormlike micelles to nTMB. We also show that other flow-induced approaches such as sonication can induce and control the emergence of onion-like and nTMB structures, which may provide a useful tool for nanotemplating.« less

Tip-Enhanced Raman Scattering Microscopy: A Step toward Nanoscale Control of Intrinsic Molecular Properties

NASA Astrophysics Data System (ADS)

Yano, Taka-aki; Hara, Masahiko

2018-06-01

Tip-enhanced Raman scattering microscopy, a family of scanning probe microscopy techniques, has been recognized as a powerful surface analytical technique with both single-molecule sensitivity and angstrom-scale spatial resolution. This review covers the current status of tip-enhanced Raman scattering microscopy in surface and material nanosciences, including a brief history, the basic principles, and applications for the nanoscale characterization of a variety of nanomaterials. The focus is on the recent trend of combining tip-enhanced Raman scattering microscopy with various external stimuli such as pressure, voltage, light, and temperature, which enables the local control of the molecular properties and functions and also enables chemical reactions to be induced on a nanometer scale.

Combining gas-phase electrophoretic mobility molecular analysis (GEMMA), light scattering, field flow fractionation and cryo electron microscopy in a multidimensional approach to characterize liposomal carrier vesicles.

PubMed

Urey, Carlos; Weiss, Victor U; Gondikas, Andreas; von der Kammer, Frank; Hofmann, Thilo; Marchetti-Deschmann, Martina; Allmaier, Günter; Marko-Varga, György; Andersson, Roland

2016-11-20

For drug delivery, characterization of liposomes regarding size, particle number concentrations, occurrence of low-sized liposome artefacts and drug encapsulation are of importance to understand their pharmacodynamic properties. In our study, we aimed to demonstrate the applicability of nano Electrospray Gas-Phase Electrophoretic Mobility Molecular Analyser (nES GEMMA) as a suitable technique for analyzing these parameters. We measured number-based particle concentrations, identified differences in size between nominally identical liposomal samples, and detected the presence of low-diameter material which yielded bimodal particle size distributions. Subsequently, we compared these findings to dynamic light scattering (DLS) data and results from light scattering experiments coupled to Asymmetric Flow-Field Flow Fractionation (AF4), the latter improving the detectability of smaller particles in polydisperse samples due to a size separation step prior detection. However, the bimodal size distribution could not be detected due to method inherent limitations. In contrast, cryo transmission electron microscopy corroborated nES GEMMA results. Hence, gas-phase electrophoresis proved to be a versatile tool for liposome characterization as it could analyze both vesicle size and size distribution. Finally, a correlation of nES GEMMA results with cell viability experiments was carried out to demonstrate the importance of liposome batch-to-batch control as low-sized sample components possibly impact cell viability. Copyright © 2016 The Authors. Published by Elsevier B.V. All rights reserved.

Structure of IgG and IgY molecules in ribosome-antibody complexes as studied by electron microscopy.

PubMed

Noll, F; Lutsch, G; Bielka, H

1982-03-01

The overall shape and dimensions of IgG (rabbit) and IgY (chicken) antibodies against ribosomal proteins have been studied in electron micrographs of ribosome-antibody complexes. The antibodies appear as Y-shaped molecules with an angle of about 90 degrees between their Fab arms. The length of one Fab arm amounts to about 10 nm. No differences between the IgG and IgY molecules could be detected electron microscopically. The data obtained on the shape of IgG and IgY correlate with those of earlier electron microscopic studies while the determined size of the Fab arms is in the range found by scattering methods.

Bio-inspired, colorful, flexible, defrostable light-scattering hybrid films for the effective distribution of LED light.

PubMed

An, Seongpil; Jo, Hong Seok; Kim, Yong Il; Song, Kyo Yong; Kim, Min-Woo; Lee, Kyu Bum; Yarin, Alexander L; Yoon, Sam S

2017-07-06

Bioluminescent jellyfish has a unique structure derived from fiber/polymer interfaces that is advantageous for effective light scattering in the dark, deep sea water. Herein, we demonstrate the fabrication of bio-inspired hybrid films by mimicry of the jellyfish's structure, leading to excellent light-scattering performance and defrosting capability. A haze value reaching 59.3% and a heating temperature of up to 292 °C were achieved with the films. Accordingly, the developed surface constitutes an attractive optical device for lighting applications, especially for street or vehicle luminaries for freezing Arctic-climate countries. The morphological details of the hybrid films were revealed by scanning electron microscopy. The light-scattering properties of these films were examined by ultraviolet-visible-infrared spectrophotometry and anti-glare effect analyses. The defrosting performance of the hybrid films was evaluated via heating tests and infra-red observations.

Dark-field microscopy studies of single metal nanoparticles: understanding the factors that influence the linewidth of the localized surface plasmon resonance.

PubMed

Hu, Min; Novo, Carolina; Funston, Alison; Wang, Haining; Staleva, Hristina; Zou, Shengli; Mulvaney, Paul; Xia, Younan; Hartland, Gregory V

2008-01-01

This article provides a review of our recent Rayleigh scattering measurements on single metal nanoparticles. Two different systems will be discussed in detail: gold nanorods with lengths between 30 and 80 nm, and widths between 8 and 30 nm; and hollow gold-silver nanocubes (termed nanoboxes or nanocages depending on their exact morphology) with edge lengths between 100 and 160 nm, and wall thicknesses of the order of 10 nm. The goal of this work is to understand how the linewidth of the localized surface plasmon resonance depends on the size, shape, and environment of the nanoparticles. Specifically, the relative contributions from bulk dephasing, electron-surface scattering, and radiation damping (energy loss via coupling to the radiation field) have been determined by examining particles with different dimensions. This separation is possible because the magnitude of the radiation damping effect is proportional to the particle volume, whereas, the electron-surface scattering contribution is inversely proportional to the dimensions. For the nanorods, radiation damping is the dominant effect for thick rods (widths greater than 20 nm), while electron-surface scattering is dominant for thin rods (widths less than 10 nm). Rods with widths in between these limits have narrow resonances-approaching the value determined by the bulk contribution. For nanoboxes and nanocages, both radiation damping and electron-surface scattering are significant at all sizes. This is because these materials have thin walls, but large edge lengths and, therefore, relatively large volumes. The effect of the environment on the localized surface plasmon resonance has also been studied for nanoboxes. Increasing the dielectric constant of the surroundings causes a red-shift and an increase in the linewidth of the plasmon band. The increase in linewidth is attributed to enhanced radiation damping.

Imaging electronic motions by ultrafast electron diffraction

NASA Astrophysics Data System (ADS)

Shao, Hua-Chieh; Starace, Anthony F.

2017-08-01

Recently ultrafast electron diffraction and microscopy have reached unprecedented temporal resolution, and transient structures with atomic precision have been observed in various reactions. It is anticipated that these extraordinary advances will soon allow direct observation of electronic motions during chemical reactions. We therefore performed a series of theoretical investigations and simulations to investigate the imaging of electronic motions in atoms and molecules by ultrafast electron diffraction. Three prototypical electronic motions were considered for hydrogen atoms. For the case of a breathing mode, the electron density expands and contracts periodically, and we show that the time-resolved scattering intensities reflect such changes of the charge radius. For the case of a wiggling mode, the electron oscillates from one side of the nucleus to the other, and we show that the diffraction images exhibit asymmetric angular distributions. The last case is a hybrid mode that involves both breathing and wiggling motions. Owing to the demonstrated ability of ultrafast electrons to image these motions, we have proposed to image a coherent population transfer in lithium atoms using currently available femtosecond electron pulses. A frequency-swept laser pulse adiabatically drives the valence electron of a lithium atom from the 2s to 2p orbitals, and a time-delayed electron pulse maps such motion. Our simulations show that the diffraction images reflect this motion both in the scattering intensities and the angular distributions.

Globular bodies: a primary cause of the opacity in senile and diabetic posterior cortical subcapsular cataracts?

PubMed

Creighton, M O; Trevithick, J R; Mousa, G Y; Percy, D H; McKinna, A J; Dyson, C; Maisel, H; Bradley, R

1978-07-01

We examined 9 cataracts from maturity onset diabetics and 4 senile posterior subcapsular cataracts by scanning electron microscopy, transmission electron microscopy, immunofluorescence for crystallin proteins and actin, histochemical methods and x-ray diffraction. The cataractous regions contained spherical globules up to 20 mu in diameter, often in a fibrous matrix. Some were extracellular Morgagnian globules, apparently formed by blebbing from the cell surface; others appeared to have been formed intracellularly. The area of globular degeneration was usually 300 mu deep, but had deeper fusiform extensions. Morphological changes in the cell cytoplasm varied according to their depth in the cataract. Electron microscopy showed intracellular and extracellular globules, many of them were bounded by lipid bilayer membranes. Immunofluorescent staining showed that all the globules contained gamma-crystallin; some contained alpha- and beta-crystallins and actin. All the globules contained higher concentrations of cysteine or cystine than the surrounding lens tissue but they did not react to stains for carbohydrate or calcium. X-ray diffraction studies showed that crystalline calcium salts were absent. Globules and cavities averaged 45% of the total area in cross section. Assuming an area of cataract to be 300 micron thick and that globules 1 mu in diameter scattered, while 2--20 mu in diameter reflected light, we calculated that light passing through such a thickness would be reduced by 65%. Thus the globules could account for most of the opacity of the cataractous area. Presumably the fibrous degeneration of the cells causes enough light scattering to account for the remainder of the reduction. Cataract patients complain of decreased visual acuity, a golden halo around objects, and difficulties when driving while facing oncoming traffic at night. These probably result from light scattering. In our previous experiments, globular bodies containing gamma-crystallin were found in cells grown in tissue culture, and blebs with increased acitn content similar to Morgagnian globules were formed in tissue culture by treating differentiated rat lens cells of stage 2 by cytochalasin D (which impaired microfilament function). These results suggest the possibility of simulating in tissue culture the morphological alterations seen in the cataractous cell.

Enhanced dye-sensitized solar cells performance using anatase TiO2 mesocrystals with the Wulff construction of nearly 100% exposed {101} facets as effective light scattering layer.

PubMed

Zhou, Yu; Wang, Xinyu; Wang, Hai; Song, Yeping; Fang, Liang; Ye, Naiqing; Wang, Linjiang

2014-03-28

Anatase TiO2 mesocrystals with a Wulff construction of nearly 100% exposed {101} facets were successfully synthesized by a facile, green solvothermal method. Their morphology, and crystal structure are characterized by powder X-ray diffraction (XRD), Field emission scanning electron microscopy (FESEM) and high-resolution transmission electron microscopy (HRTEM). Accordingly, a possible growth mechanism of anatase TiO2 mesocrystals is elucidated in this work. The as-prepared single anatase TiO2 mesocrystal's mean center diameter is about 500 nm, and the length is about 1 μm. They exhibit high light adsorbance, high reflectance and low transmittance in the visible region due to the unique nearly 100% exposed {101} facets. When utilized as the scattering layer in dye-sensitized solar cells (DSSCs), such mesocrystals effectively enhanced light harvesting and led to an increase of the photocurrent of the DSSCs. As a result, by using an anatase TiO2 mesocrystal film as a scattering overlayer of a compact commercial P25 TiO2 nanoparticle film, the double layered DSSCs show a power conversion efficiency of 7.23%, indicating a great improvement compared to the DSSCs based on a P25 film (5.39%) and anatase TiO2 mesocrystal films, respectively. The synergetic effect of P25 and the mesocrystals as well as the latters unique feature of a Wulff construction of nearly 100% exposed (101) facets are probably responsible for the enhanced photoelectrical performance. In particular, we explore the possibility of the low surface area and exposed {101} facets as an efficient light scattering layer of DSSCs. Our work suggests that anatase TiO2 mesocrystals with the Wulff construction is a promising candidate as a superior scattering material for high-performance DSSCs.

Conductive scanning probe microscopy of the semicontinuous gold film and its SERS enhancement toward two-step photo-induced charge transfer and effect of the supportive layer

NASA Astrophysics Data System (ADS)

Sinthiptharakoon, K.; Sapcharoenkun, C.; Nuntawong, N.; Duong, B.; Wutikhun, T.; Treetong, A.; Meemuk, B.; Kasamechonchung, P.; Klamchuen, A.

2018-05-01

The semicontinuous gold film, enabling various electronic applications including development of surface-enhanced Raman scattering (SERS) substrate, is investigated using conductive atomic force microscopy (CAFM) and Kelvin probe force microscopy (KPFM) to reveal and investigate local electronic characteristics potentially associated with SERS generation of the film material. Although the gold film fully covers the underlying silicon surface, CAFM results reveal that local conductivity of the film is not continuous with insulating nanoislands appearing throughout the surface due to incomplete film percolation. Our analysis also suggests the two-step photo-induced charge transfer (CT) play the dominant role in the enhancement of SERS intensity with strong contribution from free electrons of the silicon support. Silicon-to-gold charge transport is illustrated by KPFM results showing that Fermi level of the gold film is slightly inhomogeneous and far below the silicon conduction band. We propose that inhomogeneity of the film workfunction affecting chemical charge transfer between gold and Raman probe molecule is associated with the SERS intensity varying across the surface. These findings provide deeper understanding of charge transfer mechanism for SERS which can help in design and development of the semicontinuous gold film-based SERS substrate and other electronic applications.

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.

Characterizing string-of-pearls colloidal silica by multidetector hydrodynamic chromatography and comparison to multidetector size-exclusion chromatography, off-line multiangle static light scattering, and transmission electron microscopy.

PubMed

Brewer, Amandaa K; Striegel, André M

2011-04-15

The string-of-pearls-type morphology is ubiquitous, manifesting itself variously in proteins, vesicles, bacteria, synthetic polymers, and biopolymers. Characterizing the size and shape of analytes with such morphology, however, presents a challenge, due chiefly to the ease with which the "strings" can be broken during chromatographic analysis or to the paucity of information obtained from the benchmark microscopy and off-line light scattering methods. Here, we address this challenge with multidetector hydrodynamic chromatography (HDC), which has the ability to determine, simultaneously, the size, shape, and compactness and their distributions of string-of-pearls samples. We present the quadruple-detector HDC analysis of colloidal string-of-pearls silica, employing static multiangle and quasielastic light scattering, differential viscometry, and differential refractometry as detection methods. The multidetector approach shows a sample that is broadly polydisperse in both molar mass and size, with strings ranging from two to five particles, but which also contains a high concentration of single, unattached "pearls". Synergistic combination of the various size parameters obtained from the multiplicity of detectors employed shows that the strings with higher degrees of polymerization have a shape similar to the theory-predicted shape of a Gaussian random coil chain of nonoverlapping beads, while the strings with lower degrees of polymerization have a prolate ellipsoidal shape. The HDC technique is contrasted experimentally with multidetector size-exclusion chromatography, where, even under extremely gentle conditions, the strings still degraded during analysis. Such degradation is shown to be absent in HDC, as evidenced by the fact that the molar mass and radius of gyration obtained by HDC with multiangle static light scattering detection (HDC/MALS) compare quite favorably to those determined by off-line MALS analysis under otherwise identical conditions. The multidetector HDC results were also comparable to those obtained by transmission electron microscopy (TEM). Unlike off-line MALS or TEM, however, multidetector HDC is able to provide complete particle analysis based on the molar mass, size, shape, and compactness and their distributions for the entire sample population in less than 20 min. © 2011 American Chemical Society

Optimal synthesis and characterization of Ag nanofluids by electrical explosion of wires in liquids

PubMed Central

2011-01-01

Silver nanoparticles were produced by electrical explosion of wires in liquids with no additive. In this study, we optimized the fabrication method and examined the effects of manufacturing process parameters. Morphology and size of the Ag nanoparticles were determined using transmission electron microscopy and field-emission scanning electron microscopy. Size and zeta potential were analyzed using dynamic light scattering. A response optimization technique showed that optimal conditions were achieved when capacitance was 30 μF, wire length was 38 mm, liquid volume was 500 mL, and the liquid type was deionized water. The average Ag nanoparticle size in water was 118.9 nm and the zeta potential was -42.5 mV. The critical heat flux of the 0.001-vol.% Ag nanofluid was higher than pure water. PMID:21711757

Effect of in situ Al doping on structure and optical properties of ZnO nanowires grown by MOCVD

NASA Astrophysics Data System (ADS)

Souissi, H.; Jabri, S.; Souissi, A.; Lusson, A.; Galtier, P.; Meftah, A.; Sallet, V.; Oueslati, M.

2018-01-01

Al-doped ZnO nanowires (NWs) were grown on C-axis oriented sapphire by metal organic chemical vapor deposition using dimethylzinc-triethylamine (DMZn-TEN), nitrogen dioxide (NO2) and TMAl as zinc, oxygen and aluminum doping sources respectively. The NWs morphology has been characterized by scanning electron microscopy and transmission electron microscopy. The photoluminescence (PL) spectra exhibit a strong excitonic transition bond that confirms the Al incorporation in the ZnO NWs. Raman results support PL conclusion by showing additional modes in Al-doped ZnO NWs at nearly 270, 510, 579 and 641 cm-1. The micro-Raman scattering analysis along a single Al-doped ZnO needle-like NW shows an increase of the Al concentration from the basis to the tip of the wire.

Plastic protein microarray to investigate the molecular pathways of magnetic nanoparticle-induced nanotoxicity

NASA Astrophysics Data System (ADS)

Liu, Yingshuai; Li, Xuelian; Bao, Shujuan; Lu, Zhisong; Li, Qing; Li, Chang Ming

2013-05-01

Superparamagnetic iron oxide nanoparticles (SPIONs) (about 15 nm) were synthesized via a hydrothermal method and characterized by field emission scanning electron microscopy, transmission electron microscopy, dynamic light scattering, x-ray diffraction, and vibrating sample magnetometer. The molecular pathways of SPIONs-induced nanotoxicity was further investigated by protein microarrays on a plastic substrate from evaluation of cell viability, reactive oxygen species (ROS) generation and cell apoptosis. The experimental results reveal that 50 μg ml-1 or higher levels of SPIONs cause significant loss of cell viability, considerable generation of ROS and cell apoptosis. It is proposed that high level SPIONs could induce cell apoptosis via a mitochondria-mediated intrinsic pathway by activation of caspase 9 and caspase 3, an increase of the Bax/Bcl-2 ratio, and down-regulation of HSP70 and HSP90 survivor factors.

Possible superconductivity in Sr2IrO4 probed by quasiparticle interference

PubMed Central

Gao, Yi; Zhou, Tao; Huang, Huaixiang; Wang, Qiang-Hua

2015-01-01

Based on the possible superconducting (SC) pairing symmetries recently proposed, the quasiparticle interference (QPI) patterns in electron- and hole-doped Sr2IrO4 are theoretically investigated. In the electron-doped case, the QPI spectra can be explained based on a model similar to the octet model of the cuprates while in the hole-doped case, both the Fermi surface topology and the sign of the SC order parameter resemble those of the iron pnictides and there exists a QPI vector resulting from the interpocket scattering between the electron and hole pockets. In both cases, the evolution of the QPI vectors with energy and their behaviors in the nonmagnetic and magnetic impurity scattering cases can well be explained based on the evolution of the constant-energy contours and the sign structure of the SC order parameter. The QPI spectra presented in this paper can be compared with future scanning tunneling microscopy experiments to test whether there are SC phases in electron- and hole-doped Sr2IrO4 and what the pairing symmetry is. PMID:25783417

Spectral analysis of scattered light from flowers' petals

NASA Astrophysics Data System (ADS)

Ozawa, Atsumi; Uehara, Tomomi; Sekiguchi, Fumihiko; Imai, Hajime

2009-07-01

A new method was developed for studying absorption characteristics of opaque samples based on the light scattering spectroscopy. Measurements were made in white, red and violet petals of Petunia hybrida, and gave the absorption spectra in a non-destructive manner without damaging the cell structures of the petal. The red petal has absorption peak at 550 nm and the violet has three absorption peaks: at 450, 670, and 550 nm. The results were discussed in correlation with the microscopic cell structures of the petal observed with optical microscope and transmission electron microscopy (TEM). Only the cells placed in the surface have the pigments giving the color of the petal.

Atomic Structure of Au 329(SR) 84 Faradaurate Plasmonic Nanomolecules

DOE PAGES

Kumara, Chanaka; Zuo, Xiaobing; Ilavsky, Jan; ...

2015-04-03

To design novel nanomaterials, it is important to precisely control the composition, determine the atomic structure, and manipulate the structure to tune the materials property. Here we present a comprehensive characterization of the material whose composition is Au 329(SR) 84 precisely, therefore referred to as a nanomolecule. The size homogeneity was shown by electron microscopy, solution X-ray scattering, and mass spectrometry. We proposed its atomic structure to contain the Au 260 core using experiments and modeling of a total-scattering-based atomic-pair distribution functional analysis. HAADF-STEM images shows fcc-like 2.0 ± 0.1 nm diameter nanomolecules.

Environmental transmission electron microscopy for catalyst materials using a spherical aberration corrector.

PubMed

Takeda, Seiji; Kuwauchi, Yasufumi; Yoshida, Hideto

2015-04-01

Atomic resolution has been obtained using environmental transmission electron microscopy (ETEM) by installing a spherical aberration corrector (Cs-corrector) on the objective lens. Simultaneously, the technology for controlling the environment around a specimen in ETEM has advanced significantly in the past decade. Quantification methodology has recently been established for deriving relevant experimental data in catalyst materials from substantial and systematic ETEM observation at the atomic scale. With this background, this paper summarizes aspects of the evolutional microscopy technique: necessary conditions for atomic resolution in ETEM; reduction of the scattering of electrons by the medium surrounding a specimen; and an environmental cell for structural imaging of a crystalline specimen. The high spatial resolution of a Cs-corrected ETEM is demonstrated for different observation conditions. After statistical analysis combined with numerical image analysis of ETEM data is briefly described, the recent applications of the Cs-corrected ETEM to catalyst materials are reviewed. For gold nanoparticulate catalysts, the structural information on the reaction sites and adsorption sites are deduced. For Pt nanoparticulate catalysts, ETEM studies elucidate the correlation between the catalytic activity and the morphology of the nanoparticles. These studies also reveal oxidation and reduction on the topmost Pt surface layer at the atomic scale. Finally, current issues and the future perspectives of Cs-corrected ETEM are summarized, including the reproducibility of ETEM observation data, the control of environments, the critical evaluation of electron irradiation effects, the full implementation of transmission electron microscopy technology in ETEM, and the safety issues for an ETEM laboratory. Copyright © 2014 Elsevier B.V. All rights reserved.

Investigation and Control of "Sphere-Like" Buckminsterfullerene C60 and "Disk-Like" Copper(II) Phthalocyanine

NASA Astrophysics Data System (ADS)

McAfee, Terry Richard

Due to the growing global need for cheap, flexible, and portable electronics, numerous research groups from mechanical and electrical engineering, material science, chemistry, and physics have increasingly turned to organic electronics research over the last ˜5--10 years. Largely, the focus of researchers in this growing field have sought to obtain the next record holding device, allowing a heuristic approach of trial and error to become dominant focus of research rather than a fundamental understanding. Rather than working with the latest high performance organic semiconducting materials and film processing techniques, I have chosen to investigate and control the fundamental self-assembly interactions of organic photovoltaic thin films using simplified systems. Specifically, I focus on organic photovoltaic research using two of the oldest and well studies semiconducting materials, namely "sphere-like" electron donor material Buckminsterfullerene C60 and "disklike" electron acceptor material Copper(II) Phthalocyanine. I manufactured samples using the well-known technique of physical vapor deposition using a high vacuum chamber that I designed and built to accommodate my need of precise material deposition control, with codeposition capability. Films were characterized using microscopy and spectroscopy techniques locally at NCSU, including Atomic Force Microscopy, scanning tunneling microscopy, X-ray photoelectron spectroscopy, and Ultraviolet-visible spectroscopy, as well as at National Laboratory based synchrotron x-ray techniques, including Carbon and Nitrogen k-edge Total Electron Yield and Transmission Near Edge X-ray absorption fine structure spectroscopy, Carbon k-edge Resonant Soft x-ray Microscopy, Resonant Soft x-ray reflectivity, and Grazing Incidence Wide-Angle X-ray scattering.

Scatter sensitive microscopic techniques to identify contrasting mucosal structures in ultrahigh-resolution optical coherence tomograms of mouse colon

NASA Astrophysics Data System (ADS)

Tumlinson, Alexandre R.; Hariri, Lida P.; Drexler, Wolfgang; Barton, Jennifer K.

2008-02-01

Optical coherence tomography, optical coherence microscopy, reflectance confocal microscopy, and darkfield microscopy all derive contrast from the intensity of endogenous tissue scatter. We have imaged excised mouse colon tissue with these complimentary technologies to make conclusions about structural origins of scatter in the mouse colonic mucosa observed with endoscopic OCT. We find hyperintense scattering both from the cytoplasm of epithelial cells and from the boundary between epithelia and the lamina propria. We find almost no scatter from the portion of epithelial cells containing the nucleus. These observations substantiate explanations for the appearance of colonic crypts and the luminal surface.

Mega-electron-volt ultrafast electron diffraction at SLAC National Accelerator Laboratory

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

Weathersby, S. P.; Brown, G.; Chase, T. F.

Ultrafast electron probes are powerful tools, complementary to x-ray free-electron lasers, used to study structural dynamics in material, chemical, and biological sciences. High brightness, relativistic electron beams with femtosecond pulse duration can resolve details of the dynamic processes on atomic time and length scales. SLAC National Accelerator Laboratory recently launched the Ultrafast Electron Diffraction (UED) and microscopy Initiative aiming at developing the next generation ultrafast electron scattering instruments. As the first stage of the Initiative, a mega-electron-volt (MeV) UED system has been constructed and commissioned to serve ultrafast science experiments and instrumentation development. The system operates at 120-Hz repetition ratemore » with outstanding performance. In this paper, we report on the SLAC MeV UED system and its performance, including the reciprocal space resolution, temporal resolution, and machine stability.« less

Mega-electron-volt ultrafast electron diffraction at SLAC National Accelerator Laboratory.

PubMed

Weathersby, S P; Brown, G; Centurion, M; Chase, T F; Coffee, R; Corbett, J; Eichner, J P; Frisch, J C; Fry, A R; Gühr, M; Hartmann, N; Hast, C; Hettel, R; Jobe, R K; Jongewaard, E N; Lewandowski, J R; Li, R K; Lindenberg, A M; Makasyuk, I; May, J E; McCormick, D; Nguyen, M N; Reid, A H; Shen, X; Sokolowski-Tinten, K; Vecchione, T; Vetter, S L; Wu, J; Yang, J; Dürr, H A; Wang, X J

2015-07-01

Ultrafast electron probes are powerful tools, complementary to x-ray free-electron lasers, used to study structural dynamics in material, chemical, and biological sciences. High brightness, relativistic electron beams with femtosecond pulse duration can resolve details of the dynamic processes on atomic time and length scales. SLAC National Accelerator Laboratory recently launched the Ultrafast Electron Diffraction (UED) and microscopy Initiative aiming at developing the next generation ultrafast electron scattering instruments. As the first stage of the Initiative, a mega-electron-volt (MeV) UED system has been constructed and commissioned to serve ultrafast science experiments and instrumentation development. The system operates at 120-Hz repetition rate with outstanding performance. In this paper, we report on the SLAC MeV UED system and its performance, including the reciprocal space resolution, temporal resolution, and machine stability.

Thermoelectric properties of Co₄Sb₁₂ with Bi₂Te₃ nanoinclusions.

PubMed

Ghosh, Sanyukta; Bisht, Anuj; Karati, Anirudha; Rogl, Gerda; Rogl, Peter F; Murty, B S; Suwas, Satyam; Mallik, Ramesh Chandra

2018-01-08

The figure of merit (zT) of a thermoelectric material can be enhanced by incorporation of nanoinclusions into bulk material. The presence of bismuth telluride (Bi2Te3) nanoinclusions in Co4Sb12 leads to lower phonon thermal conductivity by introducing interfaces and defects; it enhances the average zT between 300-700 K. In the current study, Bi2Te3 nanoparticles were dispersed into bulk Co4Sb12 by ball-milling. The bulk was fabricated by spark plasma sintering (SPS). The presence of Bi2Te3 dispersion in Co4Sb12 was confirmed by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and electron back scattered diffraction (EBSD) technique. Energy dispersive spectroscopy (EDS) showed antimony (Sb) as an impurity phase for higher contents of Bi2Te3 in the sample. The Seebeck coefficient (S) and electrical conductivity () were measured in the temperature range of 350 - 673 K. The negative value of S indicates that most of the charge carriers were electrons. A decrease in S and increase in with Bi2Te3 content are due to the increased carrier concentration, as confirmed by Hall measurement. The thermal conductivity, measured between 423 - 673 K, decreased due to the increased phonon scattering at interfaces. A maximum zT of 0.17 was achieved at 523 K and it did not vary much throughout the temperature range. The experimental results of composites were compared by using effective medium theories. © 2018 IOP Publishing Ltd.

Wide-field imaging through scattering media by scattered light fluorescence microscopy

NASA Astrophysics Data System (ADS)

Zhou, Yulan; Li, Xun

2017-08-01

To obtain images through scattering media, scattered light fluorescence (SLF) microscopy that utilizes the optical memory effect has been developed. However, the small field of view (FOV) of SLF microscopy limits its application. In this paper, we have introduced a re-modulation method to achieve wide-field imaging through scattering media by SLF microscopy. In the re-modulation method, to raster scan the focus across the object plane, the incident wavefront is re-modulated via a spatial light modulator (SLM) in the updated phase compensation calculated using the optimized iterative algorithm. Compared with the conventional optical memory effect method, the re-modulation method can greatly increase the FOV of a SLF microscope. With the phase compensation theoretically calculated, the process of updating the phase compensation of a high speed SLM is fast. The re-modulation method does not increase the imaging time. The re-modulation method is, therefore, expected to make SLF microscopy have much wider applications in biology, medicine and physiology.

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.

Investigating fold structures of 2D materials by quantitative transmission electron microscopy.

PubMed

Wang, Zhiwei; Zhang, Zengming; Liu, Wei; Wang, Zhong Lin

2017-04-01

We report an approach developed for deriving 3D structural information of 2D membrane folds based on the recently-established quantitative transmission electron microscopy (TEM) in combination with density functional theory (DFT) calculations. Systematic multislice simulations reveal that the membrane folding leads to sufficiently strong electron scattering which enables a precise determination of bending radius. The image contrast depends also on the folding angles of 2D materials due to the variation of projection potentials, which however exerts much smaller effect compared with the bending radii. DFT calculations show that folded edges are typically characteristic of (fractional) nanotubes with the same curvature retained after energy optimization. Owing to the exclusion of Stobbs factor issue, numerical simulations were directly used in comparison with the experimental measurements on an absolute contrast scale, which results in a successful determination of bending radius of folded monolayer MoS 2 films. The method should be applicable to characterizing all 2D membranes with 3D folding features. Copyright © 2017 Elsevier Ltd. All rights reserved.

The Effect of Ultrafine-Grained Microstructure on Creep Behaviour of 9% Cr Steel

PubMed Central

Kral, Petr; Dvorak, Jiri; Sklenicka, Vaclav; Masuda, Takahiro; Horita, Zenji; Kucharova, Kveta; Kvapilova, Marie; Svobodova, Marie

2018-01-01

The effect of ultrafine-grained size on creep behaviour was investigated in P92 steel. Ultrafine-grained steel was prepared by one revolution of high-pressure torsion at room temperature. Creep tensile tests were performed at 873 K under the initially-applied stress range between 50 and 160 MPa. The microstructure was investigated using transmission electron microscopy and scanning electron microscopy equipped with an electron-back scatter detector. It was found that ultrafine-grained steel exhibits significantly faster minimum creep rates, and there was a decrease in the value of the stress exponent in comparison with coarse-grained P92 steel. Creep results also showed an abrupt decrease in the creep rate over time during the primary stage. The abrupt deceleration of the creep rate during the primary stage was shifted, with decreasing applied stress with longer creep times. The change in the decline of the creep rate during the primary stage was probably related to the enhanced precipitation of the Laves phase in the ultrafine-grained microstructure. PMID:29757206

In situ Scanning Electron Microscopy of Silicon Anode Reactions in Lithium-Ion Batteries during Charge/Discharge Processes

PubMed Central

Chen, Chih-Yao; Sano, Teruki; Tsuda, Tetsuya; Ui, Koichi; Oshima, Yoshifumi; Yamagata, Masaki; Ishikawa, Masashi; Haruta, Masakazu; Doi, Takayuki; Inaba, Minoru; Kuwabata, Susumu

2016-01-01

A comprehensive understanding of the charge/discharge behaviour of high-capacity anode active materials, e.g., Si and Li, is essential for the design and development of next-generation high-performance Li-based batteries. Here, we demonstrate the in situ scanning electron microscopy (in situ SEM) of Si anodes in a configuration analogous to actual lithium-ion batteries (LIBs) with an ionic liquid (IL) that is expected to be a functional LIB electrolyte in the future. We discovered that variations in the morphology of Si active materials during charge/discharge processes is strongly dependent on their size and shape. Even the diffusion of atomic Li into Si materials can be visualized using a back-scattering electron imaging technique. The electrode reactions were successfully recorded as video clips. This in situ SEM technique can simultaneously provide useful data on, for example, morphological variations and elemental distributions, as well as electrochemical data. PMID:27782200

Degradation of Methylammonium Lead Iodide Perovskite Structures through Light and Electron Beam Driven Ion Migration

PubMed Central

2016-01-01

Organometal halide perovskites show promising features for cost-effective application in photovoltaics. The material instability remains a major obstacle to broad application because of the poorly understood degradation pathways. Here, we apply simultaneous luminescence and electron microscopy on perovskites for the first time, allowing us to monitor in situ morphology evolution and optical properties upon perovskite degradation. Interestingly, morphology, photoluminescence (PL), and cathodoluminescence of perovskite samples evolve differently upon degradation driven by electron beam (e-beam) or by light. A transversal electric current generated by a scanning electron beam leads to dramatic changes in PL and tunes the energy band gaps continuously alongside film thinning. In contrast, light-induced degradation results in material decomposition to scattered particles and shows little PL spectral shifts. The differences in degradation can be ascribed to different electric currents that drive ion migration. Moreover, solution-processed perovskite cuboids show heterogeneity in stability which is likely related to crystallinity and morphology. Our results reveal the essential role of ion migration in perovskite degradation and provide potential avenues to rationally enhance the stability of perovskite materials by reducing ion migration while improving morphology and crystallinity. It is worth noting that even moderate e-beam currents (86 pA) and acceleration voltages (10 kV) readily induce significant perovskite degradation and alter their optical properties. Therefore, attention has to be paid while characterizing such materials using scanning electron microscopy or transmission electron microscopy techniques. PMID:26804213

Controlling self-assembly of diphenylalanine peptides at high pH using heterocyclic capping groups.

PubMed

Martin, Adam D; Wojciechowski, Jonathan P; Robinson, Andrew B; Heu, Celine; Garvey, Christopher J; Ratcliffe, Julian; Waddington, Lynne J; Gardiner, James; Thordarson, Pall

2017-03-08

Using small angle neutron scattering (SANS), it is shown that the existence of pre-assembled structures at high pH for a capped diphenylalanine hydrogel is controlled by the selection of N-terminal heterocyclic capping group, namely indole or carbazole. At high pH, changing from a somewhat hydrophilic indole capping group to a more hydrophobic carbazole capping group results in a shift from a high proportion of monomers to self-assembled fibers or wormlike micelles. The presence of these different self-assembled structures at high pH is confirmed through NMR and circular dichroism spectroscopy, scanning probe microscopy and cryogenic transmission electron microscopy.

Benefits and Limitations of Low-kV Macromolecular Imaging of Frozen-Hydrated Biological Samples

PubMed Central

Majorovits, Endre; Angert, Isabel; Kaiser, Ute; Schröder, Rasmus R.

2016-01-01

Object contrast is one of the most important parameters of macromolecular imaging. Low-voltage transmission electron microscopy has shown an increased atom contrast for carbon materials, indicating that amplitude contrast contributions increase at a higher rate than phase contrast and inelastic scattering. Here, we studied image contrast using ice-embedded tobacco mosaic virus particles as test samples at 20–80 keV electron energy. The particles showed the expected increase in contrast for lower energies, but at the same time the 2.3-nm-resolution measure decayed more rapidly. We found a pronounced signal loss below 60 keV, and therefore we conclude that increased inelastic scattering counteracts increased amplitude contrast. This model also implies that as long as the amplitude contrast does not increase with resolution, beam damage and multiple scattering will always win over increased contrast at the lowest energies. Therefore, we cannot expect that low-energy imaging of conventionally prepared samples would provide better data than state-of-the-art 200–300 keV imaging. PMID:26910420

Structural and optical properties of GaxIn1-xP layers grown by chemical beam epitaxy

NASA Astrophysics Data System (ADS)

Seong, Tae-Yeon; Yang, Jung-Ja; Ryu, Mee Yi; Song, Jong-In; Yu, Phil W.

1998-05-01

Chemical beam epitaxial (CBE) GaxIn1-xP layers (x≈0.5) grown on (001) GaAs substrates at temperatures ranging from 490 to 580°C have been investigated using transmission electron diffraction (TED), transmission electron microscopy, and photoluminescence (PL). TED examination revealed the presence of diffuse scattering 1/2{111}B positions, indicating the occurrence of typical CuPt-type ordering in the GaInP CBE layers. As the growth temperature decreased from 580 to 490°C, maxima in the intensity of the diffuse scattering moved from ½{111}B to ½{-1+δ,1-δ,0} positions, where δ is a positive value. As the growth temperature increased from 490 to 550°C, the maxima in the diffuse scattering intensity progressively approached positions of 1/2\\{bar 110\\} , i.e., the value of δ decreased from 0.25 to 0.17. Bandgap reduction (˜45 meV) was observed in the CBE GaInP layers and was attributed to the presence of ordered structures.

STM on Gate-Tunable Graphene

NASA Astrophysics Data System (ADS)

Zhang, Yuanbo

2009-03-01

We have successfully performed atomically-resolved scanning tunneling microscopy and spectroscopy (STS) on mechanically exfoliated graphene samples having tunable back-gates. We have discovered that the tunneling spectra of graphene flakes display an unexpected gap-like feature that is pinned to the Fermi level for different gate voltages, and which coexists with another depression in density-of-states that moves with gate voltage. Extensive tests and careful analysis show that the gap-feature is due to phonon-assisted inelastic tunneling, and the depression directly marks the location of the graphene Dirac point. Using tunneling spectroscopy as a new tool, we further probe the local energetic variations of the graphene charge neutral point (Dirac point) to map out spatial electron density inhomogeneities in graphene. Such measurements are two orders of magnitude higher in resolution than previous experiments, and they can be directly correlated with nanometer scale topographic features. Based on our observation of energy-dependent periodic electronic interference patterns, our measurements also reveal the nature of impurity scattering of Dirac fermions in graphene. These results are significant for understanding the sources of electron density inhomogeneity and electron scattering in graphene, and the microscopic causes of graphene electron mobility.

Application of SEM and EDX in studying biomineralization in plant tissues.

PubMed

He, Honghua; Kirilak, Yaowanuj

2014-01-01

This chapter describes protocols using formalin-acetic acid-alcohol (FAA) to fix plant tissues for studying biomineralization by means of scanning electron microscopy (SEM) and qualitative energy-dispersive X-ray microanalysis (EDX). Specimen preparation protocols for SEM and EDX mainly include fixation, dehydration, critical point drying (CPD), mounting, and coating. Gold-coated specimens are used for SEM imaging, while gold- and carbon-coated specimens are prepared for qualitative X-ray microanalyses separately to obtain complementary information on the elemental compositions of biominerals. During the specimen preparation procedure for SEM, some biominerals may be dislodged or scattered, making it difficult to determine their accurate locations, and light microscopy is used to complement SEM studies. Specimen preparation protocols for light microscopy generally include fixation, dehydration, infiltration and embedding with resin, microtome sectioning, and staining. In addition, microwave processing methods are adopted here to speed up the specimen preparation process for both SEM and light microscopy.

High-sensitivity chemical imaging for biomedicine by SRS microscopy (Conference Presentation)

NASA Astrophysics Data System (ADS)

Min, Wei

2017-02-01

Innovations in spectroscopy principles and microscopy technology have significantly impacted modern biology and medicine. While most of the contemporary bio-imaging modalities harness electronic transition, nuclear spin or radioactivity, vibrational spectroscopy has not been widely used yet. Here we will discuss an emerging chemical imaging platform, stimulated Raman scattering (SRS) microscopy, which can enhance the otherwise feeble spontaneous Raman eight orders of magnitude by virtue of stimulated emission. When coupled with stable isotopes (e.g., deuterium and 13C) or bioorthogonal chemical moieties (e.g., alkynes), SRS microscopy is well suited for probing in vivo metabolic dynamics of small bio-molecules which cannot be labeled by bulky fluorophores. Physical principle of the underlying optical spectroscopy and exciting biomedical applications such as imaging lipid metabolism, protein synthesis, DNA replication, protein degradation, RNA synthesis, glucose uptake, drug trafficking and tumor metabolism will be presented.

Data mining graphene: Correlative analysis of structure and electronic degrees of freedom in graphenic monolayers with defects

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

Ziatdinov, Maxim A.; Fujii, Shintaro; Kiguchi, Manabu

The link between changes in the material crystal structure and its mechanical, electronic, magnetic, and optical functionalities known as the structure-property relationship is the cornerstone of the contemporary materials science research. The recent advances in scanning transmission electron and scanning probe microscopies (STEM and SPM) have opened an unprecedented path towards examining the materials structure property relationships on the single-impurity and atomic-configuration levels. Lacking, however, are the statistics-based approaches for cross-correlation of structure and property variables obtained in different information channels of the STEM and SPM experiments. Here we have designed an approach based on a combination of sliding windowmore » Fast Fourier Transform, Pearson correlation matrix, linear and kernel canonical correlation, to study a relationship between lattice distortions and electron scattering from the SPM data on graphene with defects. Our analysis revealed that the strength of coupling to strain is altered between different scattering channels which can explain coexistence of several quasiparticle interference patterns in the nanoscale regions of interest. In addition, the application of the kernel functions allowed us extracting a non-linear component of the relationship between the lattice strain and scattering intensity in graphene. Lastly, the outlined approach can be further utilized to analyzing correlations in various multi-modal imaging techniques where the information of interest is spatially distributed and has usually a complex multidimensional nature.« less

Data mining graphene: Correlative analysis of structure and electronic degrees of freedom in graphenic monolayers with defects

DOE PAGES

Ziatdinov, Maxim A.; Fujii, Shintaro; Kiguchi, Manabu; ...

2016-11-09

The link between changes in the material crystal structure and its mechanical, electronic, magnetic, and optical functionalities known as the structure-property relationship is the cornerstone of the contemporary materials science research. The recent advances in scanning transmission electron and scanning probe microscopies (STEM and SPM) have opened an unprecedented path towards examining the materials structure property relationships on the single-impurity and atomic-configuration levels. Lacking, however, are the statistics-based approaches for cross-correlation of structure and property variables obtained in different information channels of the STEM and SPM experiments. Here we have designed an approach based on a combination of sliding windowmore » Fast Fourier Transform, Pearson correlation matrix, linear and kernel canonical correlation, to study a relationship between lattice distortions and electron scattering from the SPM data on graphene with defects. Our analysis revealed that the strength of coupling to strain is altered between different scattering channels which can explain coexistence of several quasiparticle interference patterns in the nanoscale regions of interest. In addition, the application of the kernel functions allowed us extracting a non-linear component of the relationship between the lattice strain and scattering intensity in graphene. Lastly, the outlined approach can be further utilized to analyzing correlations in various multi-modal imaging techniques where the information of interest is spatially distributed and has usually a complex multidimensional nature.« less

Electronic Phase Separation in the Slightly Underdoped Iron Pnictide Superconductor Ba{sub 1-x}K{sub x}Fe{sub 2}As{sub 2}

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

Park, J. T.; Inosov, D. S.; Sun, G. L.

2009-03-20

Here we present a combined study of the slightly underdoped novel pnictide superconductor Ba{sub 1-x}K{sub x}Fe{sub 2}As{sub 2} by means of x-ray powder diffraction, neutron scattering, muon-spin rotation ({mu}SR), and magnetic force microscopy (MFM). Static antiferromagnetic order sets in below T{sub m}{approx_equal}70 K as inferred from the neutron scattering and zero-field-{mu}SR data. Transverse-field {mu}SR below T{sub c} shows a coexistence of magnetically ordered and nonmagnetic states, which is also confirmed by MFM imaging. We explain such coexistence by electronic phase separation into antiferromagnetic and superconducting- or normal-state regions on a lateral scale of several tens of nanometers. Our findings indicatemore » that such mesoscopic phase separation can be considered an intrinsic property of some iron pnictide superconductors.« less

Differences in Physical and Biochemical Properties of Thermus scotoductus SA-01 Cultured with Dielectric or Convection Heating.

PubMed

Cockrell, Allison L; Fitzgerald, Lisa A; Cusick, Kathleen D; Barlow, Daniel E; Tsoi, Stanislav D; Soto, Carissa M; Baldwin, Jeffrey W; Dale, Jason R; Morris, Robert E; Little, Brenda J; Biffinger, Justin C

2015-09-01

A thermophile, Thermus scotoductus SA-01, was cultured within a constant-temperature (65°C) microwave (MW) digester to determine if MW-specific effects influenced the growth and physiology of the organism. As a control, T. scotoductus cells were also cultured using convection heating at the same temperature as the MW studies. Cell growth was analyzed by optical density (OD) measurements, and cell morphologies were characterized using electron microscopy imaging (scanning electron microscopy [SEM] and transmission electron microscopy [TEM]), dynamic light scattering (DLS), and atomic force microscopy (AFM). Biophysical properties (i.e., turgor pressure) were also calculated with AFM, and biochemical compositions (i.e., proteins, nucleic acids, fatty acids) were analyzed by attenuated total reflectance-Fourier transform infrared (ATR-FTIR) spectroscopy. Gas chromatography-mass spectrometry (GC-MS) was used to analyze the fatty acid methyl esters extracted from cell membranes. Here we report successful cultivation of a thermophile with only dielectric heating. Under the MW conditions for growth, cell walls remained intact and there were no indications of membrane damage or cell leakage. Results from these studies also demonstrated that T. scotoductus cells grown with MW heating exhibited accelerated growth rates in addition to altered cell morphologies and biochemical compositions compared with oven-grown cells. Copyright © 2015, American Society for Microbiology. All Rights Reserved.

Creation and study of triterpenoid nanoparticles and radioprotective substance genistein.

PubMed

Nguyen, H Q; Chupin, V V; Prokhorov, D I; Chikunov, I E; Kovtun, V Yu; Tarumov, R A; Grebenyuk, A N; Shvets, V I

2015-01-01

This work is devoted to the study and obtaining of new radioprotective agents based on natural flavonoid genistein and spherical amorphous nanoparticles (SANPs) produced from a mixture of birch bark triterpenoids. The physicochemical characteristics of the nanoparticles were studied by electron microscopy, dynamic light scattering, and UV-VIS spectroscopy. The radioprotective efficacy of the nanodrug in vivo and the possibility of its use as a radioprotective agent was shown.

Comparative study of the magnetic properties of La3Ni2B‧O9 for B‧ = Nb, Taor Sb

NASA Astrophysics Data System (ADS)

Chin, Chun-Mann; Battle, Peter D.; Blundell, Stephen J.; Hunter, Emily; Lang, Franz; Hendrickx, Mylène; Paria Sena, Robert; Hadermann, Joke

2018-02-01

Polycrystalline samples of La3Ni2NbO9 and La3Ni2TaO9 have been characterised by X-ray and neutron diffraction, electron microscopy, magnetometry and muon spin relaxation (μSR); the latter technique was also applied to La3Ni2SbO9. On the length scale of a neutron diffraction experiment, the six-coordinate sites of the monoclinic perovskite structure are occupied in a 1:1 ordered manner by Ni and a random ⅓Ni/⅔B‧ mixture. Electron microscopy demonstrated that this 1:1 ordering is maintained over microscopic distances, although diffuse scattering indicative of short-range ordering on the mixed site was observed. No magnetic Bragg scattering was observed in neutron diffraction patterns collected from La3Ni2B‧O9 (B‧ = Nb or Ta) at 5 K although in each case μSR identified the presence of static spins below 30 K. Magnetometry showed that La3Ni2NbO9 behaves as a spin glass below 29 K but significant short-range interactions are present in La3Ni2TaO9 below 85 K. The contrasting properties of these compounds are discussed in terms of their microstructure.

The Influence of Beam Broadening on the Spatial Resolution of Annular Dark Field Scanning Transmission Electron Microscopy.

PubMed

de Jonge, Niels; Verch, Andreas; Demers, Hendrix

2018-02-01

The spatial resolution of aberration-corrected annular dark field scanning transmission electron microscopy was studied as function of the vertical position z within a sample. The samples consisted of gold nanoparticles (AuNPs) positioned in different horizontal layers within aluminum matrices of 0.6 and 1.0 µm thickness. The highest resolution was achieved in the top layer, whereas the resolution was reduced by beam broadening for AuNPs deeper in the sample. To examine the influence of the beam broadening, the intensity profiles of line scans over nanoparticles at a certain vertical location were analyzed. The experimental data were compared with Monte Carlo simulations that accurately matched the data. The spatial resolution was also calculated using three different theoretical models of the beam blurring as function of the vertical position within the sample. One model considered beam blurring to occur as a single scattering event but was found to be inaccurate for larger depths of the AuNPs in the sample. Two models were adapted and evaluated that include estimates for multiple scattering, and these described the data with sufficient accuracy to be able to predict the resolution. The beam broadening depended on z 1.5 in all three models.

The use of small angle X-ray scattering (SAXS) for the characterisation of lustre surfaces in Renaissance majolica

NASA Astrophysics Data System (ADS)

Fermo, P.; Cariati, F.; Cipriani, C.; Canetti, M.; Padeletti, G.; Brunetti, B.; Sgamellotti, A.

2002-01-01

In this work some Renaissance lustre decorated ceramics have been examined. Our attention was directed to lustre which is a thin decorative metallic film applied on the surfaces of previously glazed ancient pottery. Some 16th century lustre ceramics shards from Deruta, Umbria (Italy) have been analysed by small angle X-ray scattering (SAXS) in order to characterise the dimension of the metal nanocrystals forming the thin lustre layer. This technique appeared to be a powerful tool to characterise lustre films nanostructure and may be successfully used for this purpose together with transmission electron microscopy (TEM). Furthermore, SAXS measurements are extremely suitable for the determination of polydispersity and average interparticle distance. The lustre surfaces have been also analysed by scanning electron microscopy plus X-ray energy dispersive spectrometry (SEM-EDX) in order to identify the metals present (silver, copper or both of them) and to establish copper/silver ratios. From the comparison between SAXS results and compositional data, it was possible to conclude that copper particles are smaller than the silver ones. We have evidenced how the microtexture as well as the chemical composition of the lustre layers are responsible for the gold or red colour typical of the lustre films.

Surface-enhanced Raman scattering activity of niobium surface after irradiation with femtosecond laser pulses

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

Ivanov, Victor G.; Georgi Nadjakov Institute of Solid State Physics, BAS, 72 Tzarigradsko Chaussee, 1784 Sofia; Vlakhov, Emil S.

2015-11-28

The chemical modification of the niobium (Nb) surface after irradiation with femtosecond laser pulses was investigated by scanning electron microscopy coupled with energy dispersive spectroscopy, atomic force microscopy, grazing incidence X-ray diffraction, and micro-Raman spectroscopy. The physical-chemical analyses indicated that the laser treatment results in oxidation of the Nb surface, as well as in the formation of Nb hydrides. Remarkably, after the samples' washing in ethanol, a strong Surface-Enhanced Raman Scattering (SERS) signal originating from the toluene residual traces was evidenced. Further, it was observed that the laser irradiated Nb surface is able to provide a SERS enhancement of ∼1.3 × 10{supmore » 3} times for rhodamine 6G solutions. Thus, for the first time it was shown that Nb/Nb oxide surfaces could exhibit SERS functionality, and so one can expect applications in biological/biochemical screening or for sensing of dangerous environmental substances.« less

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.

New histopathologic and ultrastructural findings in Reis-Bücklers corneal dystrophy caused by the Arg124Leu mutation of TGFBI gene.

PubMed

Qiu, Wen-Ya; Zheng, Li-Bin; Pan, Fei; Wang, Bei-Bei; Yao, Yu-Feng

2016-09-02

Reis-Bücklers corneal dystrophy (RBCD) was consistently reported as a corneal dystrophy only affected Bowman's layer and superficial corneal stroma, and superficial keratectomy was a recommendation surgery for treatment in literatures. The study reported new histopathological and ultrastructural findings in RBCD caused by the Arg124Leu mutation of transforming growth factor induced (TGFBI) gene in a four-generation Chinese pedigree. Subjects including eight patients and seven unaffected family members received slit-lamp biomicroscopy and photography. DNA was obtained from all subjects, and exons 4 and 11 to 14 of TGFBI gene were analyzed by polymerase chain reaction and the products were sequenced. Anterior segment optical coherence tomography (AS OCT) and in vivo confocal microscopy were conducted for ten eyes of five patients. Based on the results of AS OCT and in vivo confocal microscopy, deep anterior lamellar keratoplasty (DLKP) using cryopreserved donor cornea was applied for four eyes of four patients. Four lamellar dystrophic corneal buttons were studied by light and transmission electron microscopy, and TGFBI immunohistochemistry. Eight patients had typical clinical manifestations of RBCD presenting recurrent painful corneal erosion starting in their early first decades, along with age-dependent progressive geographic corneal opacities. TGFBI sequencing revealed a heterozygous mutation, Arg124Leu in all eight patients. Anterior segment optical coherence tomography and in vivo confocal microscopy showed the dystrophic deposits involved not only in subepithelial and superficial stroma, but also in mid- or posterior stroma in four examined advanced eyes. Light microscopy showed Bowman's layer was absent, replaced by abnormal deposits stain bright red with Masson's trichrome. In superficial cornea, the deposits stacked and produced three to five continuous bands parallel to the corneal collagen lamellae. In mid- to posterior stroma, numerous granular or dot- like aggregates were heavily scattered, and most of them presented around the nuclei of stromal keratocytes. Transmission electron microscopy revealed the multiple electron-dense rod-shaped deposits aggregated and formed a characteristic pattern of three to five continuous bands in superficial cornea, which were similar to those seen under light microscopy. In mid- to posterior stroma, clusters of rod-shaped bodies were scattered extracellular or intracellular of the stromal keratocytes between the stromal lamellae suggesting the close relationship between mutated proteins and keratocyte. The study offer evidences indicating DLKP is a viable treatment option for advanced RBCD to avoid recurrence, and the mutated TGFBIp in dystrophic corneas are of keratocytes origin.

Particle formation in SiOx film deposition by low frequency plasma enhanced chemical vapor deposition

NASA Astrophysics Data System (ADS)

Yamaguchi, Tomoyo; Sakamoto, Naoshi; Shimozuma, Mitsuo; Yoshino, Masaki; Tagashira, Hiroaki

1998-01-01

Dust particle formation dynamics in the process of SiOx film deposition from a SiH4 and N2O gas mixture by a low frequency plasma enhanced chemical vapor deposition have been investigated using scanning electron microscopy and laser light scattering. The deposited films are confirmed to be SiOx from the measurements of Auger electron spectroscopy, x-ray photoelectron spectroscopy, and Fourier transform infrared spectroscopy. It is observed by scanning electron microscopy that particles are deposited on Si substrate at the plasma power frequency f=5 kHz and above both with and without substrate heating (400 °C), while no particle is deposited below f=1 kHz. Moreover, the laser light scattering indicates that particles are generated at the plasma power frequency of f=3 kHz and above in the gas phase, and that they are not generated in the gas phase at below f=3 kHz. Properties (the refractive index, resistivity, and Vickers hardness) of the films with particles are inferior to those of the films without particles. This article has revealed experimentally the effect of plasma power frequency on SiOx particle formation and makes a contribution to the explication of the particle formation mechanism. We suggest that high-quality film deposition with the low frequency plasma enhanced chemical vapor deposition method is attained at f=1 kHz or less without substrate heating.

Ultra-bright pulsed electron beam with low longitudinal emittance

DOEpatents

Zolotorev, Max

2010-07-13

A high-brightness pulsed electron source, which has the potential for many useful applications in electron microscopy, inverse photo-emission, low energy electron scattering experiments, and electron holography has been described. The source makes use of Cs atoms in an atomic beam. The source is cycled beginning with a laser pulse that excites a single Cs atom on average to a band of high-lying Rydberg nP states. The resulting valence electron Rydberg wave packet evolves in a nearly classical Kepler orbit. When the electron reaches apogee, an electric field pulse is applied that ionizes the atom and accelerates the electron away from its parent ion. The collection of electron wave packets thus generated in a series of cycles can occupy a phase volume near the quantum limit and it can possess very high brightness. Each wave packet can exhibit a considerable degree of coherence.

Coherent Anti-Stokes Raman Scattering Spectroscopy of Single Molecules in Solution

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

Sunney Xie, Wei Min, Chris Freudiger, Sijia Lu

2012-01-18

During this funding period, we have developed two breakthrough techniques. The first is stimulated Raman scattering microscopy, providing label-free chemical contrast for chemical and biomedical imaging based on vibrational spectroscopy. Spontaneous Raman microscopy provides specific vibrational signatures of chemical bonds, but is often hindered by low sensitivity. We developed a three-dimensional multiphoton vibrational imaging technique based on stimulated Raman scattering (SRS). The sensitivity of SRS imaging is significantly greater than that of spontaneous Raman microscopy, which is achieved by implementing high-frequency (megahertz) phase-sensitive detection. SRS microscopy has a major advantage over previous coherent Raman techniques in that it offers background-freemore » and readily interpretable chemical contrast. We demonstrated a variety of biomedical applications, such as differentiating distributions of omega-3 fatty acids and saturated lipids in living cells, imaging of brain and skin tissues based on intrinsic lipid contrast, and monitoring drug delivery through the epidermis. This technology offers exciting prospect for medical imaging. The second technology we developed is stimulated emission microscopy. Many chromophores, such as haemoglobin and cytochromes, absorb but have undetectable fluorescence because the spontaneous emission is dominated by their fast non-radiative decay. Yet the detection of their absorption is difficult under a microscope. We use stimulated emission, which competes effectively with the nonradiative decay, to make the chromophores detectable, as a new contrast mechanism for optical microscopy. We demonstrate a variety of applications of stimulated emission microscopy, such as visualizing chromoproteins, non-fluorescent variants of the green fluorescent protein, monitoring lacZ gene expression with a chromogenic reporter, mapping transdermal drug distribu- tions without histological sectioning, and label-free microvascular imaging based on endogenous contrast of haemoglobin. For all these applications, sensitivity is orders of magnitude higher than for spontaneous emission or absorption contrast, permitting nonfluorescent reporters for molecular imaging. Although we did not accomplish the original goal of detecting single-molecule by CARS, our quest for high sensitivity of nonlinear optical microscopy paid off in providing the two brand new enabling technologies. Both techniques were greatly benefited from the use of high frequency modulation for microscopy, which led to orders of magnitude increase in sensitivity. Extensive efforts have been made on optics and electronics to accomplish these breakthroughs.« less

Analysis of Scanned Probe Images for Magnetic Focusing in Graphene

DOE PAGES

Bhandari, Sagar; Lee, Gil-Ho; Kim, Philip; ...

2017-02-21

We have used cooled scanning probe microscopy (SPM) to study electron motion in nanoscale devices. The charged tip of the microscope was raster-scanned at constant height above the surface as the conductance of the device was measured. The image charge scatters electrons away, changing the path of electrons through the sample. Using this technique, we imaged cyclotron orbits that flow between two narrow contacts in the magnetic focusing regime for ballistic hBN–graphene–hBN devices. We present herein an analysis of our magnetic focusing imaging results based on the effects of the tip-created charge density dip on the motion of ballistic electrons.more » The density dip locally reduces the Fermi energy, creating a force that pushes electrons away from the tip. When the tip is above the cyclotron orbit, electrons are deflected away from the receiving contact, creating an image by reducing the transmission between contacts. The data and our analysis suggest that the graphene edge is rather rough, and electrons scattering off the edge bounce in random directions. However, when the tip is close to the edge, it can enhance transmission by bouncing electrons away from the edge, toward the receiving contact. Our results demonstrate that cooled SPM is a promising tool to investigate the motion of electrons in ballistic graphene devices.« less

Analysis of Scanned Probe Images for Magnetic Focusing in Graphene

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

Bhandari, Sagar; Lee, Gil-Ho; Kim, Philip

We have used cooled scanning probe microscopy (SPM) to study electron motion in nanoscale devices. The charged tip of the microscope was raster-scanned at constant height above the surface as the conductance of the device was measured. The image charge scatters electrons away, changing the path of electrons through the sample. Using this technique, we imaged cyclotron orbits that flow between two narrow contacts in the magnetic focusing regime for ballistic hBN–graphene–hBN devices. We present herein an analysis of our magnetic focusing imaging results based on the effects of the tip-created charge density dip on the motion of ballistic electrons.more » The density dip locally reduces the Fermi energy, creating a force that pushes electrons away from the tip. When the tip is above the cyclotron orbit, electrons are deflected away from the receiving contact, creating an image by reducing the transmission between contacts. The data and our analysis suggest that the graphene edge is rather rough, and electrons scattering off the edge bounce in random directions. However, when the tip is close to the edge, it can enhance transmission by bouncing electrons away from the edge, toward the receiving contact. Our results demonstrate that cooled SPM is a promising tool to investigate the motion of electrons in ballistic graphene devices.« less

Invited Review Article: Methods for imaging weak-phase objects in electron microscopy

PubMed Central

Glaeser, Robert M.

2013-01-01

Contrast has traditionally been produced in electron-microscopy of weak phase objects by simply defocusing the objective lens. There now is renewed interest, however, in using devices that apply a uniform quarter-wave phase shift to the scattered electrons relative to the unscattered beam, or that generate in-focus image contrast in some other way. Renewed activity in making an electron-optical equivalent of the familiar “phase-contrast” light microscope is based in part on the improved possibilities that are now available for device microfabrication. There is also a better understanding that it is important to take full advantage of contrast that can be had at low spatial frequency when imaging large, macromolecular objects. In addition, a number of conceptually new phase-plate designs have been proposed, thus increasing the number of options that are available for development. The advantages, disadvantages, and current status of each of these options is now compared and contrasted. Experimental results that are, indeed, superior to what can be accomplished with defocus-based phase contrast have been obtained recently with two different designs of phase-contrast aperture. Nevertheless, extensive work also has shown that fabrication of such devices is inconsistent, and that their working lifetime is short. The main limitation, in fact, appears to be electrostatic charging of any device that is placed into the electron diffraction pattern. The challenge in fabricating phase plates that are practical to use for routine work in electron microscopy thus may be more in the area of materials science than in the area of electron optics. PMID:24289381

Electron tomography of HEK293T cells using scanning electron microscope-based scanning transmission electron microscopy.

PubMed

You, Yun-Wen; Chang, Hsun-Yun; Liao, Hua-Yang; Kao, Wei-Lun; Yen, Guo-Ji; Chang, Chi-Jen; Tsai, Meng-Hung; Shyue, Jing-Jong

2012-10-01

Based on a scanning electron microscope operated at 30 kV with a homemade specimen holder and a multiangle solid-state detector behind the sample, low-kV scanning transmission electron microscopy (STEM) is presented with subsequent electron tomography for three-dimensional (3D) volume structure. Because of the low acceleration voltage, the stronger electron-atom scattering leads to a stronger contrast in the resulting image than standard TEM, especially for light elements. Furthermore, the low-kV STEM yields less radiation damage to the specimen, hence the structure can be preserved. In this work, two-dimensional STEM images of a 1-μm-thick cell section with projection angles between ±50° were collected, and the 3D volume structure was reconstructed using the simultaneous iterative reconstructive technique algorithm with the TomoJ plugin for ImageJ, which are both public domain software. Furthermore, the cross-sectional structure was obtained with the Volume Viewer plugin in ImageJ. Although the tilting angle is constrained and limits the resulting structural resolution, slicing the reconstructed volume generated the depth profile of the thick specimen with sufficient resolution to examine cellular uptake of Au nanoparticles, and the final position of these nanoparticles inside the cell was imaged.

Self healing of defected graphene

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

Chen, Jianhui; Shi, Tuwan; Cai, Tuocheng

For electronics applications, defects in graphene are usually undesirable because of their ability to scatter charge carriers, thereby reduce the carrier mobility. It would be extremely useful if the damage can be repaired. In this work, we employ Raman spectroscopy, X-ray photoemission spectroscopy, transmission electron microscopy, and electrical measurements to study defects in graphene introduced by argon plasma bombardment. We have found that majority of these defects can be cured by a simple thermal annealing process. The self-healing is attributed to recombination of mobile carbon adatoms with vacancies. With increasing level of plasma induced damage, the self-healing becomes less effective.

The effect of pathological processes on absorption and scattering spectra of samples of bile and pancreatic juice

NASA Astrophysics Data System (ADS)

Giraev, K. M.; Ashurbekov, N. A.; Magomedov, M. A.; Murtazaeva, A. A.; Medzhidov, R. T.

2015-07-01

Spectra of optical transmission coefficients and optical reflectance for bile and pancreatic juice samples were measured experimentally for different forms of pathologies of the pancreas within the range of 250-2500 nm. The absorption and scattering spectra, as well as the spectrum of the anisotropy factor of scattering, were determined based on the results obtained using the reverse Monte Carlo method. The surface morphology for the corresponding samples of the biological media was studied employing electron microscopy. The dynamics of the optical properties of the biological media was determined depending on the stage of the pathology. It has been demonstrated that the results of the study presented are in a good agreement with pathophysiological data and could supplement and broaden the results of conventional methods for diagnostics of the pancreas.

Novel of core-shell AlOOH/Cu nanostructures: Synthesis, characterization, antimicrobial activity and in vitro toxicity in Neuro-2a cells

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

Bakina, O. V., E-mail: ovbakina@ispms.tsc.ru; Fomenko, A. N., E-mail: alserova@ispms.tsc.ru; Korovin, M. S., E-mail: msk@ispms.tsc.ru

Core-shell micro/nanostructures were fabricated by the reaction of Al/Cu bimetallic nanoparticles with water. Al/Cu nanoparticles have been obtained using the method of simultaneous electrical explosion of a pair of the corresponding metal wires in an argon atmosphere. The nanoparticles are chemically active and interact with water at 60°C to form core-shell micro/nanostructures. The obtained products were characterized by means of X-ray diffraction, scanning electron microscopy, transmission electron microscopy and dynamic light scattering and the nitrogen adsorption method. The antibacterial activity of the synthesized structures was investigated against E. coli and St. aureus. The toxic effect of these nanostructures against themore » Neuro-2a neuroblastoma cell line was investigated. AlOOH/Cu nanostructures are shown to inhibit cell proliferation. The AlOOH/Cu nanostructures are good candidates for medical applications.« less

Synthesis of Norbornene Derived Helical Copolymer by Simple Molecular Marriage Approach to Produce Smart Nanocarrier

NASA Astrophysics Data System (ADS)

Mane, Shivshankar R.; Sathyan, Ashlin; Shunmugam, Raja

2017-03-01

A novel library of norbornene derived helical copolymer has been synthesized through the coupling of two homopolymers via Molecular Marriage Approach. The helicity is governed by the non-covalent interactions like hydrogen bonding, π-π stacking and the influence of hydrophobic and hydrophilic motifs. The detailed characterization of the copolymer (Copoly 1) has been provided and the super structures are confirmed through dynamic light scattering (DLS), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The observed size of the aggregates was about 200 nm. The density functional theory (DFT) is favorably supported for the formation of proposed structure of Copoly 1. Circular dichroism (CD) measurement has confirmed the one handed helical structure of the copolymer. Reservoir capability of this pH responsive polymer (Copoly 1) to encapsulate anti-cancer drug doxorubicin (DOX) warrants its potential applications in the field of bio-medical sciences.

Cryo-Scanning Electron Microscopy of Captured Cirrus Ice Particles

NASA Astrophysics Data System (ADS)

Magee, N. B.; Boaggio, K.; Bandamede, M.; Bancroft, L.; Hurler, K.

2016-12-01

We present the latest collection of high-resolution cryo-scanning electron microscopy images and microanalysis of cirrus ice particles captured by high-altitude balloon (ICE-Ball, see abstracts by K. Boaggio and M. Bandamede). Ice particle images and sublimation-residues are derived from particles captured during approximately 15 balloon flights conducted in Pennsylvania and New Jersey over the past 12 months. Measurements include 3D digital elevation model reconstructions of ice particles, and associated statistical analyses of entire particles and particle sub-facets and surfaces. This 3D analysis reveals that morphologies of most ice particles captured deviate significantly from ideal habits, and display geometric complexity and surface roughness at multiple measureable scales, ranging from 100's nanometers to 100's of microns. The presentation suggests potential a path forward for representing scattering from a realistically complex array of ice particle shapes and surfaces.

Ultrasensitive ROS-Responsive Coassemblies of Tellurium-Containing Molecules and Phospholipids.

PubMed

Wang, Lu; Fan, Fuqiang; Cao, Wei; Xu, Huaping

2015-07-29

Reactive oxygen species (ROS) play crucial roles in cell signaling and redox homeostasis and are strongly related to metabolic activities. The increase of the ROS concentration in organisms can result in several diseases, such as cardiovascular diseases and cancer. The concentration of ROS in biologically relevant conditions is typically as low as around tens of micromolars to 100 μM H2O2, which makes it necessary to develop ultrasensitive ROS-responsive systems. A general approach is reported here to fabricate an ultrasensitive ROS-responsive system via coassembly between tellurium-containing molecules and phospholipids, combining the ROS-responsiveness of tellurium and the biocompatibility of phospholipids. By using dynamic light scattering, transmission electron microscopy, scanning electron microscopy, and NMR spectra, coassembly behaviors and the responsiveness of the coassemblies have been investigated. These coassemblies can respond to 100 μM H2O2, which is a biologically relevant ROS concentration, and demonstrate reversible redox properties.

Sonoelectrochemical one-pot synthesis of Pt - Carbon black nanocomposite PEMFC electrocatalyst.

PubMed

Karousos, Dionysios S; Desdenakis, Kostantinos I; Sakkas, Petros M; Sourkouni, Georgia; Pollet, Bruno G; Argirusis, Christos

2017-03-01

Simultaneous electrocatalytic Pt-nanoparticle synthesis and decoration of Vulcan XC-72 carbon black substrate was achieved in a novel one-step-process, combining galvanostatic pulsed electrodeposition and pulsed ultrasonication with high power, low-frequency (20kHz) ultrasound. Aqueous chloroplatinic acid precursor baths, as well as carbon black suspensions in the former, were examined and decoration was proven by a combination of characterization methods, namely: dynamic light scattering, transmission electron microscopy, scanning electron microscopy with EDX-analysis and cyclic voltammetry. In particular, PVP was shown to have a beneficial stabilizing effect against free nanoparticle aggregation, ensuring narrow size distributions of the nanoparticles synthesized, but is also postulated to prevent the establishment of a strong metal-substrate interaction. Current pulse amplitude was identified as the most critical nanoparticle size-determining parameters, while only small size particles, under 10nm, appeared to be attached to carbon black. Copyright © 2016 Elsevier B.V. All rights reserved.

Nanostructured zirconium phosphate as ion exchanger: Synthesis, size dependent property and analytical application in radiochemical separation.

PubMed

Chakraborty, Rajesh; Bhattacharaya, Koustava; Chattopadhyay, Pabitra

2014-02-01

Nanostructured zirconium phosphates (ZPs) of different sizes were synthesized using Tritron X-100 (polyethylene glycol-p-isooctylphenyl ether) surfactant. The materials were characterized by FTIR and powdered X-ray diffraction (XRD). The structural and morphological details of the material were established by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The SEM study was followed by energy dispersive spectroscopic analysis (EDS) for elemental analysis of the sample. The particle sizes were determined by dynamic light scattering (DLS) method. Ion exchange capacity of these nanomaterials towards different metal ions was measured and size-dependent ion exchange property of the materials was investigated thoroughly. The nanomaterial of the smallest size (ca. 21.04nm) was employed to separate carrier-free (137m)Ba from (137)Cs in column chromatographic technique using 1.0M HNO3 as eluting agent at pH=5. © 2013 Elsevier Ltd. All rights reserved.

Physicochemical properties of micelles of poly(styrene-b-[3-(methacryloylamino)propyl]trimethylammonium chloride-b-ethylene oxide) in aqueous solutions.

PubMed

Liu, Jingjing; Liu, Dian; Yokoyama, Yuuichi; Yusa, Shin-Ichi; Nakashima, Kenichi

2009-01-20

Polymeric micelles from a new triblock copolymer, polystyrene-block-poly[(3-(methacryloylamino)propyl)trimethylammonium chloride]-block-poly(ethylene oxide) (PS-b-PMAPTAC-b-PEO), were prepared in aqueous solutions and characterized by various techniques including dynamic light scattering (DLS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and fluorescence spectroscopy. The micelle consists of a PS core, PMAPTAC shell, and PEO corona. It was revealed by SEM and DLS measurements that the micelles have a spherical structure with a hydrodynamic diameter about 75 nm. The addition of tungstate to the micellar solution caused a morphological change in the micelles from extended to shrunken spheres, which can be attributed to the fact that electrostatic repulsion among the cationic PMAPTAC blocks is canceled by the negative charge of the bound tungstate ions. Effective incorporation of tungstate ions into the micelles were confirmed by TEM and zeta-potential measurements.

Ultra-small and anionic starch nanospheres: formation and vitro thrombolytic behavior study.

PubMed

Huang, Yinjuan; Ding, Shenglong; Liu, Mingzhu; Gao, Chunmei; Yang, Jinlong; Zhang, Xinjie; Ding, Bin

2013-07-25

This paper is considered as the first report on the investigation of nattokinase (NK) release from anionic starch nanospheres. The ultra-small and anionic starch nanospheres were prepared by the method of reverse micro-emulsion crosslinking in this work. Starch nanospheres were characterized through Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and dynamic light scattering (DLS). Effects of preparation conditions on particle size were studied. The cytotoxicity, biodegradable and vitro thrombolytic behaviors of nattokinase (NK) loaded anionic starch nanospheres were also studied. The results showed that the anionic starch nanospheres are non-toxic, biocompatible and biodegradable. Moreover, the anionic starch nanospheres can protect NK from fast biodegradation hence prolongs the circulation in vivo and can reduce the risk of acute hemorrhage complication by decreasing the thrombolysis rate. Copyright © 2013 Elsevier Ltd. All rights reserved.

Incipient crystallization of transition-metal tungstates under microwaves probed by Raman scattering and transmission electron microscopy

NASA Astrophysics Data System (ADS)

Siqueira, Kisla P. F.; Dias, Anderson

2011-11-01

Microwave synthesis was used to produce nanosized transition-metal tungstates in environmentally friendly conditions not yet reported by the literature: 110 and 150 °C, for times of 10 and 20 min. X-ray diffraction evidenced incipient crystallized materials, while transmission electron microscopy indicates nanostructured regions of about 2-5 nm inside an amorphous matrix. Raman spectroscopy was used to probe short-range ordering in the achieved samples and also to obtain a reliable set of spectra containing all the Raman-active bands predicted by group-theory calculations. The vibrational spectra showed no extra feature, indicating that the microwave processing was able to produce short-range ordered materials without tetrahedral distortions. These distortions are frequently reported when commercially modified kitchen microwave units are employed. In this work, the syntheses were conducted in a commercial apparatus especially designed for fully controlled temperature-time-pressure conditions.

Solution and electron microscopy characterization of lactococcal phage baseplates expressed in Escherichia coli.

PubMed

Campanacci, Valérie; Veesler, David; Lichière, Julie; Blangy, Stéphanie; Sciara, Giuliano; Moineau, Sylvain; van Sinderen, Douwe; Bron, Patrick; Cambillau, Christian

2010-10-01

We report here the characterization of several large structural protein complexes forming the baseplates (or part of them) of Siphoviridae phages infecting Lactococcus lactis: TP901-1, Tuc2009 and p2. We revisited a "block cloning" expression strategy and extended this approach to genomic fragments encoding proteins whose interacting partners have not yet been clearly identified. Biophysical characterization of some of these complexes using circular dichroism and size exclusion chromatography, coupled with on-line light scattering and refractometry, demonstrated that the over-produced recombinant proteins interact with each other to form large (up to 1.9MDa) and stable baseplate assemblies. Some of these complexes were characterized by electron microscopy confirming their structural homogeneity as well as providing a picture of their overall molecular shapes and symmetry. Finally, using these results, we were able to highlight similarities and differences with the well characterized much larger baseplate of the myophage T4.

Preparation and characterization of novel carbon dioxide adsorbents based on polyethylenimine-modified Halloysite nanotubes.

PubMed

Cai, Haohao; Bao, Feng; Gao, Jie; Chen, Tao; Wang, Si; Ma, Rui

2015-01-01

New nano-sized carbon dioxide (CO2) adsorbents based on Halloysite nanotubes impregnated with polyethylenimine (PEI) were designed and synthesized, which were excellent adsorbents for the capture of CO2 at room temperature and had relatively high CO2 adsorption capacity. The prepared adsorbents were characterized by various techniques such as Fourier transform infrared spectrometry, gel permeation chromatography, dynamic light scattering, thermogravimetry, thermogravimetry-Fourier transform-infrared spectrometry, scanning electron microscopy and transmission electron microscopy. The adsorption characteristics and capacity were studied at room temperature, the highest CO2 adsorption capacity of 156.6 mg/g-PEI was obtained and the optimal adsorption capacity can reach a maximum value of 54.8 mg/g-adsorbent. The experiment indicated that this kind of adsorbent has a high stability at 80°C and PEI-impregnated adsorbents showed good reversibility and stability during cyclic adsorption-regeneration tests.

Comparative analysis of the effect of low-dimensional alumina structures on cell lines L929 and Neuro-2a

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

Fomenko, A. N., E-mail: alserova@ispms.tsc.ru; Korovin, M. S., E-mail: msk@ispms.tsc.ru

The paper presents the toxicity evaluation of nanostructures on the basis of alumina of different shape (nanofibers, nanoplates, nanosheets, nanosheet agglomerates) and with similar physical and chemical properties (particle size, specific surface area, phase composition, and zeta potential). The nanostructures were examined by transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray diffraction (XRD), low-temperature nitrogen adsorption, and dynamic light scattering (DLS). The cytotoxicity of nanostructures was estimated using L929 fibroblast cells and Neuro-2a tumor cells. It has been found that the L929 cells are less subject to the influence of alumina nanoparticles than the Neuro-2a tumor cells. Probably, themore » differences in the proliferation activity of normal and tumor cells in contact with the synthesized nanostructures are due to a change in the pH of the cell microenvironment.« less

Novel of core-shell AlOOH/Cu nanostructures: Synthesis, characterization, antimicrobial activity and in vitro toxicity in Neuro-2a cells

NASA Astrophysics Data System (ADS)

Bakina, O. V.; Fomenko, A. N.; Korovin, M. S.; Glazkova, E. A.; Svarovskaya, N. V.

2016-08-01

Core-shell micro/nanostructures were fabricated by the reaction of Al/Cu bimetallic nanoparticles with water. Al/Cu nanoparticles have been obtained using the method of simultaneous electrical explosion of a pair of the corresponding metal wires in an argon atmosphere. The nanoparticles are chemically active and interact with water at 60°C to form core-shell micro/nanostructures. The obtained products were characterized by means of X-ray diffraction, scanning electron microscopy, transmission electron microscopy and dynamic light scattering and the nitrogen adsorption method. The antibacterial activity of the synthesized structures was investigated against E. coli and St. aureus. The toxic effect of these nanostructures against the Neuro-2a neuroblastoma cell line was investigated. AlOOH/Cu nanostructures are shown to inhibit cell proliferation. The AlOOH/Cu nanostructures are good candidates for medical applications.

Comparative analysis of the effect of low-dimensional alumina structures on cell lines L929 and Neuro-2a

NASA Astrophysics Data System (ADS)

Fomenko, A. N.; Korovin, M. S.

2016-08-01

The paper presents the toxicity evaluation of nanostructures on the basis of alumina of different shape (nanofibers, nanoplates, nanosheets, nanosheet agglomerates) and with similar physical and chemical properties (particle size, specific surface area, phase composition, and zeta potential). The nanostructures were examined by transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray diffraction (XRD), low-temperature nitrogen adsorption, and dynamic light scattering (DLS). The cytotoxicity of nanostructures was estimated using L929 fibroblast cells and Neuro-2a tumor cells. It has been found that the L929 cells are less subject to the influence of alumina nanoparticles than the Neuro-2a tumor cells. Probably, the differences in the proliferation activity of normal and tumor cells in contact with the synthesized nanostructures are due to a change in the pH of the cell microenvironment.

Synthesis of Norbornene Derived Helical Copolymer by Simple Molecular Marriage Approach to Produce Smart Nanocarrier.

PubMed

Mane, Shivshankar R; Sathyan, Ashlin; Shunmugam, Raja

2017-03-22

A novel library of norbornene derived helical copolymer has been synthesized through the coupling of two homopolymers via Molecular Marriage Approach. The helicity is governed by the non-covalent interactions like hydrogen bonding, π-π stacking and the influence of hydrophobic and hydrophilic motifs. The detailed characterization of the copolymer (Copoly 1) has been provided and the super structures are confirmed through dynamic light scattering (DLS), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The observed size of the aggregates was about 200 nm. The density functional theory (DFT) is favorably supported for the formation of proposed structure of Copoly 1. Circular dichroism (CD) measurement has confirmed the one handed helical structure of the copolymer. Reservoir capability of this pH responsive polymer (Copoly 1) to encapsulate anti-cancer drug doxorubicin (DOX) warrants its potential applications in the field of bio-medical sciences.

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.

Study of Etching Pits in a Large-grain Single Cell Bulk Niobium Cavity

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

Zhao, Xin; Ciovati, Gianluigi; Reece, Charles E.

2009-11-01

Performance of SRF cavities are limited by non-linear localized effects. The variation of local material characters between "hot" and "cold" spots is thus of intense interest. Such locations were identified in a BCP-etched large-grain single-cell cavity and removed for examination by high resolution electron microscopy (SEM), electron-back scattering diffraction microscopy (EBSD), optical microscopy, and 3D profilometry. Pits with clearly discernable crystal facets were observed in both "hotspot" and "coldspot" specimens. The pits were found in-grain, at bi-crystal boundaries, and on tri-crystal junctions. They are interpreted as etch pits induced by surface crystal defects (e.g. dislocations). All "coldspots" examined had qualitativelymore » low density of etching pits or very shallow tri-crystal boundary junction. EBSD revealed crystal structure surrounding the pits via crystal phase orientation mapping, while 3D profilometry gave information on the depth and size of the pits. In addition, a survey of the samples by energy dispersive X-ray analysis (EDX) did not show any significant contamination of the samples surface.« less

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

Plasmonics and SERS activity of post-transition metal nanoparticles

NASA Astrophysics Data System (ADS)

Bezerra, A. G.; Machado, T. N.; Woiski, T. D.; Turchetti, D. A.; Lenz, J. A.; Akcelrud, L.; Schreiner, W. H.

2018-05-01

Nanoparticles of the post-transition metals, In, Sn, Pb, and Bi, and of the metalloid Sb were produced by laser ablation synthesis in solution (LASiS) and tested for localized surface plasmon resonances (LSPR) and surface-enhanced Raman scattering (SERS). The nanoparticles were characterized by UV-Vis optical absorption, dynamic light scattering (DLS), and transmission electron microscopy (TEM). Several organic and biological molecules were tested, and SERS activity was demonstrated for all tested nanoparticles and molecules. The Raman enhancement factor for each nanoparticle class and molecule was experimentally determined. The search for new plasmonic nanostructures is important mainly for life sciences-related applications and this study expands the range of SERS active systems.

Graphene-based textured surface by pulsed laser deposition as a robust platform for surface enhanced Raman scattering applications

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

Tite, T.; Donnet, C.; Loir, A.-S.

We have developed a surface enhanced Raman scattering (SERS)-active substrate based on gold nanoparticles-decorated few-layer (fl) graphene grown by pulsed laser deposition. Diamond-Like Carbon film has been converted to fl-graphene after thermal annealing at low temperature. The formation of fl-graphene was confirmed by Raman spectroscopy, and surface morphology was highlighted by scanning electron microscopy. We found that textured fl-graphene film with nanoscale roughness was highly beneficial for SERS detection. Rhodamine 6G and p-aminothiophenol proposed as test molecules were detected with high sensitivity. The detection at low concentration of deltamethrin, an active molecule of a commercial pesticide was further demonstrated.

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

Surface-functionalized cockle shell–based calcium carbonate aragonite polymorph as a drug nanocarrier

PubMed Central

Mohd Abd Ghafar, Syairah Liyana; Hussein, Mohd Zobir; Rukayadi, Yaya; Abu Bakar Zakaria, Md Zuki

2017-01-01

Calcium carbonate aragonite polymorph nanoparticles derived from cockle shells were prepared using surface functionalization method followed by purification steps. Size, morphology, and surface properties of the nanoparticles were characterized using transmission electron microscopy, field emission scanning electron microscopy, dynamic light scattering, zetasizer, X-ray powder diffraction, and Fourier transform infrared spectrometry techniques. The potential of surface-functionalized calcium carbonate aragonite polymorph nanoparticle as a drug-delivery agent were assessed through in vitro drug-loading test and drug-release test. Transmission electron microscopy, field emission scanning electron microscopy, and particle size distribution analyses revealed that size, morphology, and surface characterization had been improved after surface functionalization process. Zeta potential of the nanoparticles was found to be increased, thereby demonstrating better dispersion among the nanoparticles. Purification techniques showed a further improvement in the overall distribution of nanoparticles toward more refined size ranges <100 nm, which specifically favored drug-delivery applications. The purity of the aragonite phase and their chemical analyses were verified by X-ray powder diffraction and Fourier transform infrared spectrometry studies. In vitro biological response of hFOB 1.19 osteoblast cells showed that surface functionalization could improve the cytotoxicity of cockle shell–based calcium carbonate aragonite nanocarrier. The sample was also sensitive to pH changes and demonstrated good abilities to load and sustain in vitro drug. This study thus indicates that calcium carbonate aragonite polymorph nanoparticles derived from cockle shells, a natural biomaterial, with modified surface characteristics are promising and can be applied as efficient carriers for drug delivery. PMID:28572724

Morphology and Dynamic Mechanical Properties of Diglycidyl Ether of Bisphenol-A Toughened with Carboxyl-Terminated Butadiene-Acrylonitrile

NASA Technical Reports Server (NTRS)

Hong, S. D.; Chung, S. Y.; Fedors, R. F.; Moacanin, J.; Gupta, A.

1984-01-01

The fracture toughness of an incorporation of a carboxyl-terminated butadiene acrylonitrile (CTBN) elastomer in diglycidyl ether bisphenol A (DGEBA) resin was investigated. Measurements of dynamic mechanical properties, scanning electron microscopy and small-angle X-ray scattering were carried out to characterize the state of cure, morphology and particle size and size distribution of the neat resins and their graphite fiber reinforced composites.

From structure to structural dynamics: Ahmed Zewail's legacy.

PubMed

Chergui, Majed; Thomas, John Meurig

2017-07-01

In this brief tribute to Ahmed Zewail, we highlight and place in the historical context, several of the major achievements that he and his colleagues have made in Femtochemistry (of which he was the principal instigator) and his introduction of ultrafast electron scattering, diffraction, microscopy and spectroscopy. By achieving a sub-picosecond temporal resolution, coupled with a picometer spatial resolution, he revolutionised our understanding of the corpus of chemical, physical, biological and materials science systems.

Understanding and Controlling the Electronic Properties of Graphene Using Scanning Probe Microscopy

DTIC Science & Technology

2014-07-21

Dirac point in gated bilayer graphene, Applied Physics Letters, (12 2009): 243502. doi : 10.1063/1.3275755 Brian J. LeRoy, Adam T. Roberts, Rolf...of soliton motion and stacking in trilayer graphene, Nature Materials , (04 2014): 0. doi : 10.1038/nmat3965 Matthew Yankowitz, Joel I-Jan Wang...of bilayer graphene via quasiparticle scattering, APL Materials , (09 2014): 92503. doi : Matthew Yankowitz, Fenglin Wang, Chun Ning Lau, Brian J

Graphene Plasmonics for Tunable Terahertz Metamaterials

DTIC Science & Technology

2011-10-01

anomalous quantumHall effect15,16 andKlein tunnelling17,18 in electrical transport to a universal absorption constant19,20 and tunable interband ...electron scattering spectroscopy25,26 and inelastic scanning tunnelling microscopy27. However, the fundamental behaviour of light–plasmon coupling in...ribbon arrays. Here TCNP is the transmission coefficient at CNP and DT¼ T2 TCNP. The 2DT/TCNP spectra of a gated 4 mm sample (Vg¼22.0 V) for terahertz

Photochemical mineralization of europium, titanium, and iron oxyhydroxide nanoparticles in the ferritin protein cage.

PubMed

Klem, Michael T; Mosolf, Jesse; Young, Mark; Douglas, Trevor

2008-04-07

The Fe storage protein ferritin was used as a size-constrained reaction vessel for the photoreduction and reoxidation of complexed Eu, Fe, and Ti precursors for the formation of oxyhydroxide nanoparticles. The resultant materials were characterized by dynamic light scattering, gel electrophoresis, UV-vis spectroscopy, and transmission electron microscopy. The photoreduction and reoxidation process is inspired by biological sequestration mechanisms observed in some marine siderophore systems.

Evolution of Microstructure in a Nickel-based Superalloy as a Function of Ageing Time

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

Chen, Wei-Ren; Smith, Gregory Scott; Porcar, L.

2011-01-01

An experimental investigation, combining synchrotron X-ray powder diffraction, small-angle neutron-scattering, and transmission electron microscopy, has been undertaken to study the microstructure of nanoprecipitates in a nickel-based superalloy. Upon increasing the ageing time during a heat-treatment process, the average size of the precipitates first decreases before changing to a monotonical growth stage. Possible reasons for this observed structural evolution, which is predicted thermodynamically, are suggested.

CO2-switchable fluorescence of a dendritic polymer and its applications

NASA Astrophysics Data System (ADS)

Gao, Chunmei; Lü, Shaoyu; Liu, Mingzhu; Wu, Can; Xiong, Yun

2015-12-01

The synthesis and properties of CO2 responsive and fluorescent dendritic polymers, poly(amido amine)/Pluronic F127 (PAMAM/F127), are reported in this paper. The morphologies and sizes of PAMAM/F127 dendritic polymers were investigated by dynamic light scattering (DLS) and transmission electron microscopy (TEM). PAMAM/F127 dendritic polymers showed unimolecular micelle morphologies at low concentrations, and changed to multimolecular micelles at higher concentrations. Additionally, fluorescence spectra and confocal laser scanning microscopy images showed that PAMAM/F127 dendritic polymers exhibited a fluorescent enhancement response to the presence of CO2. Apart from that, the release behavior of PAMAM/F127 gels under simulated body fluids was investigated by choosing curcumin as the hydrophobic drug. The results indicated that PAMAM/F127 dendritic polymers can be used to improve the solubility of curcumin, and the drug released faster in the presence of CO2. Such CO2 responsive fluorescent dendritic polymers are potentially applicable in cellular imaging or drug controlled release.The synthesis and properties of CO2 responsive and fluorescent dendritic polymers, poly(amido amine)/Pluronic F127 (PAMAM/F127), are reported in this paper. The morphologies and sizes of PAMAM/F127 dendritic polymers were investigated by dynamic light scattering (DLS) and transmission electron microscopy (TEM). PAMAM/F127 dendritic polymers showed unimolecular micelle morphologies at low concentrations, and changed to multimolecular micelles at higher concentrations. Additionally, fluorescence spectra and confocal laser scanning microscopy images showed that PAMAM/F127 dendritic polymers exhibited a fluorescent enhancement response to the presence of CO2. Apart from that, the release behavior of PAMAM/F127 gels under simulated body fluids was investigated by choosing curcumin as the hydrophobic drug. The results indicated that PAMAM/F127 dendritic polymers can be used to improve the solubility of curcumin, and the drug released faster in the presence of CO2. Such CO2 responsive fluorescent dendritic polymers are potentially applicable in cellular imaging or drug controlled release. Electronic supplementary information (ESI) available. See DOI: 10.1039/c5nr06729d

Atomic-scale Visualization of Electronic Nematicity and Cooper Pairing in Iron-based Superconductors

NASA Astrophysics Data System (ADS)

Allan, Milan P.

2013-03-01

The mechanism of high-temperature superconductivity in the relatively novel iron-based high-Tc superconductors is unresolved, both in terms of how the phases evolve with doping, and in terms of the actual Cooper pairing process. To explore these issues, we used spectroscopic-imaging scanning tunneling microscopy to study the electronic structure of CaFe2As2 in the antiferromagnetic-orthorhombic `parent' state from which the superconductivity emerges. We discovered and visualized the now widely studied electronic `nematicity' of this phase, whose suppression is associated with the emergence of superconductivity (Science 327, 181, 2010). As subsequent transport experiments discovered a related anisotropic conductance which increases with dopant concentration, the interplay between the electronic structure surrounding each dopant atom, quasiparticle scattering therefrom, and the transport nematicity has become a pivotal focus of research. We find that substituting Co for Fe atoms in underdoped Ca(Fe1-xCox)2As2 generates a dense population of identical and strongly anisotropic impurity states that are distributed randomly but aligned with the antiferromagnetic a-axis. We also demonstrate, by imaging their surrounding interference patterns, that these impurity states scatter quasiparticles and thus influence transport in a highly anisotropic manner (M.P. Allan et al., 2013). Next, we studied the momentum dependence of the energy gaps of iron-based superconductivity, now focusing on LiFeAs. If strong electron-electron interactions mediate the Cooper pairing, then momentum-space anisotropic superconducting energy gaps Δi (k) were predicted by multiple techniques to appear on the different electronic bands i. We introduced intraband Bogoliubov quasiparticle scattering interference (QPI) techniques for the determination of anisotropic energy gaps to test these hypotheses and discovered the anisotropy, magnitude, and relative orientations of the energy gaps on multiple bands (Science 336, 563 (2012)). Finally, the electron-electron interactions generating Cooper pairing are often conjectured to involve bosonic spin fluctuations generated by interband scattering of electrons. We explore the STM signatures of both the interband scattering and the electron-boson coupling self-energy in LiFeAs, and detect the signatures of the electron-boson coupling (M.P. Allan et al., in preparation). In collaboration with A.W. Rost, T.-M. Chuang, F. Massee, M.S. Golden, Y. Xie, M.H. Fisher, E.-A. Kim, K. Lee, Ni Ni, S.L. Bud'ko, P.C. Canfield, Q. Wang, D.S. Dessau, K. Kihou, C.H. Lee, A. Iyo, H. Eisaki, D.J. Scalapino, A.P. Mackenzie and J.C. Davis

The application of inelastic neutron scattering to explore the significance of a magnetic transition in an iron based Fischer-Tropsch catalyst that is active for the hydrogenation of CO

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

Warringham, Robbie; McFarlane, Andrew R.; Lennon, David, E-mail: David.Lennon@Glasgow.ac.uk

2015-11-07

An iron based Fischer-Tropsch synthesis catalyst is evaluated using CO hydrogenation at ambient pressure as a test reaction and is characterised by a combination of inelastic neutron scattering (INS), powder X-ray diffraction, temperature-programmed oxidation, Raman scattering, and transmission electron microscopy. The INS spectrum of the as-prepared bulk iron oxide pre-catalyst (hematite, α-Fe{sub 2}O{sub 3}) is distinguished by a relatively intense band at 810 cm{sup −1}, which has previously been tentatively assigned as a magnon (spinon) feature. An analysis of the neutron scattering intensity of this band as a function of momentum transfer unambiguously confirms this assignment. Post-reaction, the spinon featuremore » disappears and the INS spectrum is characterised by the presence of a hydrocarbonaceous overlayer. A role for the application of INS in magnetic characterisation of iron based FTS catalysts is briefly considered.« less

Biomineralization of endolithic microbes in rocks from the McMurdo Dry Valleys of Antarctica: implications for microbial fossil formation and their detection.

PubMed

Wierzchos, Jacek; Sancho, Leopoldo García; Ascaso, Carmen

2005-04-01

In some zones of Antarctica's cold and dry desert, the extinction of cryptoendolithic microorganisms leaves behind inorganic traces of microbial life. In this paper, we examine the transition from live microorganisms, through their decay, to microbial fossils using in situ microscopy (transmission electron microscopy, scanning electron microscopy in back-scattered electron mode) and microanalytical (energy dispersive X-ray spectroscopy) techniques. Our results demonstrate that, after their death, endolithic microorganisms inhabiting Commonwealth Glacier sandstone from the Antarctica McMurdo Dry Valleys become mineralized. In some cases, epicellular deposition of minerals and/or simply filling up of empty moulds by minerals leads to the formation of cell-shaped structures that may be considered biomarkers. The continuous deposition of allochthonous clay minerals and sulfate-rich salts fills the sandstone pores. This process can give rise to microbial fossils with distinguishable cell wall structures. Often, fossilized cell interiors were of a different chemical composition to the mineralized cell walls. We propose that the microbial fossil formation observed was induced by mineral precipitation resulting from inorganic processes occurring after the death of cryptoendolithic microorganisms. Nevertheless, it must have been the organic template that provoked the diffusion of mineral elements and gave rise to their characteristic distribution pattern inside the fossilized cells.

The electron microscope appearance of the subchondral bone plate in the human femoral head in osteoarthritis and osteoporosis

PubMed Central

LI, BAOHUA; MARSHALL, DEBORAH; ROE, MARTIN; ASPDEN, RICHARD M.

1999-01-01

The subchondral bone plate supports the articular cartilage in diarthrodial joints. It has a significant mechanical function in transmitting loads from the cartilage into the underlying cancellous bone and has been implicated in the destruction of cartilage in osteoarthritis (OA) and its sparing in osteoporosis (OP), but little is known of its composition, structure or material properties. This study investigated the microscopic appearance and mineral composition of the subchondral bone plate in femoral heads from patients with OA or OP to determine how these correspond to changes in composition and stiffness found in other studies. Freeze-fractured full-depth samples of the subchondral bone plate from the femoral heads of patients with osteoarthritis, osteoporosis or a matched control group were examined using back scattered and secondary emission scanning electron microscopy. Other samples were embedded and polished and examined using back-scattered electron microscopy and electron probe microanalysis. The appearances of the samples from the normal and osteoporotic patients were very similar, with the subchondral bone plate overlayed by a layer of calcified cartilage. Osteoporotic samples presented a more uniform fracture surface and the relative thicknesses of the layers appeared to be different. In contrast, the OA bone plate appeared to be porous and have a much more textured surface. There were occasional sites of microtrabecular bone formation between the trabeculae of the underlying cancellous bone, which were not seen in the other groups, and more numerous osteoclast resorption pits. The calcified cartilage layer was almost absent and the bone plate was apparently thickened. The appearance of the osteoarthritic subchondral bone plate was, therefore, considerably different from both the normal and the osteoporotic, strongly indicative of abnormal cellular activity. PMID:10473297

Encapsulation efficiency of CdSe/ZnS quantum dots by liposomes determined by thermal lens microscopy

PubMed Central

Batalla, Jessica; Cabrera, Humberto; San Martín-Martínez, Eduardo; Korte, Dorota; Calderón, Antonio; Marín, Ernesto

2015-01-01

In this study the encapsulation of core shell carboxyl CdSe/ZnS quantum dots (QDs) by phospholipids liposome complexes is presented. It makes the quantum dots water soluble and photo-stable. Fluorescence self-quenching of the QDs inside the liposomes was observed. Therefore, the thermal lens microscopy (TLM) was found to be an useful tool for measuring the encapsulation efficiency of the QDs by the liposomes, for which an optimum value of 36% was determined. The obtained limit of detection (LOD) for determining QDs concentration by TLM was 0.13 nM. Moreover, the encapsulated QDs showed no prominent cytotoxicity toward Breast cancer cells line MDA-MB-231. This study was supported by UV-visible spectroscopy, high resolution transmission electron microscopy (HRTEM) and dynamic light scattering measurements (DLS). PMID:26504640

Size and surface effects on the magnetism of magnetite and maghemite nanoparticles

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

Nikiforov, V. N., E-mail: pppnvn@yandex.ru; Ignatenko, A. N.; Irkhin, V. Yu.

2017-02-15

The size effects of magnetite and maghemite nanoparticles on their magnetic properties (magnetic moment, Curie temperature, blocking temperature, etc.) have been investigated. Magnetic separation and centrifugation of an aqueous solution of nanoparticles were used for their separation into fractions; their sizes were measured by atomic force microscopy, dynamic light scattering, and electron microscopy. A change in the size leads to a change in the Curie temperature and magnetic moment per formula unit. Both native nanoparticles and those covered with a bioresorbable layer have been considered. The magnetic properties have been calculated by the Monte Carlo method for the classical Heisenbergmore » model with various bulk and surface magnetic moments.« less

Interaction of Water-Soluble CdTe Quantum Dots with Bovine Serum Albumin

PubMed Central

2011-01-01

Semiconductor nanoparticles (quantum dots) are promising fluorescent markers, but it is very little known about interaction of quantum dots with biological molecules. In this study, interaction of CdTe quantum dots coated with thioglycolic acid (TGA) with bovine serum albumin was investigated. Steady state spectroscopy, atomic force microscopy, electron microscopy and dynamic light scattering methods were used. It was explored how bovine serum albumin affects stability and spectral properties of quantum dots in aqueous media. CdTe–TGA quantum dots in aqueous solution appeared to be not stable and precipitated. Interaction with bovine serum albumin significantly enhanced stability and photoluminescence quantum yield of quantum dots and prevented quantum dots from aggregating. PMID:27502633

Controlling self-assembly of diphenylalanine peptides at high pH using heterocyclic capping groups

PubMed Central

Martin, Adam D.; Wojciechowski, Jonathan P.; Robinson, Andrew B.; Heu, Celine; Garvey, Christopher J.; Ratcliffe, Julian; Waddington, Lynne J.; Gardiner, James; Thordarson, Pall

2017-01-01

Using small angle neutron scattering (SANS), it is shown that the existence of pre-assembled structures at high pH for a capped diphenylalanine hydrogel is controlled by the selection of N-terminal heterocyclic capping group, namely indole or carbazole. At high pH, changing from a somewhat hydrophilic indole capping group to a more hydrophobic carbazole capping group results in a shift from a high proportion of monomers to self-assembled fibers or wormlike micelles. The presence of these different self-assembled structures at high pH is confirmed through NMR and circular dichroism spectroscopy, scanning probe microscopy and cryogenic transmission electron microscopy. PMID:28272523

Polymer-coated surface enhanced Raman scattering (SERS) gold nanoparticles for multiplexed labeling of chronic lymphocytic leukemia cells

NASA Astrophysics Data System (ADS)

MacLaughlin, Christina M.; Parker, Edward P. K.; Walker, Gilbert C.; Wang, Chen

2012-01-01

The ease and flexibility of functionalization and inherent light scattering properties of plasmonic nanoparticles make them suitable contrast agents for measurement of cell surface markers. Immunophenotyping of lymphoproliferative disorders is traditionally undertaken using fluorescence detection methods which have a number of limitations. Herein, surface-enhanced Raman scattering (SERS) gold nanoparticles conjugated to monoclonal antibodies are used for the selective targeting of CD molecules on the surface of chronic lymphocytic leukemia (CLL) cells. Raman-active reporters were physisorbed on to the surface of 60 nm spherical Au nanoparticles, the particles were coated with 5kDa polyethylene glycol (PEG) including functionalities for conjugation to monoclonal IgG1 antibodies. A novel method for quantifying the number of antibodies bound to SERS probes on an individual basis as opposed to obtaining averages from solution was demonstrated using metal dots in transmission electron microscopy (TEM). The specificity of the interaction between SERS probes and surface CD molecules of CLL cells was assessed using Raman spectroscopy and dark field microscopy. An in-depth study of SERS probe targeting to B lymphocyte marker CD20 was undertaken, and proof-of-concept targeting using different SERS nanoparticle dyes specific for cell surface CD19, CD45 and CD5 demonstrated using SERS spectroscopy.

Electronic and structural aspects of spin transitions observed by optical microscopy. The case of [Fe(ptz)6](BF4)2.

PubMed

Chong, Christian; Mishra, Haritosh; Boukheddaden, Kamel; Denise, Stéphane; Bouchez, Guillaume; Collet, Eric; Ameline, Jean-Claude; Naik, Anil D; Garcia, Yann; Varret, François

2010-02-11

The colorimetric analysis of images recorded with an optical microscope during the onset of the spin crossover transformation allows monitoring separately the involved electronic and structural aspects, through the separation of resonant absorption and scattering effects. Complementary information can also be obtained by using the polarized modes of the microscope. These potentialities are illustrated by the observation of [Fe(ptz)(6)](BF(4))(2) single crystals during the onset of the thermal transitions in the 110-140 K range. We characterized the interplay between the electronic (HS <--> LS) and structural (order <--> disorder) transformations. Elastic stresses and mechanical effects (hopping, self-cleavage) generated by the volume change upon electronic transition are also illustrated, with their impact on the photoswitching properties of the crystals.

Ultrastructural and x-ray microanalytical observations of minocycline-related hyperpigmentation of the skin

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

Sato, S.; Murphy, G.F.; Bernhard, J.D.

1981-09-01

In order to elucidate the nature and distribution of the pigment responsible for the circumscribed blue-black cutaneous hyperpigmentation occurring after administration of minocycline hydrochloride, transmission electron microscopy and energy-dispersive electron x-ray microanalysis were performed on lesional skin. Ultrastructural observations demonstrated electron-dense iron-containing particles either incorporated into a variety of siderosomes, within dermal histiocytes, free within the cytoplasm, or, rarely, scattered among dermal collagen fibers. Electron x-ray microanalysis confirmed iron content present within these particles. Although siderosomal inclusions contained occasional melanosome complexes, the degree of deposition of electron-dense iron-containing particles in dermal histiocytes seemed to be primarily responsible for the blue-blackmore » discoloration of the skin. The present study is an investigation of the structure and composition of the pigment responsible for minocycline-related cutaneous hyperpigmentation.« less

Visualizing buried silicon atoms at the Cd-Si(111)-7 ×7 interface with localized electrons

NASA Astrophysics Data System (ADS)

Tao, Min-Long; Xiao, Hua-Fang; Sun, Kai; Tu, Yu-Bing; Yuan, Hong-Kuan; Xiong, Zu-Hong; Wang, Jun-Zhong; Xue, Qi-Kun

2017-09-01

We report the atomic-scale imaging of the buried Cd-Si(111)-7 ×7 interface with a low temperature scanning tunneling microscopy (STM). The Cd(0001) films grown on Si(111)-7 ×7 reveal the electronic growth mode, and manifest a series of quantum-well states. In the low-bias STM images, not only the 7 ×7 reconstruction but also individual Si adatoms buried by thick Cd islands are clearly visible. The two successive layers of Cd islands exhibit the distinct contrasts due to the quantum size effect. Moreover, we found a small gap appeared at Fermi level owing to the Anderson localization induced by interface scattering. The perfect transparency of Cd films can be attributed to the anisotropic electron motion, i.e., lateral electron localization and transverse motion like free-electron.

Chemical and morphological characterization of III-V strained layered heterostructures

NASA Astrophysics Data System (ADS)

Gray, Allen Lindsay

This dissertation describes investigations into the chemical and morphological characterization of III-V strained layered heterostructures by high-resolution x-ray diffraction. The purpose of this work is two-fold. The first was to use high-resolution x-ray diffraction coupled with transmission electron microscopy to characterize structurally a quaternary AlGaAsSb/InGaAsSb multiple quantum well heterostructure laser device. A method for uniquely determining the chemical composition of the strain quaternary quantum well, information previously thought to be unattainable using high resolution x-ray diffraction is thoroughly described. The misconception that high-resolution x-ray diffraction can separately find the well and barrier thickness of a multi-quantum well from the pendellosung fringe spacing is corrected, and thus the need for transmission electron microscopy is motivated. Computer simulations show that the key in finding the well composition is the intensity of the -3rd order satellite peaks in the diffraction pattern. The second part of this work addresses the evolution of strain relief in metastable multi-period InGaAs/GaAs multi-layered structures by high-resolution x-ray reciprocal space maps. Results are accompanied by transmission electron and differential contrast microscopy. The evolution of strain relief is tracked from a coherent "pseudomorphic" growth to a dislocated state as a function of period number by examining the x-ray diffuse scatter emanating from the average composition (zeroth-order) of the multi-layer. Relaxation is determined from the relative positions of the substrate with respect to the zeroth-order peak. For the low period number, the diffuse scatter from the multi-layer structure region arises from periodic, coherent crystallites. For the intermediate period number, the displacement fields around the multi-layer structure region transition to random coherent crystallites. At the higher period number, displacement fields of overlapping dislocations from relaxation of the random crystallites cause the initial stages of relaxation of the multi-layer structure. At the highest period number studied, relaxation of the multi-layer structure becomes bi-modal characterized by overlapping dislocations caused by mosaic block relaxation and periodically spaced misfit dislocations formed by 60°-type dislocations. The relaxation of the multi-layer structure has an exponential dependence on the diffuse scatter length-scale, which is shown to be a sensitive measure of the onset of relaxation.

Hierarchically assembled Au microspheres and sea urchin-like architectures: formation mechanism and SERS study

NASA Astrophysics Data System (ADS)

Wang, Xiansong; Yang, Da-Peng; Huang, Peng; Li, Min; Li, Chao; Chen, Di; Cui, Daxiang

2012-11-01

The hierarchically assembled Au microspheres/sea urchin-like structures have been synthesized in aqueous solution at room temperature with and without proteins (bovine serum albumin, BSA) as mediators. The average diameter of an individual Au microsphere is 300-600 nm, which is composed of some compact nanoparticles with an average diameter of about 15 nm. Meanwhile, the sea urchin-like Au architecture exhibits an average diameter of 600-800 nm, which is made up of some nanopricks with an average length of 100-200 nm. These products are characterized by means of scanning electron microscopy (SEM), X-ray diffraction (XRD) and transmission electronic microscopy (TEM). It is found that the BSA and ascorbic acid (AA) have great effects on the morphology of the resulting products. Two different growth mechanisms are proposed. The study on surface enhanced Raman scattering (SERS) activities is also carried out between Au microspheres and Au sea urchin-like architectures. It is found that Au urchin-like architectures possess much higher SERS activity than the Au microspheres. Our work may shed light on the design and synthesis of hierarchically self-assembled 3D micro/nano-architectures for SERS, catalysis and biosensors.The hierarchically assembled Au microspheres/sea urchin-like structures have been synthesized in aqueous solution at room temperature with and without proteins (bovine serum albumin, BSA) as mediators. The average diameter of an individual Au microsphere is 300-600 nm, which is composed of some compact nanoparticles with an average diameter of about 15 nm. Meanwhile, the sea urchin-like Au architecture exhibits an average diameter of 600-800 nm, which is made up of some nanopricks with an average length of 100-200 nm. These products are characterized by means of scanning electron microscopy (SEM), X-ray diffraction (XRD) and transmission electronic microscopy (TEM). It is found that the BSA and ascorbic acid (AA) have great effects on the morphology of the resulting products. Two different growth mechanisms are proposed. The study on surface enhanced Raman scattering (SERS) activities is also carried out between Au microspheres and Au sea urchin-like architectures. It is found that Au urchin-like architectures possess much higher SERS activity than the Au microspheres. Our work may shed light on the design and synthesis of hierarchically self-assembled 3D micro/nano-architectures for SERS, catalysis and biosensors. Electronic supplementary information (ESI) available. See DOI: 10.1039/c2nr32405a

Periodic disorder along ramie cellulose microfibrils.

PubMed

Nishiyama, Yoshiharu; Kim, Ung-Jin; Kim, Dae-Young; Katsumata, Kyoko S; May, Roland P; Langan, Paul

2003-01-01

Small angle neutron scattering studies have been carried out on cellulose fibers from ramie and Populus maximowicii (cotton wood). Labile hydrogen atoms were replaced by deuterium atoms, in water-accessible disordered regions of the fibers, to increase the neutron scattering contrast between the disordered and crystalline regions. A meridional Bragg reflection, corresponding to a longitudinal periodicity of 150 nm, was observed when scattering collected from hydrogenated and deuterated dry ramie fibers was subtracted. No Bragg reflection was observed with the cotton wood fibers, probably because of lower orientation of the microfibrils in the cell wall. The ramie fibers were then subjected to electron microscopy, acid hydrolysis, gel permeation chromatography, and viscosity studies. The leveling off degree of polymerization (LODP) of the hydrolyzed samples matched exactly the periodicity observed in the diffraction studies. The weight loss related to the LODP was only about 1.5%, and thus, the microfibrils can be considered to have 4-5 disordered residues every 300 residues.

Reflectance of topologically disordered photonic-crystal films

NASA Astrophysics Data System (ADS)

Vigneron, Jean-Pol; Lousse, Virginie M.; Biro, Laszlo P.; Vertesy, Zofia; Balint, Zolt

2005-04-01

Periodicity implies the creation of discretely diffracted beams while various departures from periodicity lead to broadened scattering angles. This effect is investigated for disturbed lattices exhibiting randomly varying periods. In the Born approximation, the diffused reflection is shown to be related to a pair correlation function constructed from the distribution of the film scattering power. The technique is first applied to a natural photonic crystal found on the ventral side of the wings of the butterfly Cyanophrys remus, where scanning electron microscopy reveals the formation of polycrystalline photonic structures. Second, the disorder in the distribution of the cross-ribs on the scales another butterfly, Lycaena virgaureae, is investigated. The irregular arrangement of scatterers found in chitin structure of this insect produces light reflection in the long-wavelength part of the visible range, with a quite unusual broad directionality. The use of the pair correlation function allows to propose estimates of the diffusive spreading in these very different systems.

Suppression of Quasiparticle Scattering Signals in Bilayer Graphene Due to Layer Polarization and Destructive Interference

NASA Astrophysics Data System (ADS)

Jolie, Wouter; Lux, Jonathan; Pörtner, Mathias; Dombrowski, Daniela; Herbig, Charlotte; Knispel, Timo; Simon, Sabina; Michely, Thomas; Rosch, Achim; Busse, Carsten

2018-03-01

We study chemically gated bilayer graphene using scanning tunneling microscopy and spectroscopy complemented by tight-binding calculations. Gating is achieved by intercalating Cs between bilayer graphene and Ir(111), thereby shifting the conduction band minima below the chemical potential. Scattering between electronic states (both intraband and interband) is detected via quasiparticle interference. However, not all expected processes are visible in our experiment. We uncover two general effects causing this suppression: first, intercalation leads to an asymmetrical distribution of the states within the two layers, which significantly reduces the scanning tunneling spectroscopy signal of standing waves mainly present in the lower layer; second, forward scattering processes, connecting points on the constant energy contours with parallel velocities, do not produce pronounced standing waves due to destructive interference. We present a theory to describe the interference signal for a general n -band material.

Cavity-enhanced Raman microscopy of individual carbon nanotubes

PubMed Central

Hümmer, Thomas; Noe, Jonathan; Hofmann, Matthias S.; Hänsch, Theodor W.; Högele, Alexander; Hunger, David

2016-01-01

Raman spectroscopy reveals chemically specific information and provides label-free insight into the molecular world. However, the signals are intrinsically weak and call for enhancement techniques. Here, we demonstrate Purcell enhancement of Raman scattering in a tunable high-finesse microcavity, and utilize it for molecular diagnostics by combined Raman and absorption imaging. Studying individual single-wall carbon nanotubes, we identify crucial structural parameters such as nanotube radius, electronic structure and extinction cross-section. We observe a 320-times enhanced Raman scattering spectral density and an effective Purcell factor of 6.2, together with a collection efficiency of 60%. Potential for significantly higher enhancement, quantitative signals, inherent spectral filtering and absence of intrinsic background in cavity-vacuum stimulated Raman scattering render the technique a promising tool for molecular imaging. Furthermore, cavity-enhanced Raman transitions involving localized excitons could potentially be used for gaining quantum control over nanomechanical motion and open a route for molecular cavity optomechanics. PMID:27402165

Suppression of Quasiparticle Scattering Signals in Bilayer Graphene Due to Layer Polarization and Destructive Interference.

PubMed

Jolie, Wouter; Lux, Jonathan; Pörtner, Mathias; Dombrowski, Daniela; Herbig, Charlotte; Knispel, Timo; Simon, Sabina; Michely, Thomas; Rosch, Achim; Busse, Carsten

2018-03-09

We study chemically gated bilayer graphene using scanning tunneling microscopy and spectroscopy complemented by tight-binding calculations. Gating is achieved by intercalating Cs between bilayer graphene and Ir(111), thereby shifting the conduction band minima below the chemical potential. Scattering between electronic states (both intraband and interband) is detected via quasiparticle interference. However, not all expected processes are visible in our experiment. We uncover two general effects causing this suppression: first, intercalation leads to an asymmetrical distribution of the states within the two layers, which significantly reduces the scanning tunneling spectroscopy signal of standing waves mainly present in the lower layer; second, forward scattering processes, connecting points on the constant energy contours with parallel velocities, do not produce pronounced standing waves due to destructive interference. We present a theory to describe the interference signal for a general n-band material.

Analysis of improvement in performance and design parameters for enhancing resolution in an atmospheric scanning electron microscope.

PubMed

Yoon, Yeo Hun; Kim, Seung Jae; Kim, Dong Hwan

2015-12-01

The scanning electron microscope is used in various fields to go beyond diffraction limits of the optical microscope. However, the electron pathway should be conducted in a vacuum so as not to scatter electrons. The pretreatment of the sample is needed for use in the vacuum. To directly observe large and fully hydrophilic samples without pretreatment, the atmospheric scanning electron microscope (ASEM) is needed. We developed an electron filter unit and an electron detector unit for implementation of the ASEM. The key of the electron filter unit is that electrons are transmitted while air molecules remain untransmitted through the unit. The electron detector unit collected the backscattered electrons. We conducted experiments using the selected materials with Havar foil, carbon film and SiN film. © 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.

Isolation and characterization of nanocrystalline cellulose from roselle-derived microcrystalline cellulose.

PubMed

Kian, Lau Kia; Jawaid, Mohammad; Ariffin, Hidayah; Karim, Zoheb

2018-07-15

Roselle fiber is a renewable and sustainable agricultural waste enriched with cellulose polysaccharides. The isolation of Nanocrystalline cellulose (NCC) from roselle-derived microcrystalline cellulose (MCC) is an alternative approach to recover the agricultural roselle plant residue. In the present study, acid hydrolysis with different reaction time was carried out to degrade the roselle-derived MCC to form NCC. The characterizations of isolated NCC were conducted through Fourier Transform Infrared Ray (FTIR), Transmission Electron Microscopy (TEM), Field Emission Scanning Electron Microscopy (FESEM), Atomic Force Microscopy (AFM), Dynamic Light Scattering (DLS), Energy Dispersive Spectroscopy (EDS), X-ray Diffraction (XRD), Thermogravimetric Analysis (TGA) and Differential Scanning Calorimetry (DSC). As evaluated from the performed morphological investigations, the needle-like shape NCC nanostructures were observed under TEM and AFM microscopy studies, while irregular rod-like shape of NCC was observed under FESEM analysis. With 60min hydrolysis time, XRD analysis demonstrated the highest NCC crystallinity degree with 79.5%. In thermal analysis by TGA and DSC, the shorter hydrolysis time tended to produce NCC with higher thermal stability. Thus, the isolated NCC from roselle-derived MCC has high potential to be used in application of pharmaceutical and biomedical fields for nanocomposite fabrication. Copyright © 2018 Elsevier B.V. All rights reserved.

Scanning electron microscope measurement of width and shape of 10nm patterned lines using a JMONSEL-modeled library.

PubMed

Villarrubia, J S; Vladár, A E; Ming, B; Kline, R J; Sunday, D F; Chawla, J S; List, S

2015-07-01

The width and shape of 10nm to 12 nm wide lithographically patterned SiO2 lines were measured in the scanning electron microscope by fitting the measured intensity vs. position to a physics-based model in which the lines' widths and shapes are parameters. The approximately 32 nm pitch sample was patterned at Intel using a state-of-the-art pitch quartering process. Their narrow widths and asymmetrical shapes are representative of near-future generation transistor gates. These pose a challenge: the narrowness because electrons landing near one edge may scatter out of the other, so that the intensity profile at each edge becomes width-dependent, and the asymmetry because the shape requires more parameters to describe and measure. Modeling was performed by JMONSEL (Java Monte Carlo Simulation of Secondary Electrons), which produces a predicted yield vs. position for a given sample shape and composition. The simulator produces a library of predicted profiles for varying sample geometry. Shape parameter values are adjusted until interpolation of the library with those values best matches the measured image. Profiles thereby determined agreed with those determined by transmission electron microscopy and critical dimension small-angle x-ray scattering to better than 1 nm. Published by Elsevier B.V.

Nonlinear plasmonic imaging techniques and their biological applications

NASA Astrophysics Data System (ADS)

Deka, Gitanjal; Sun, Chi-Kuang; Fujita, Katsumasa; Chu, Shi-Wei

2017-01-01

Nonlinear optics, when combined with microscopy, is known to provide advantages including novel contrast, deep tissue observation, and minimal invasiveness. In addition, special nonlinearities, such as switch on/off and saturation, can enhance the spatial resolution below the diffraction limit, revolutionizing the field of optical microscopy. These nonlinear imaging techniques are extremely useful for biological studies on various scales from molecules to cells to tissues. Nevertheless, in most cases, nonlinear optical interaction requires strong illumination, typically at least gigawatts per square centimeter intensity. Such strong illumination can cause significant phototoxicity or even photodamage to fragile biological samples. Therefore, it is highly desirable to find mechanisms that allow the reduction of illumination intensity. Surface plasmon, which is the collective oscillation of electrons in metal under light excitation, is capable of significantly enhancing the local field around the metal nanostructures and thus boosting up the efficiency of nonlinear optical interactions of the surrounding materials or of the metal itself. In this mini-review, we discuss the recent progress of plasmonics in nonlinear optical microscopy with a special focus on biological applications. The advancement of nonlinear imaging modalities (including incoherent/coherent Raman scattering, two/three-photon luminescence, and second/third harmonic generations that have been amalgamated with plasmonics), as well as the novel subdiffraction limit imaging techniques based on nonlinear behaviors of plasmonic scattering, is addressed.

Dimensions and Global Twist of Single-Layer DNA Origami Measured by Small-Angle X-ray Scattering.

PubMed

Baker, Matthew A B; Tuckwell, Andrew J; Berengut, Jonathan F; Bath, Jonathan; Benn, Florence; Duff, Anthony P; Whitten, Andrew E; Dunn, Katherine E; Hynson, Robert M; Turberfield, Andrew J; Lee, Lawrence K

2018-06-04

The rational design of complementary DNA sequences can be used to create nanostructures that self-assemble with nanometer precision. DNA nanostructures have been imaged by atomic force microscopy and electron microscopy. Small-angle X-ray scattering (SAXS) provides complementary structural information on the ensemble-averaged state of DNA nanostructures in solution. Here we demonstrate that SAXS can distinguish between different single-layer DNA origami tiles that look identical when immobilized on a mica surface and imaged with atomic force microscopy. We use SAXS to quantify the magnitude of global twist of DNA origami tiles with different crossover periodicities: these measurements highlight the extreme structural sensitivity of single-layer origami to the location of strand crossovers. We also use SAXS to quantify the distance between pairs of gold nanoparticles tethered to specific locations on a DNA origami tile and use this method to measure the overall dimensions and geometry of the DNA nanostructure in solution. Finally, we use indirect Fourier methods, which have long been used for the interpretation of SAXS data from biomolecules, to measure the distance between DNA helix pairs in a DNA origami nanotube. Together, these results provide important methodological advances in the use of SAXS to analyze DNA nanostructures in solution and insights into the structures of single-layer DNA origami.

Electron radiography

DOEpatents

Merrill, Frank E.; Morris, Christopher

2005-05-17

A system capable of performing radiography using a beam of electrons. Diffuser means receive a beam of electrons and diffuse the electrons before they enter first matching quadrupoles where the diffused electrons are focused prior to the diffused electrons entering an object. First imaging quadrupoles receive the focused diffused electrons after the focused diffused electrons have been scattered by the object for focusing the scattered electrons. Collimator means receive the scattered electrons and remove scattered electrons that have scattered to large angles. Second imaging quadrupoles receive the collimated scattered electrons and refocus the collimated scattered electrons and map the focused collimated scattered electrons to transverse locations on an image plane representative of the electrons' positions in the object.

Development of structure in natural silk spinning and poly(vinyl alcohol) hydrogel formation

NASA Astrophysics Data System (ADS)

Willcox, Patricia Jeanene

This research involves the characterization of structure and structure formation in aqueous systems. Particularly, these studies investigate the effect of various processing variables on the structure formation that occurs upon conversion from aqueous solution to fiber or hydrogel. The two processes studied include natural silk fiber spinning and physical gelation of poly(vinyl alcohol), PVOH, in water. The techniques employed combine cryogenic technology for sample preparation and direct observation by transmission electron microscopy with electron diffraction, atomic force microscopy, optical rheometry, X-ray scattering and optical microscopy. In order to explore the full range of structure formation in natural silk spinning, studies are conducted in vivo and in vitro. In vivo structural investigations are accomplished through the cryogenic quenching and subsequent microtoming of live silk-spinning animals, Nephila clavipes (spider) and Bombyx mori (silkworm). Observations made using transmission electron microscopy, electron diffraction and atomic force microscopy indicate a cholesteric liquid crystalline mesophase of aqueous silk fibroin in both species. The mechanism of structure formation in solution is studied in vitro using optical rheometry on aqueous solutions made from regenerated Bombyx mori cocoon silk. Concentrated solutions exhibit birefringence under flow, with a wormlike conformation of the silk molecules in concentrated salt solution. Changes in salt concentration and pH of the aqueous silk solutions result in differing degrees of alignment and aggregation. These results suggest that structural control in the natural silk spinning process is accomplished by chemical manipulation of the electrostatic interactions and hydrogen bonding between chains. Application of cryogenic methods in transmission electron microscopy also provides a unique look at hydration-dependent structures in gels of poly(vinyl alcohol) produced by freeze-thaw processing. Morphologies ranging from circular pores to fibrillar networks are observed in gels formed from aqueous PVOH solutions subjected to cycles of freezing and thawing. These morphologies can be directly associated with the progressive nature of the mechanism of gelation as it proceeds from liquid-liquid phase separation to crystallization with increased cycling. A comparison of the structures produced by cycling and by aging suggests that there is a similarity in structural changes, but a superposition of the effects of cycling and aging is not possible.

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.

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

Wilbur, Jeffrey D.; Gomez, Enrique D.; Ellsworth, Mark W.

A procedure for creating samples that can be repeatedly cycled between weakly aligned and strongly aligned states is described. Poly(styrene-b-isoprene) block copolymer samples were first shear-aligned and then cross-linked using a high energy electron beam. Samples with more than 1.0 cross-links per chain on average showed almost complete recovery of their initial alignment state even after 20 cycles of heating above the order–disorder transition temperature of the un-cross-linked block copolymer. Samples with 1.1 cross-links per chain, which showed over 90% loss of alignment on heating and almost 100% recovery of alignment on cooling, provided the best example of a reversiblemore » aligned-to-unaligned transition. Samples with lower cross-linking densities exhibited irreversible loss of alignment upon heating, while those with higher cross-linking densities exhibited less than 90% loss of alignment upon heating. Alignment was quantified by a technique that we call two color depolarized light scattering (TCDLS), an extension of the traditional depolarized light scattering experiment used to determine the state of order in block copolymers. Qualitative confirmation of our interpretation of TCDLS data was obtained by small-angle X-ray scattering and transmission electron microscopy.« less

Out-of-plane electron transport in finite layer MoS2

NASA Astrophysics Data System (ADS)

Holzapfel, R.; Weber, J.; Lukashev, P. V.; Stollenwerk, A. J.

2018-05-01

Ballistic electron emission microscopy (BEEM) has been used to study the processes affecting electron transport along the [0001] direction of finite layer MoS2 flakes deposited onto the surface of Au/Si(001) Schottky diodes. Prominent features present in the differential spectra from the MoS2 flakes are consistent with the density of states of finite layer MoS2 calculated using density functional theory. The ability to observe the electronic structure of the MoS2 appears to be due to the relatively smooth density of states of Si in this energy range and a substantial amount of elastic or quasi-elastic scattering along the MoS2/Au/Si(001) path. Demonstration of these measurements using BEEM suggests that this technique could potentially be used to study electron transport through van der Waals heterostructures, with applications in a number of electronic devices.

Ultrafast studies of coexisting electronic order in cuprate superconductors

NASA Astrophysics Data System (ADS)

Hinton, James; Thewalt, Eric; Alpichshev, Zhanybek; Sternbach, Aaron; McLeod, Alex; Ji, L.; Veit, Mike; Dorrow, Chelsey; Koralek, Jake; Xhao, Xudong; Barisic, Neven; Kemper, Alexander; Gedik, Nuh; Greven, Martin; Basov, Dimitri; Orenstein, Joe

The cuprate family of high temperature superconductors displays a variety of electronic phases which emerge when charge carriers are added to the antiferromagnetic parent compound. These electronic phases are characterized by subtle differences in the low energy electronic excitations. Ultrafast time-resolved reflectivity (TRR) provides an ideal tool for investigating the cuprate phase diagram, as small changes in the electronic structure can produce significant contrast in the non-equilibrium reflectivity. Here we present TRR measurements of cuprate superconductors, focusing on the model single-layer cuprate HgBa2CuO4+δ. We observe a cusp-like feature in the quasiparticle lifetime near the superconducting transition temperature Tc. This feature can be understood using a model of coherently-mixed charge-density wave and superconducting pairing. We propose extending this technique to the nanoscale using ultrafast scattering scanning near-field microscopy (u-SNOM). This will allow us to explore how these electronic phases coexist and compete in real-space.

Water-assisted growth of graphene on carbon nanotubes by the chemical vapor deposition method.

PubMed

Feng, Jian-Min; Dai, Ye-Jing

2013-05-21

Combining carbon nanotubes (CNTs) with graphene has been proved to be a feasible method for improving the performance of graphene for some practical applications. This paper reports a water-assisted route to grow graphene on CNTs from ferrocene and thiophene dissolved in ethanol by the chemical vapor deposition method in an argon flow. A double injection technique was used to separately inject ethanol solution and water for the preparation of graphene/CNTs. First, CNTs were prepared from ethanol solution and water. The injection of ethanol solution was suspended and water alone was injected into the reactor to etch the CNTs. Thereafter, ethanol solution was injected along with water, which is the key factor in obtaining graphene/CNTs. Transmission electron microscopy, scanning electron microscopy, X-ray diffraction, and Raman scattering analyses confirmed that the products were the hybrid materials of graphene/CNTs. X-ray photo-electron spectroscopy analysis showed the presence of oxygen rich functional groups on the surface of the graphene/CNTs. Given the activity of the graphene/CNT surface, CdS quantum dots adhered onto it uniformly through simple mechanical mixing.

Effect of Pulse Detonation-Plasma Technology Treatment on T8 Steel Microstructures

NASA Astrophysics Data System (ADS)

Yu, Jiuming; Zhang, Linwei; Liu, Keming; Lu, Lei; Lu, Deping; Zhou, Haitao

2017-12-01

T8 steel surfaces were treated by pulse detonation-plasma technology (PDT) at capacitance values of 600, 800, and 1000 μF, and the effects of PDT were analyzed using x-ray diffraction, scanning electron microscopy, transmission electron microscopy, electron back-scattered diffraction, and micro-hardness tester and friction wear tester. The surface of T8 steel is first smoothed out, and then, craters are formed due to the inhomogeneity of the PDT energy and targeting during PDT treatment. The initial martensite in the T8 steel surface layer changes to austenite, and Fe3N is formed due to nitriding. The thickness of the modified layer, which is composed of columnar and fine grain structures, increases with the increasing capacity. Preferential orientation occurred in the {110} 〈 001 〉 direction in the modified layer, and the number of low-angle grain boundaries increased significantly after PDT treatment. The micro-hardness and wear resistance of the T8 steel was improved by PDT treatment, even doubled after the treatment with the capacitance of 1000 μF.

Mass Determination of Rous Sarcoma Virus Virions by Scanning Transmission Electron Microscopy

PubMed Central

Vogt, Volker M.; Simon, Martha N.

1999-01-01

The internal structural protein of retroviruses, Gag, comprises most of the mass of the virion, and Gag itself can give rise to virus-like particles when expressed in appropriate cells. Previously the stoichiometry of Gag in virions was inferred from indirect measurements carried out 2 decades ago. We now have directly determined the masses of individual particles of the prototypic avian retrovirus, Rous sarcoma virus (RSV), by using scanning transmission electron microscopy. In this technique, the number of scattered electrons in the dark-field image integrated over an individual freeze-dried virus particle on a grid is directly proportional to its mass. The RSV virions had a mean mass of 2.5 × 108 Da, corresponding to about 1,500 Gag molecules per virion. The population of virions was not homogeneous, with about one-third to two-thirds of the virions deviating from the mean by more than 10% of the mass in two respective preparations. The mean masses for virions carrying genomes of 7.4 or 9.3 kb were indistinguishable, suggesting that mass variability is not due to differences in RNA incorporation. PMID:10400808

Inter-particle interaction dependent evaporation-induced assembly in contact-free micro-colloidal droplets

NASA Astrophysics Data System (ADS)

Sen, Debasis; Biswas, Priyanka; Melo, J. S.

2018-04-01

Evaporation-induced assembly of constituent particles in tiny dispersion droplet allows an efficient way to realize nano-structured micro-granules with potential for various applications. Morphology of the granules, obtained by such one-step dispersion to granular transformation, is decided by several physicochemical conditions. Here we demonstrate that the inter-particle interaction plays a crucial role in deciding the assembled morphology. Resultant granules are investigated by complementary techniques, Electron microscopy and small-angle scattering.

Thermoplastic/Nanotube Composite Fibers

NASA Astrophysics Data System (ADS)

Haggenmueller, Reto; Fischer, John; Winey, Karen

2000-03-01

A combination of solvent casting and melt mixing methods are used to compound selected thermoplastics with single-wall carbon nanotubes. Subsequently, melt extrusion is used to form thermoplastic-nanotube composite fibers. The structural characteristics are investigated by electron microscopy and x-ray scattering methods. In addition the electrical, thermal and mechanical properties were measured. Correlations are sought between the viscoelastic properties of the compounded materials, the nanotube loading and elongation ratio after spinning, and the properties of the resultant fibers.

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

Alenaizi, R.; Radiman, S.; Mohamed, F.

The morphology of vesicles system with defined particle size and shape is one of interest in our technical applications. Here we have used dynamic light scattering technique and transmission electron microscopy for structural characterization of N-dimethylglycine Betaine with 5-cholesten-3β-ol vesicles in aqueous solutions. An isotropic one phase region is found in the very diluted regions depending on Betaine/Cholesterol ratio. The isotropic region was stable for more than 3 months at room temperature, with monodispersed unilamellar vesicles ∼ 300nm.

Biomimetic synthesis of chiral erbium-doped silver/peptide/silica core-shell nanoparticles (ESPN)

NASA Astrophysics Data System (ADS)

Mantion, Alexandre; Graf, Philipp; Florea, Ileana; Haase, Andrea; Thünemann, Andreas F.; Mašić, Admir; Ersen, Ovidiu; Rabu, Pierre; Meier, Wolfgang; Luch, Andreas; Taubert, Andreas

2011-12-01

Peptide-modified silver nanoparticles have been coated with an erbium-doped silica layer using a method inspired by silica biomineralization. Electron microscopy and small-angle X-ray scattering confirm the presence of an Ag/peptide core and silica shell. The erbium is present as small Er2O3 particles in and on the silica shell. Raman, IR, UV-Vis, and circular dichroism spectroscopies show that the peptide is still present after shell formation and the nanoparticles conserve a chiral plasmon resonance. Magnetic measurements find a paramagnetic behavior. In vitro tests using a macrophage cell line model show that the resulting multicomponent nanoparticles have a low toxicity for macrophages, even on partial dissolution of the silica shell.Peptide-modified silver nanoparticles have been coated with an erbium-doped silica layer using a method inspired by silica biomineralization. Electron microscopy and small-angle X-ray scattering confirm the presence of an Ag/peptide core and silica shell. The erbium is present as small Er2O3 particles in and on the silica shell. Raman, IR, UV-Vis, and circular dichroism spectroscopies show that the peptide is still present after shell formation and the nanoparticles conserve a chiral plasmon resonance. Magnetic measurements find a paramagnetic behavior. In vitro tests using a macrophage cell line model show that the resulting multicomponent nanoparticles have a low toxicity for macrophages, even on partial dissolution of the silica shell. Electronic supplementary information (ESI) available: Figures S1 to S12, Tables S1 and S2. See DOI: 10.1039/c1nr10930h

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

Thuy, Nguyen Thanh, E-mail: ngtthuy02@yahoo.com; Huy, Tran Quang, E-mail: huytq@nihe.org.vn; Nga, Phan Thi

We describe the ultrastructure of the NamDinh virus (NDiV), a new member of the order Nidovirales grown in the C6/36 mosquito cell line. Uninfected and NDiV-infected cells were investigated by electron microscopy 24–48 h after infection. The results show that the viral nucleocapsid-like particles form clusters concentrated in the vacuoles, the endoplasmic reticulum, and are scattered in the cytoplasm. Mature virions of NDiV were released as budding particles on the cell surface where viral components appear to lie beneath and along the plasma membrane. Free homogeneous virus particles were obtained by ultracentrifugation on sucrose gradients of culture fluids. The sizemore » of the round-shaped particles with a complete internal structure was 80 nm in diameter. This is the first study to provide information on the morphogenesis and ultrastructure of the first insect nidovirus NDiV, a missing evolutionary link in the emergence of the viruses with the largest RNA genomes. - Highlights: • NamDinh virus (NDiV), a new member of the order Nidovirales was tested in cultured cell line. • The morphogenesis and ultrastructure of NDiV were investigated by electron microscopy. • The viral nucleocapsid-like particles clustered and scattered in the cytoplasm. • NDiVs were released as budding particles on the cell surface. • The size of the viral particles with a complete internal structure was 80 nm in diameter.« less

Morphologic and proteomic characterization of exosomes released by cultured extravillous trophoblast cells

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

Atay, Safinur; Gercel-Taylor, Cicek; Kesimer, Mehmet

Exosomes represent an important intercellular communication vehicle, mediating events essential for the decidual microenvironment. While we have demonstrated exosome induction of pro-inflammatory cytokines, to date, no extensive characterization of trophoblast-derived exosomes has been provided. Our objective was to provide a morphologic and proteomic characterization of these exosomes. Exosomes were isolated from the conditioned media of Swan71 human trophoblast cells by ultrafiltration and ultracentrifugation. These were analyzed for density (sucrose density gradient centrifugation), morphology (electron microscopy), size (dynamic light scattering) and protein composition (Ion Trap mass spectrometry and western immunoblotting). Based on density gradient centrifugation, microvesicles from Sw71 cells exhibit amore » density between 1.134 and 1.173 g/ml. Electron microscopy demonstrated that microvesicles from Sw71 cells exhibit the characteristic cup-shaped morphology of exosomes. Dynamic light scattering showed a bell-shaped curve, indicating a homogeneous population with a mean size of 165 nm {+-} 0.5 nm. Ion Trap mass spectrometry demonstrated the presence of exosome marker proteins (including CD81, Alix, cytoskeleton related proteins, and Rab family). The MS results were confirmed by western immunoblotting. Based on morphology, density, size and protein composition, we defined the release of exosomes from extravillous trophoblast cells and provide their first extensive characterization. This characterization is essential in furthering our understanding of 'normal' early pregnancy.« less

Imaging secondary structure of individual amyloid fibrils of a β2-microglobulin fragment using near-field infrared spectroscopy.

PubMed

Paulite, Melissa; Fakhraai, Zahra; Li, Isaac T S; Gunari, Nikhil; Tanur, Adrienne E; Walker, Gilbert C

2011-05-18

Amyloid fibril diseases are characterized by the abnormal production of aggregated proteins and are associated with many types of neuro- and physically degenerative diseases. X-ray diffraction techniques, solid-state magic-angle spinning NMR spectroscopy, circular dichroism (CD) spectroscopy, and transmission electron microscopy studies have been utilized to detect and examine the chemical, electronic, material, and structural properties of amyloid fibrils at up to angstrom spatial resolution. However, X-ray diffraction studies require crystals of the fibril to be analyzed, while other techniques can only probe the bulk solution or solid samples. In the work reported here, apertureless near-field scanning infrared microscopy (ANSIM) was used to probe the secondary structure of individual amyloid fibrils made from an in vitro solution. Simultaneous topographic and infrared images of individual amyloid fibrils synthesized from the #21-31 peptide fragment of β(2)-microglobulin were acquired. Using this technique, IR spectra of the amyloid fibrils were obtained with a spatial resolution of less than 30 nm. It is observed that the experimental scattered field spectrum correlates strongly with that calculated using the far-field absorption spectrum. The near-field images of the amyloid fibrils exhibit much lower scattering of the IR radiation at approximately 1630 cm(-1). In addition, the near-field images also indicate that composition and/or structural variations among individual amyloid fibrils were present. © 2011 American Chemical Society

Viscoelasticity and structure of blood clots generated in-vitro by rheometry: A comparison between human, horse, rat, and camel.

PubMed

Dibiasi, Christoph; Plewka, Jacek; Ploszczanski, Leon; Glanz, Veronika; Lichtenegger, Helga; Windberger, Ursula

2018-04-14

Although the coagulation system is evolutionary well preserved, profound species differences exist in viscoelastic as well as in common laboratory tests of coagulation. Evaluating differences in clot formation and material characterisation of clots of four mammalian species on macro-, micro- and nanoscales by the means of rheometry, scanning electron microscopy (SEM) and small angle x-ray scattering (SAXS). Blood samples were collected from healthy human volunteers, laboratory rats (HL/LE inbred strain), warmblood horses and dromedary camels. Clot formation was observed by oscillating shear rheometry until plateau formation of the shear storage modulus G', at which point selected clots were prepared for scanning electron microscopy. SEM images were analysed for fibre diameter and fractal dimension. Additionally, scattering profiles for plasma and whole blood samples were obtained with SAXS. Viscoelasticity of clots showed great interspecies variation: clots of rats and horses exhibited shorter clotting times and higher G' plateau values, when compared to human clots. Camel clots showed unique clotting characteristics with no G' plateau formation in the timeframe observed. Less differentiating features were found with SEM and SAXS, although the rat fibre network appears to be more convoluted and dense, which resulted in a higher fractal dimension. Clotting kinetic differs between the species, which is not only of clinical interest, but could also be an important finding for animal models of blood coagulation.

Near-Field Imaging of Free Carriers in ZnO Nanowires with a Scanning Probe Tip Made of Heavily Doped Germanium

NASA Astrophysics Data System (ADS)

Sakat, Emilie; Giliberti, Valeria; Bollani, Monica; Notargiacomo, Andrea; Pea, Marialilia; Finazzi, Marco; Pellegrini, Giovanni; Hugonin, Jean-Paul; Weber-Bargioni, Alexander; Melli, Mauro; Sassolini, Simone; Cabrini, Stefano; Biagioni, Paolo; Ortolani, Michele; Baldassarre, Leonetta

2017-11-01

A novel scanning probe tip made of heavily doped semiconductor is fabricated and used instead of standard gold-coated tips in infrared scattering-type near-field microscopy. Midinfrared near-field microscopy experiments are conducted on ZnO nanowires with a lateral resolution better than 100 nm, using tips made of heavily electron-doped germanium with a plasma frequency in the midinfrared (plasma wavelength of 9.5 μ m ). Nanowires embedded in a dielectric matrix are imaged at two wavelengths, 11.3 and 8.0 μ m , above and below the plasma wavelength of the tips. An opposite sign of the imaging contrasts between the nanowire and the dielectric matrix is observed at the two infrared wavelengths, indicating a clear role of the free-electron plasma in the heavily doped germanium tip in building the imaging contrast. Electromagnetic simulations with a multispherical dipole model accounting for the finite size of the tip are well consistent with the experiments. By comparison of the simulated and measured imaging contrasts, an estimate for the local free-carrier density in the investigated ZnO nanowires in the low 1019 cm-3 range is retrieved. The results are benchmarked against the scattering intensity and phase maps obtained on the same sample with a gold-coated probe tip in pseudoheterodyne detection mode.

Accumulation and interparticle connections of triangular Ag-coated Au nanoprisms by oil-coating method for surface-enhanced Raman scattering applications

NASA Astrophysics Data System (ADS)

Noda, Yuta; Asaka, Toru; Fudouzi, Hiroshi; Hayakawa, Tomokatsu

2018-03-01

To examine the optical responses of surface-enhanced Raman scattering (SERS) for tuned plasmonic nanoparticles, triangular Ag-coated Au (Au@Ag) nanoprisms with different sizes were separately synthesized, which were well controlled in their size (edge-length) and localized surface plasmon resonance (LSPR) wavelength (69.0 ± 8.4 to 173.8 ± 25.6 nm in size and 662-943 nm in LSPR wavelength). The mechanism of Ag shell formation on the Au nanoprisms was also studied with scanning transmission electron microscopy-energy dispersive X-ray spectroscopy (STEM-EDS). The Au@Ag nanoprisms were immobilized by covering a colloidal solution containing the nanoprisms with silicone oil and evaporating the solvent in the oil (oil-coating method) so as to form a layer of accumulated plasmonic Au@Ag nanoprisms that had LSPR peak wavelengths tuned from 839 to 1182 nm. The accumulation conditions were analyzed by field-emission scanning electron microscopy (FE-SEM) and a Raman mapping technique. The Au@Ag nanoprisms under excitation at 632.8 nm exhibited higher SERS signals of rhodamine 6G, and SERS-mapped images of the novel immobilized films were obtained at different magnifications. It was concluded that accumulated Au@Ag nanoprisms undergoing tip-planar interconnections could produce enhanced local fields, resulting in higher SERS signals.

Engineered silica nanoparticles as additives in lubricant oils

PubMed Central

López, Teresa Díaz-Faes; González, Alfonso Fernández; Del Reguero, Ángel; Matos, María; Díaz-García, Marta E; Badía-Laíño, Rosana

2015-01-01

Silica nanoparticles (SiO2 NPs) synthesized by the sol–gel approach were engineered for size and surface properties by grafting hydrophobic chains to prevent their aggregation and facilitate their contact with the phase boundary, thus improving their dispersibility in lubricant base oils. The surface modification was performed by covalent binding of long chain alkyl functionalities using lauric acid and decanoyl chloride to the SiO2 NP surface. The hybrid SiO2 NPs were characterized by scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy, simultaneous differential thermal analysis, nuclear magnetic resonance and dynamic light scattering, while their dispersion in two base oils was studied by static multiple light scattering at low (0.01% w/v) and high (0.50%w/v) concentrations. The nature of the functional layer and the functionalization degree seemed to be directly involved in the stability of the suspensions. The potential use of the functional SiO2 NPs as lubricant additives in base oils, specially designed for being used in hydraulic circuits, has been outlined by analyzing the tribological properties of the dispersions. The dendritic structure of the external layer played a key role in the tribological characteristics of the material by reducing the friction coefficient and wear. These nanoparticles reduce drastically the waste of energy in friction processes and are more environmentally friendly than other additives. PMID:27877840

A menu of electron probes for optimising information from scanning transmission electron microscopy.

PubMed

Nguyen, D T; Findlay, S D; Etheridge, J

2018-01-01

We assess a selection of electron probes in terms of the spatial resolution with which information can be derived about the structure of a specimen, as opposed to the nominal image resolution. Using Ge [001] as a study case, we investigate the scattering dynamics of these probes and determine their relative merits in terms of two qualitative criteria: interaction volume and interpretability. This analysis provides a 'menu of probes' from which an optimum probe for tackling a given materials science question can be selected. Hollow cone, vortex and spherical wave fronts are considered, from unit cell to Ångstrom size, and for different defocus and specimen orientations. Copyright © 2017 Elsevier B.V. All rights reserved.

Combining Electronic and Geometric Effects of ZnO-Promoted Pt Nanocatalysts for Aqueous Phase Reforming of 1-Propanol

DOE PAGES

Lei, Yu; Lee, Sungsik; Low, Ke -Bin; ...

2016-04-26

Compared with Pt/Al 2O 3, sintering-resistant Pt nanoparticle catalysts promoted by ZnO significantly improved the reactivity and selectivity toward hydrogen formation in the aqueous phase reforming (APR) of 1-propanol. The improved performance was found to benefit from both the electronic and geometric effects of ZnO thin films. In situ small-angle X-ray scattering and scanning transmission electron microscopy showed that ZnO-promoted Pt possessed promising thermal stability under APR reaction conditions. In situ X-ray absorption spectroscopy showed clear charge transfer between ZnO and Pt nanoparticles. The improved reactivity and selectivity seemed to benefit from having both Pt-ZnO and Pt-Al 2O 3 interfaces.

Quantum Detection and Invisibility in Coherent Nanostructures

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

Fransson, J.

2010-04-28

We address quantum invisibility in the context of electronics in nanoscale quantum structures. In analogy with metamaterials, we use the freedom of design that quantum corrals provide and show that quantum mechanical objects can be hidden inside the corral, with respect to inelastic electron scattering spectroscopy in combination with scanning tunneling microscopy, and we propose a design strategy. A simple illustration of the invisibility is given in terms of an elliptic quantum corral containing a molecule, with a local vibrational mode, at one of the foci. Our work has implications to quantum information technology and presents new tools for nonlocalmore » quantum detection and distinguishing between different molecules.« less

Capturing the crystalline phase of two-dimensional nanocrystal superlattices in action.

PubMed

Jiang, Zhang; Lin, Xiao-Min; Sprung, Michael; Narayanan, Suresh; Wang, Jin

2010-03-10

Critical photonic, electronic, and magnetic applications of two-dimensional nanocrystal superlattices often require nanostructures in perfect single-crystal phases with long-range order and limited defects. Here we discovered a crystalline phase with quasi-long-range positional order for two-dimensional nanocrystal superlattice domains self-assembled at the liquid-air interface during droplet evaporation, using in situ time-resolved X-ray scattering along with rigorous theories on two dimensional crystal structures. Surprisingly, it was observed that drying these superlattice domains preserved only an orientational order but not a long-range positional order, also supported by quantitative analysis of transmission electron microscopy images.

Growth and characterization of manganese doped gallium nitride nanowires.

PubMed

Kumar, V Suresh; Kesavamoorthy, R; Kumar, J

2008-08-01

Manganese doped GaN nanowires have been grown by chemical vapour transport method on sapphire (0001) substrates in the temperature range of 800-1050 degrees C. The surface features of nanowires have been investigated using Scanning Electron Microscopy (SEM), Energy Dispersive X-ray analysis (EDAX), Raman scattering studies and Electron Paramagnetic Resonance (EPR). SEM images showed that the morphology of the one dimensional materials included straight nanorods and nanowires around 70-80 nm. Raman spectrum showed the GaMnN vibrational modes at 380, 432 and 445 cm(-1). EPR measurements were performed on Mn doped GaN nanowires in order to evaluate the magnetic behaviour.

Vortex properties of two-dimensional superconducting Pb films.

PubMed

Ning, Y X; Song, C L; Wang, Y L; Chen, Xi; Jia, J F; Xue, Q K; Ma, X C

2010-02-17

Using low temperature scanning tunnelling microscopy/spectroscopy (STM/STS) we have investigated the vortex behaviours of two-dimensional superconducting Pb films at different thicknesses. STS at the vortex core shows an evolution of electronic states with film thickness. Transition from the clean limit to the dirty limit of superconductivity is identified, which can be ascribed to the decreased electronic mean free path induced by stronger scattering from the disordered interface at smaller thicknesses. A magnetic field dependent vortex core size is observed even for such a low- κ superconductor. The weak pinning induced by surface defects leads to the formation of a distorted hexagonal vortex lattice.

Predicting scattering scanning near-field optical microscopy of mass-produced plasmonic devices

NASA Astrophysics Data System (ADS)

Otto, Lauren M.; Burgos, Stanley P.; Staffaroni, Matteo; Ren, Shen; Süzer, Özgün; Stipe, Barry C.; Ashby, Paul D.; Hammack, Aeron T.

2018-05-01

Scattering scanning near-field optical microscopy enables optical imaging and characterization of plasmonic devices with nanometer-scale resolution well below the diffraction limit. This technique enables developers to probe and understand the waveguide-coupled plasmonic antenna in as-fabricated heat-assisted magnetic recording heads. In order to validate and predict results and to extract information from experimental measurements that is physically comparable to simulations, a model was developed to translate the simulated electric field into expected near-field measurements using physical parameters specific to scattering scanning near-field optical microscopy physics. The methods used in this paper prove that scattering scanning near-field optical microscopy can be used to determine critical sub-diffraction-limited dimensions of optical field confinement, which is a crucial metrology requirement for the future of nano-optics, semiconductor photonic devices, and biological sensing where the near-field character of light is fundamental to device operation.

Vapor-Redissolution Technique for Reduction of POLYMER/Si Arrayed Waveguide Grating Loss

NASA Astrophysics Data System (ADS)

Zhang, Haiming; Zhang, Daming; Qin, Zhenkun; Ma, Chunsheng

An efficient vapor-redissolution technique is used to greatly reduce sidewall scattering loss in the polymer arrayed waveguide grating (AWG) fabricated on a silicon substrate. Smoother sidewalls are achieved and verified by scanning electron microscopy. Reduction of sidewall scattering loss is further measured for the loss measurement of both straight waveguides and AWG devices. The sidewall loss in straight polymer waveguide is decreased by 2.1 dB/cm, the insertion loss of our AWG device is reduced by about 5.5 dB for the central channel and 6.7 dB for the edge channels, the crosstalk is reduced by 2.5 dB, and 3-dB bandwidth is narrowed by 0.05 nm after the vapor-redissoluton treatment.

Darkfield microspectroscopy of nanostructures on silver tip-enhanced Raman scattering probes

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

Itoh, Tamitake, E-mail: tamitake-itou@aist.go.jp; Yamamoto, Yuko S., E-mail: yamayulab@gmail.com; Department of Chemistry, School of Science and Technology, Kagawa University, Takamatsu, Kagawa 761-0396

2016-01-11

We report an evaluation method employing darkfield microspectroscopy for silver probes used in tip-enhanced Raman scattering (TERS). By adjusting the darkfield illumination, the diffracted light from the probe outlines disappears and the diffracted light from the surface nanostructures and tips of the probes appears as colorful spots. Scanning electron microscopy reveals that the spectral variations in these spots reflect the shapes of the surface nanostructures. The tip curvatures correlate to the spectral maxima of their spots. Temporal color changes in the spots indicate the deterioration due to the oxidation of the silver surfaces. These results show that the proposed methodmore » is useful for in situ evaluation of plasmonic properties of TERS probes.« less

Surface-enhanced Raman scattering from silver nanostructures with different morphologies

NASA Astrophysics Data System (ADS)

Zhang, W. C.; Wu, X. L.; Kan, C. X.; Pan, F. M.; Chen, H. T.; Zhu, J.; Chu, Paul K.

2010-07-01

Scanning electron microscopy and X-ray diffraction reveal that four different types of crystalline silver nanostructures including nanoparticles, nanowires, nanocubes, and bipyramids are synthesized by a solvothermal method by reducing silver nitrate with ethylene glycol using poly(vinylpyrrolidone) as an adsorption agent and adding different quantities of sodium chloride to the solution. These nanostructures which exhibit different surface plasma resonance properties in the ultraviolet-visible region are shown to be good surface-enhanced Raman scattering (SERS) substrates using rhodamine 6G molecules. Our results demonstrate that the silver nanocubes, bipyramids with sharp corners and edges, and aggregated silver nanoparticles possess better SERS properties than the silver nanowires, indicating that they can serve as high-sensitivity substrates in SERS-based measurements.

Characterization of oligomerization of a peptide from the ebola virus glycoprotein by small-angle neutron scattering

NASA Astrophysics Data System (ADS)

Egorov, V. V.; Gorshkov, A. N.; Murugova, T. N.; Vasin, A. V.; Lebedev, D. V.; Isaev-Ivanov, V. V.; Kiselev, O. I.

2016-01-01

Transmission electron microscopy (TEM) and small-angle neutron scattering (SANS) studies showed that model peptides QNALVCGLRQ (G33) and QNALVCGLRG (G31) corresponding to region 551-560 of the GP protein of the Sudan Ebola virus are prone to oligomerization in solution. Both peptides can form amyloid-like fibrills. The G33 peptide forms fibrils within one day of incubation, whereas the fibrillogenesis of the G31 peptide is observed only after incubation for several months. The possible role of the observed processes in the pathogenesis and the possibility of applying a combination of the TEM and SANS techniques to search for new compounds that are able to influence the protein oligomerization are discussed.

Hierarchical structure and dynamics of oligocarbonate-functionalized PEG block copolymer gels

NASA Astrophysics Data System (ADS)

Prabhu, Vivek; Wei, Guangmin; Ali, Samim; Venkataraman, Shrinivas; Yang, Yi Yan; Hedrick, James

Hierarchical, self-assembled block copolymers in aqueous solutions provide advanced materials for biomaterial applications. Recent advancements in the synthesis of aliphatic polycarbonates have shown nontraditional micellar and hierarchical structures driven by the supramolecular assembly of the carbonate block functionality that includes cholesterol, vitamin D, and fluorene. This presentation shall describe the supramolecular assembly structure and dynamics observed by static and dynamic light scattering, small-angle neutron scattering and transmission electron microscopy in a model pi-pi stacking driven fluorene system. The combination of real-space and reciprocal space methods to develop appropriate models that quantify the structure from the micelle to transient gel network will be discussed. 1) Biomedical Research Council, Agency for Science, Technology and Research, Singapore, 2) NIST Materials Genome Initiative.

Future of Electron Scattering and Diffraction

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

Hall, Ernest; Stemmer, Susanne; Zheng, Haimei

2014-02-25

The ability to correlate the atomic- and nanoscale-structure of condensed matter with physical properties (e.g., mechanical, electrical, catalytic, and optical) and functionality forms the core of many disciplines. Directing and controlling materials at the quantum-, atomic-, and molecular-levels creates enormous challenges and opportunities across a wide spectrum of critical technologies, including those involving the generation and use of energy. The workshop identified next generation electron scattering and diffraction instruments that are uniquely positioned to address these grand challenges. The workshop participants identified four key areas where the next generation of such instrumentation would have major impact: A – Multidimensional Visualizationmore » of Real Materials B – Atomic-scale Molecular Processes C – Photonic Control of Emergence in Quantum Materials D – Evolving Interfaces, Nucleation, and Mass Transport Real materials are comprised of complex three-dimensional arrangements of atoms and defects that directly determine their potential for energy applications. Understanding real materials requires new capabilities for three-dimensional atomic scale tomography and spectroscopy of atomic and electronic structures with unprecedented sensitivity, and with simultaneous spatial and energy resolution. Many molecules are able to selectively and efficiently convert sunlight into other forms of energy, like heat and electric current, or store it in altered chemical bonds. Understanding and controlling such process at the atomic scale require unprecedented time resolution. One of the grand challenges in condensed matter physics is to understand, and ultimately control, emergent phenomena in novel quantum materials that necessitate developing a new generation of instruments that probe the interplay among spin, charge, orbital, and lattice degrees of freedom with intrinsic time- and length-scale resolutions. Molecules and soft matter require imaging and spectroscopy with high spatial resolution without damaging their structure. The strong interaction of electrons with matter allows high-energy electron pulses to gather structural information before a sample is damaged. Electron ScatteringImaging, diffraction, and spectroscopy are the fundamental capabilities of electron-scattering instruments. The DOE BES-funded TEAM (Transmission Electron Aberration-corrected Microscope) project achieved unprecedented sub-atomic spatial resolution in imaging through aberration-corrected transmission electron microscopy. To further advance electron scattering techniques that directly enable groundbreaking science, instrumentation must advance beyond traditional two-dimensional imaging. Advances in temporal resolution, recording the full phase and energy spaces, and improved spatial resolution constitute a new frontier in electron microscopy, and will directly address the BES Grand Challenges, such as to “control the emergent properties that arise from the complex correlations of atomic and electronic constituents” and the “hidden states” “very far away from equilibrium”. Ultrafast methods, such as the pump-probe approach, enable pathways toward understanding, and ultimately controlling, the chemical dynamics of molecular systems and the evolution of complexity in mesoscale and nanoscale systems. Central to understanding how to synthesize and exploit functional materials is having the ability to apply external stimuli (such as heat, light, a reactive flux, and an electrical bias) and to observe the resulting dynamic process in situ and in operando, and under the appropriate environment (e.g., not limited to UHV conditions). To enable revolutionary advances in electron scattering and science, the participants of the workshop recommended three major new instrumental developments: A. Atomic-Resolution Multi-Dimensional Transmission Electron Microscope: This instrument would provide quantitative information over the entire real space, momentum space, and energy space for visualizing dopants, interstitials, and light elements; for imaging localized vibrational modes and the motion of charged particles and vacancies; for correlating lattice, spin, orbital, and charge; and for determining the structure and molecular chemistry of organic and soft matter. The instrument will be uniquely suited to answer fundamental questions in condensed matter physics that require understanding the physical and electronic structure at the atomic scale. Key developments include stable cryogenic capabilities that will allow access to emergent electronic phases, as well as hard/soft interfaces and radiation- sensitive materials. B. Ultrafast Electron Diffraction and Microscopy Instrument: This instrument would be capable of nano-diffraction with 10 fs temporal resolution in stroboscopic mode, and better than 100 fs temporal resolution in single shot mode. The instrument would also achieve single- shot real-space imaging with a spatial/temporal resolution of 10 nm/10 ps, representing a thousand fold improvement over current microscopes. Such a capability would be complementary to x-ray free electron lasers due to the difference in the nature of electron and x-ray scattering, enabling space-time mapping of lattice vibrations and energy transport, facilitating the understanding of molecular dynamics of chemical reactions, the photonic control of emergence in quantum materials, and the dynamics of mesoscopic materials. C. Lab-In-Gap Dynamic Microscope: This instrument would enable quantitative measurements of materials structure, composition, and bonding evolution in technologically relevant environments, including liquids, gases and plasmas, thereby assuring the understanding of structure function relationship at the atomic scale with up to nanosecond temporal resolution. This instrument would employ a versatile, modular sample stage and holder geometry to allow the multi-modal (e.g., optical, thermal, mechanical, electrical, and electrochemical) probing of materials’ functionality in situ and in operando. The electron optics encompasses a pole piece that can accommodate the new stage, differential pumping, detectors, aberration correctors, and other electron optical elements for measurement of materials dynamics. To realize the proposed instruments in a timely fashion, BES should aggressively support research and development of complementary and enabling instruments, including new electron sources, advanced electron optics, new tunable specimen pumps and sample stages, and new detectors. The proposed instruments would have transformative impact on physics, chemistry, materials science, engineering« less

Fluorescent Imaging of Single Nanoparticles and Viruses on a Smart Phone

PubMed Central

Wei, Qingshan; Qi, Hangfei; Luo, Wei; Tseng, Derek; Ki, So Jung; Wan, Zhe; Göröcs, Zoltán; Bentolila, Laurent A.; Wu, Ting-Ting; Sun, Ren; Ozcan, Aydogan

2014-01-01

Optical imaging of nanoscale objects, whether it is based on scattering or fluorescence, is a challenging task due to reduced detection signal-to-noise ratio and contrast at subwavelength dimensions. Here, we report a field-portable fluorescence microscopy platform installed on a smart phone for imaging of individual nanoparticles as well as viruses using a lightweight and compact opto-mechanical attachment to the existing camera module of the cell phone. This hand-held fluorescent imaging device utilizes (i) a compact 450 nm laser diode that creates oblique excitation on the sample plane with an incidence angle of ~75°, (ii) a long-pass thin-film interference filter to reject the scattered excitation light, (iii) an external lens creating 2× optical magnification, and (iv) a translation stage for focus adjustment. We tested the imaging performance of this smart-phone-enabled microscopy platform by detecting isolated 100 nm fluorescent particles as well as individual human cytomegaloviruses that are fluorescently labeled. The size of each detected nano-object on the cell phone platform was validated using scanning electron microscopy images of the same samples. This field-portable fluorescence microscopy attachment to the cell phone, weighing only ~186 g, could be used for specific and sensitive imaging of subwavelength objects including various bacteria and viruses and, therefore, could provide a valuable platform for the practice of nanotechnology in field settings and for conducting viral load measurements and other biomedical tests even in remote and resource-limited environments. PMID:24016065

Nanoscale structural and electronic characterization of α-RuCl3 layered compound

NASA Astrophysics Data System (ADS)

Ziatdinov, Maxim; Maksov, Artem; Banerjee, Arnab; Zhou, Wu; Berlijn, Tom; Yan, Jiaqiang; Nagler, Stephen; Mandrus, David; Baddorf, Arthur; Kalinin, Sergei

The exceptional interplay of spin-orbit effects, Coulomb interaction, and electron-lattice coupling is expected to produce an elaborate phase space of α-RuCl3 layered compound, which to date remains largely unexplored. Here we employ a combination of scanning transmission electron microscopy (STEM) and scanning tunneling microscopy (STM) for detailed evaluation of the system's microscopic structural and electronic orders with a sub-nanometer precision. The STM and STEM measurements are further supported by neutron scattering, X-Ray diffraction, density functional theory (DFT), and multivariate statistical analysis. Our results show a trigonal distortion of Cl octahedral ligand cage along the C3 symmetry axes in each RuCl3 layer. The lattice distortion is limited mainly to the Cl subsystem leaving the Ru honeycomb lattice nearly intact. The STM topographic and spectroscopic characterization reveals an intra unit cell electronic symmetry breaking in a spin-orbit coupled Mott insulating phase on the Cl-terminated surface of α-RuCl3. The associated long-range charge order (CO) pattern is linked to a surface component of Cl cage distortion. We finally discuss a fine structure of CO and its potential relation to variations of average unit cell geometries found in multivariate analysis of STEM data. The research was sponsored by the U.S. Department of Energy.

Microstructural characterization of weld joints of 9Cr reduced activation ferritic martensitic steel fabricated by different joining methods

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

Thomas Paul, V.; Saroja, S.; Albert, S.K.

This paper presents a detailed electron microscopy study on the microstructure of various regions of weldment fabricated by three welding methods namely tungsten inert gas welding, electron beam welding and laser beam welding in an indigenously developed 9Cr reduced activation ferritic/martensitic steel. Electron back scatter diffraction studies showed a random micro-texture in all the three welds. Microstructural changes during thermal exposures were studied and corroborated with hardness and optimized conditions for the post weld heat treatment have been identified for this steel. Hollomon–Jaffe parameter has been used to estimate the extent of tempering. The activation energy for the tempering processmore » has been evaluated and found to be corresponding to interstitial diffusion of carbon in ferrite matrix. The type and microchemistry of secondary phases in different regions of the weldment have been identified by analytical transmission electron microscopy. - Highlights: • Comparison of microstructural parameters in TIG, electron beam and laser welds of RAFM steel • EBSD studies to illustrate the absence of preferred orientation and identification of prior austenite grain size using phase identification map • Optimization of PWHT conditions for indigenous RAFM steel • Study of kinetics of tempering and estimation of apparent activation energy of the process.« less

Laser-Induced, Local Oxidation of Copper Nanoparticle Films During Raman Measurements

NASA Astrophysics Data System (ADS)

Hight Walker, Angela R.; Cheng, Guangjun; Calizo, Irene

2011-03-01

The optical properties of gold and silver nanoparticles and their films have been thoroughly investigated as surface enhanced Raman scattering (SERS) substrates and chemical reaction promoters. Similar to gold and silver nanoparticles, copper nanoparticles exhibit distinct plasmon absorptions in the visible region. The work on copper nanoparticles and their films is limited due to their oxidization in air. However, their high reactivity actually provides an opportunity to exploit the laser-induced thermal effect and chemical reactions of these nanoparticles. Here, we present our investigation of the local oxidation of a copper nanoparticle film induced by a visible laser source during Raman spectroscopic measurements. The copper nanoparticle film is prepared by drop-casting chemically synthesized copper colloid onto silicon oxide/silicon substrate. The local oxidation induced by visible lasers in Raman spectroscopy is monitored with the distinct scattering peaks for copper oxides. Optical microscopy and scanning electron microscopy have been used to characterize the laser-induced morphological changes in the film. The results of this oxidation process with different excitation wavelengths and different laser powers will be presented.

Detection and isolation of cell-derived microparticles are compromised by protein complexes resulting from shared biophysical parameters.

PubMed

György, Bence; Módos, Károly; Pállinger, Eva; Pálóczi, Krisztina; Pásztói, Mária; Misják, Petra; Deli, Mária A; Sipos, Aron; Szalai, Anikó; Voszka, István; Polgár, Anna; Tóth, Kálmán; Csete, Mária; Nagy, György; Gay, Steffen; Falus, András; Kittel, Agnes; Buzás, Edit I

2011-01-27

Numerous diseases, recently reported to associate with elevated microvesicle/microparticle (MP) counts, have also long been known to be characterized by accelerated immune complex (IC) formation. The goal of this study was to investigate the potential overlap between parameters of protein complexes (eg, ICs or avidin-biotin complexes) and MPs, which might perturb detection and/or isolation of MPs. In this work, after comprehensive characterization of MPs by electron microscopy, atomic force microscopy, dynamic light-scattering analysis, and flow cytometry, for the first time, we drive attention to the fact that protein complexes, especially insoluble ICs, overlap in biophysical properties (size, light scattering, and sedimentation) with MPs. This, in turn, affects MP quantification by flow cytometry and purification by differential centrifugation, especially in diseases in which IC formation is common, including not only autoimmune diseases, but also hematologic disorders, infections, and cancer. These data may necessitate reevaluation of certain published data on patient-derived MPs and contribute to correct the clinical laboratory assessment of the presence and biologic functions of MPs in health and disease.

Characterization of core/shell structures based on CdTe and GaAs nanocrystalline layers deposited on SnO2 microwires

NASA Astrophysics Data System (ADS)

Ghimpu, L.; Ursaki, V. V.; Pantazi, A.; Mesterca, R.; Brâncoveanu, O.; Shree, Sindu; Adelung, R.; Tiginyanu, I. M.; Enachescu, M.

2018-04-01

We report the fabrication and characterization of SnO2/CdTe and SnO2/GaAs core/shell microstructures. CdTe or GaAs shell layers were deposited by radio-frequency (RF) magnetron sputtering on core SnO2 microwires synthesized by a flame-based thermal oxidation method. The produced structures were characterized by scanning electron microscopy (SEM), high-resolution scanning transmission electron microscope (HR-STEM), X-ray diffraction (XRD), Raman scattering and FTIR spectroscopy. It was found that the SnO2 core is of the rutile type, while the shells are composed of CdTe or GaAs nanocrystallites of zincblende structure with the dimensions of crystallites in the range of 10-20 nm. The Raman scattering investigations demonstrated that the quality of the porous nanostructured shell is improved by annealing at temperatures of 420-450 °C. The prospects of implementing these microstructures in intrinsic type fiber optic sensors are discussed.

Structure, Nanomechanics and Dynamics of Dispersed Surfactant-Free Clay Nanocomposite Films

NASA Astrophysics Data System (ADS)

Zhang, Xiao; Zhao, Jing; Snyder, Chad; Karim, Alamgir; National Institute of Standards; Technology Collaboration

Natural Montmorillonite particles were dispersed as tactoids in thin films of polycaprolactone (PCL) through a flow coating technique assisted by ultra-sonication. Wide angle X-ray scattering (WAXS), Grazing-incidence wide angle X-ray scattering (GI-WAXS), and transmission electron microscopy (TEM) were used to confirm the level of dispersion. These characterization techniques are in conjunction with its nanomechanical properties via strain-induced buckling instability for modulus measurements (SIEBIMM), a high throughput technique to characterize thin film mechanical properties. The linear strengthening trend of the elastic modulus enhancements was fitted with Halpin-Tsai (HT) model, correlating the nanoparticle geometric effects and mechanical behaviors based on continuum theories. The overall aspect ratio of dispersed tactoids obtained through HT model fitting is in reasonable agreement with digital electron microscope image analysis. Moreover, glass transition behaviors of the composites were characterized using broadband dielectric relaxation spectroscopy. The segmental relaxation behaviors indicate that the associated mechanical property changes are due to the continuum filler effect rather than the interfacial confinement effect.

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

Song, Yu; Yamani, Zahra; Cao, Chongde

Iron-based superconductivity develops near an antiferromagnetic order and out of a bad-metal normal state, which has been interpreted as originating from a proximate Mott transition. Whether an actual Mott insulator can be realized in the phase diagram of the iron pnictides remains an open question. Here we use transport, transmission electron microscopy, X-ray absorption spectroscopy, resonant inelastic X-ray scattering and neutron scattering to demonstrate that NaFe 1-xCu xAs near x≈0.5 exhibits real space Fe and Cu ordering, and are antiferromagnetic insulators with the insulating behaviour persisting above the Néel temperature, indicative of a Mott insulator. On decreasing x from 0.5,more » the antiferromagnetic-ordered moment continuously decreases, yielding to superconductivity ~x=0.05. Our discovery of a Mott-insulating state in NaFe 1-xCu xAs thus makes it the only known Fe-based material, in which superconductivity can be smoothly connected to the Mott-insulating state, highlighting the important role of electron correlations in the high-T c superconductivity.« less

Monodisperse mesoporous silica nanoparticles of distinct topology.

PubMed

Luo, Leilei; Liang, Yucang; Erichsen, Egil Sev; Anwander, Reiner

2017-06-01

Monodisperse and uniform high-quality MCM(Mobil Composition of Matter)-48-type CMSNs (Cubic Mesoporous Silica Nanoparticles) are readily prepared by simply optimizing the molar ratio of ethanol and surfactant in the system TEOS-CTAB-NaOH-H 2 O-EtOH (TEOS=tetraethyl orthosilicate, CTAB=cetyltrimethylammonium bromide, EtOH=ethanol). In the absence of ethanol only hexagonal mesoporous silica with ellipsoidal and spherical morphology are obtained. The presence of ethanol drives a mesophase transformation from hexagonal to mixed hexagonal/cubic, further to purely cubic, and finally to a mixed cubic/lamellar. This is accompanied by a morphology evolution involving a mixture of ellipses/spheres, regular rods, uniform spheres, and finally a mixture of spheres/flakes. Preserving the three-dimensional (3D) cubic MCM-48 structure, use of a small amount of ethanol is beneficial to the improvement of the monodispersity of the CMSNs. Moreover, the quality of the CMSNs can also be controlled by changing the surfactant concentration or adjusting the stirring rate. All MSNs were characterized using powder X-ray diffraction, transmission electron microscopy, scanning electron microscopy, and N 2 physisorption, indicating highly long-range ordered pore arrays, high specific surface areas (max. 1173 m 2 g -1 ) as well as high pore volumes (max. 1.14 cm 3 g -1 ). The monodispersity of the CMSNs was verified by statistical particle size distribution from SEM (scanning electron microscopy)/TEM (transmission electron microscopy) images and DLS (dynamic light scattering). The mesophase transformation can be rationalized on the basis of an ethanol-driven change of the surfactant packing structure and charge matching at the surfactant/silicate interface. The corresponding morphology evolution can be elucidated by an ethanol-controlled hydrolysis rate of TEOS and degree of condensation of oligomeric silicate species via a nucleation and growth process. Copyright © 2017 Elsevier Inc. All rights reserved.

Fourier Transform Infrared (FTIR) Spectroscopy, Ultraviolet Resonance Raman (UVRR) Spectroscopy, and Atomic Force Microscopy (AFM) for Study of the Kinetics of Formation and Structural Characterization of Tau Fibrils.

PubMed

Ramachandran, Gayathri

2017-01-01

Kinetic studies of tau fibril formation in vitro most commonly employ spectroscopic probes such as thioflavinT fluorescence and laser light scattering or negative stain transmission electron microscopy. Here, I describe the use of Fourier transform infrared (FTIR) spectroscopy, ultraviolet resonance Raman (UVRR) spectroscopy, and atomic force microscopy (AFM) as complementary probes for studies of tau aggregation. The sensitivity of vibrational spectroscopic techniques (FTIR and UVRR) to secondary structure content allows for measurement of conformational changes that occur when the intrinsically disordered protein tau transforms into cross-β-core containing fibrils. AFM imaging serves as a gentle probe of structures populated over the time course of tau fibrillization. Together, these assays help further elucidate the structural and mechanistic complexity inherent in tau fibril formation.

Calcium phosphate nanoparticles as versatile carrier for small and large molecules across cell membranes

NASA Astrophysics Data System (ADS)

Sokolova, Viktoriya; Rotan, Olga; Klesing, Jan; Nalbant, Perihan; Buer, Jan; Knuschke, Torben; Westendorf, Astrid M.; Epple, Matthias

2012-06-01

The successful transport of molecules across the cell membrane is a key point in biology and medicine. In most cases, molecules alone cannot penetrate the cell membrane, therefore an efficient carrier is needed. Calcium phosphate nanoparticles (diameter: 100-250 nm, depending on the functionalization) were loaded with fluorescent oligonucleotides, peptide, proteins, antibodies, polymers or porphyrins and characterized by dynamic light scattering, nanoparticle tracking analysis and scanning electron microscopy. Any excess of molecules was removed by ultracentrifugation, and the dissolved molecules at the same concentration were used as control. The uptake of such fluorescence-labeled nanoparticles into HeLa cells was monitored by fluorescence microscopy and confocal laser scanning microscopy. Calcium phosphate nanoparticles were able to transport all molecules across the cell membrane, whereas the dissolved molecules alone were taken up only to a very small extent or even not at all.

Analysis of electron beam induced deposition (EBID) of residual hydrocarbons in electron microscopy

NASA Astrophysics Data System (ADS)

Rykaczewski, Konrad; White, William B.; Fedorov, Andrei G.

2007-03-01

In this work we have developed a comprehensive dynamic model of electron beam induced deposition (EBID) of residual hydrocarbon coupling mass transport, electron transport and scattering, and species decomposition to predict the deposition of carbon nanopillars. The simulations predict the local species and electron density distributions, as well as the three-demensional morphology and the growth rate of the deposit. Since the process occurs in a high vacuum environment, surface diffusion is considered as the primary transport mode of surface-adsorbed hydrocarbon precursor. The governing surface transport equation (STE) of the adsorbed species is derived and solved numerically. The transport, scattering, and absorption of primary electron as well as secondary electron generation are treated using the Monte Carlo method. Low energy secondary electrons are the major contributors to hydrocarbon decomposition due to their energy range matching peak dissociation reaction cross section energies for precursor molecules. The deposit and substrate are treated as a continuous entity allowing the simulation of the growth of a realistically sized deposit rather than a large number of cells representing each individual atom as in previously published simulations [Mitsuishi et al., Ultramicroscopy 103, 17 (2005); Silvis-Cividjian, Ph.D. thesis, University of Delft, 2002]. Such formulation allows for simple coupling of the STE with the dynamic growth of the nanopillar. Three different growth regimes occurring in EBID are identified using scaling analysis, and simulations are used to describe the deposit morphology and precursor surface concentration specific for each growth regime.

Recent advances in plant-mediated engineered gold nanoparticles and their application in biological system.

PubMed

Siddiqi, Khwaja Salahuddin; Husen, Azamal

2017-03-01

For biosynthesis of gold nanoparticles different parts of a plant are used as they contain metabolites such as alkaloids, flavonoids, phenols, terpenoids, alcohols, sugars and proteins which act as reducing agents to produce nanoparticles. They also act as capping agent and stabilizer for them. They are used in medicine, agriculture and many other technologies. The attention is therefore focussed on all plant species which have either aroma or colour in their leaves, flowers or roots for the synthesis of nanoparticles because they all contain such chemicals which reduce the metal ions to metal nanoparticles. The size and morphology of gold nanoparticles is dependent on the biogenic-synthetic route, incubation time, temperature, concentration and pH of the solution. In this review, we have discussed the latest developments for the fabrication of gold nanoparticles from herbal extract, their characterization by UV-vis., Fourier transform infrared spectroscopy, transmission electron microscopy, scanning electron microscopy, X-ray diffraction, atomic force microscopy, energy-dispersive X-ray spectroscopy, dynamic light scattering and Zeta Potential techniques. Their application in drug delivery, cancer treatment, catalysis and as antimicrobial agent has also been discussed. Copyright © 2016 Elsevier GmbH. All rights reserved.

Evaluation of self-assembled HCPT-loaded PEG-b-PLA nanoparticles by comparing with HCPT-loaded PLA nanoparticles.

PubMed

Yang, Xiangrui; Wu, Shichao; Wang, Yange; Li, Yang; Chang, Di; Luo, Yin; Ye, Shefang; Hou, Zhenqing

2014-12-01

We present a dialysis technique to prepare the 10-hydroxycamptothecin (HCPT)-loaded nanoparticles (NPs) using methoxypolyethylene glycol-poly(D,L-lactide) (PEG-b-PLA) and PLA, respectively. Both HCPT-loaded PEG-b-PLA NPs and HCPT-loaded PLA NPs were characterized by differential scanning calorimetry (DSC), dynamic light scattering (DLS), transmission electron microscopy (TEM), scanning electron microscopy (SEM) and confocal laser scanning microscopy (CLSM). The results showed that the HCPT-loaded PEG-b-PLA NPs and HCPT-loaded PLA NPs presented a hydrodynamic particle size of 120.1 and 226.8 nm, with a polydispersity index of 0.057 and 0.207, a zeta potential of -31.2 and -45.7 mV, drug encapsulation efficiency of 44.52% and 44.94%, and drug-loaded content of 7.42% and 7.49%, respectively. The HCPT-loaded PEG-b-PLA NPs presented faster drug release rate compared to the HCPT-loaded PLA NPs. The HCPT-loaded PEG-b-PLA NPs presented higher cytotoxicity than the HCPT-loaded PLA NPs. These results suggested that the HCPT-loaded PEG-b-PLA NPs presented better characteristics for drug delivery compared to HCPT-loaded PLA NPs.

Ultrathin NiGe films prepared via catalytic solid-vapor reaction of Ni with GeH(4).

PubMed

Peter, Antony P; Opsomer, Karl; Adelmann, Christoph; Schaekers, Marc; Meersschaut, Johan; Richard, Olivier; Vaesen, Inge; Moussa, Alain; Franquet, Alexis; Zsolt, Tokei; Van Elshocht, Sven

2013-10-09

A low-temperature (225-300 °C) solid-vapor reaction process is reported for the synthesis of ultrathin NiGe films (∼6-23 nm) on 300 mm Si wafers covered with thermal oxide. The films were prepared via catalytic chemical vapor reaction of germane (GeH4) gas with physical vapor deposited (PVD) Ni films of different thickness (2-10 nm). The process optimization by investigating GeH4 partial pressure, reaction temperature, and time shows that low resistive, stoichiometric, and phase pure NiGe films can be formed within a broad window. NiGe films crystallized in an orthorhombic structure and were found to exhibit a smooth morphology with homogeneous composition as evidenced by glancing angle X-ray diffraction (GIXRD), scanning electron microscopy (SEM), atomic force microscopy (AFM), and Rutherford back-scattering (RBS) analysis. Transmission electron microscopy (TEM) analysis shows that the NiGe layers exhibit a good adhesion without voids and a sharp interface on the thermal oxide. The NiGe films were found to be morphologically and structurally stable up to 500 °C and exhibit a resistivity value of 29 μΩ cm for 10 nm NiGe films.

Dual Enzyme-Responsive Capsules of Hyaluronic Acid-block-Poly(Lactic Acid) for Sensing Bacterial Enzymes.

PubMed

Tücking, Katrin-Stephanie; Grützner, Verena; Unger, Ronald E; Schönherr, Holger

2015-07-01

The synthesis of novel amphiphilic hyaluronic acid (HYA) and poly(lactic acid) (PLA) block copolymers is reported as the key element of a strategy to detect the presence of pathogenic bacterial enzymes. In addition to the formation of defined HYA-block-PLA assemblies, the encapsulation of fluorescent reporter dyes and the selective enzymatic degradation of the capsules by hyaluronidase and proteinase K are studied. The synthesis of the dual enzyme-responsive HYA-b-PLA is carried out by copper-catalyzed Huisgen 1,3-dipolar cycloaddition. The resulting copolymers are assembled in water to form vesicular structures, which are characterized by scanning electron microscopy, transmission electron microscopy, dynamic light scattering (DLS), and fluorescence lifetime imaging microscopy (FLIM). DLS measurements show that both enzymes cause a rapid decrease in the hydrodynamic diameter of the nanocapsules. Fluorescence spectroscopy data confirm the liberation of encapsulated dye, which indicates the disintegration of the capsules and validates the concept of enzymatically triggered payload release. Finally, cytotoxicity assays confirm that the HYA-b-PLA nanocapsules are biocompatible with primary human dermal microvascular endothelial cells. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

One-step, low-temperature fabrication of CdS quantum dots by watermelon rind: a green approach

PubMed Central

Lakshmipathy, Rajasekhar; Sarada, Nallani Chakravarthula; Chidambaram, K; Pasha, Sk Khadeer

2015-01-01

We investigated the one-step synthesis of CdS nanoparticles via green synthesis that used aqueous extract of watermelon rind as a capping and stabilizing agent. Preliminary phytochemical analysis depicted the presence of carbohydrates which can act as capping and stabilizing agents. Synthesized CdS nanoparticles were characterized using UV-visible, Fourier transform infrared spectroscopy, X-ray diffraction, EDX, dynamic light scattering, transmission electron microscopy, and atomic force microscopy techniques. The CdS nanoparticles were found to be size- and shape-controlled and were stable even after 3 months of synthesis. The results suggest that watermelon rind, an agro-waste, can be used for synthesis of CdS nanoparticles without any addition of stabilizing and capping agents. PMID:26491319

Morphological Characterization of Silicone Hydrogels

NASA Astrophysics Data System (ADS)

Gido, Samuel

2007-03-01

Silicone hydrogel materials are used in the latest generation of extended wear soft contact lenses. To ensure comfort and eye health, these materials must simultaneously exhibit high oxygen permeability and high water permeability / hydrophilicity. The materials achieve these opposing requirements based on bicontinuous composite of nanoscale domains of oxygen permeable (silicones) and hydrophilic (water soluble polymer) materials. The microphase separated morphology of silicone hydrogel contact lens materials was imaged using field emission gun scanning transmission electron microscopy (FEGSTEM), and atomic force microscopy (AFM). Additional morphological information was provided by small angle X-ray scattering (SAXS). These results all indicate a nanophase separated structure of silicone rich (oxygen permeable) and carbon rich (water soluble polymer) domains separated on a length scale of about 10 nm.

Nanoparticle conversion to biofilms: in vitro demonstration using serum-derived mineralo-organic nanoparticles.

PubMed

Wong, Tsui-Yin; Peng, Hsin-Hsin; Wu, Cheng-Yeu; Martel, Jan; Ojcius, David M; Hsu, Fu-Yung; Young, John D

2015-01-01

Mineralo-organic nanoparticles (NPs) detected in biological fluids have been described as precursors of physiological and pathological calcifications in the body. Our main objective was to examine the early stages of mineral NP formation in body fluids. A nanomaterial approach based on atomic force microscopy, dynamic light scattering, electron microscopy and spectroscopy was used. The mineral particles, which contain the serum proteins albumin and fetuin-A, initially precipitate in the form of round amorphous NPs that gradually grow in size, aggregate and coalesce to form crystalline mineral films similar to the structures observed in calcified human arteries. Our study reveals the early stages of particle formation and provides a platform to analyze the role(s) of mineralo-organic NPs in human tissues.

Raman enhancement by graphene-Ga2O3 2D bilayer film.

PubMed

Zhu, Yun; Yu, Qing-Kai; Ding, Gu-Qiao; Xu, Xu-Guang; Wu, Tian-Ru; Gong, Qian; Yuan, Ning-Yi; Ding, Jian-Ning; Wang, Shu-Min; Xie, Xiao-Ming; Jiang, Mian-Heng

2014-01-28

2D β-Ga2O3 flakes on a continuous 2D graphene film were prepared by a one-step chemical vapor deposition on liquid gallium surface. The composite was characterized by optical microscopy, scanning electron microscopy, Raman spectroscopy, energy dispersive spectroscopy, and X-ray photoelectron spectroscopy (XPS). The experimental results indicate that Ga2O3 flakes grew on the surface of graphene film during the cooling process. In particular, tenfold enhancement of graphene Raman scattering signal was detected on Ga2O3 flakes, and XPS indicates the C-O bonding between graphene and Ga2O3. The mechanism of Raman enhancement was discussed. The 2D Ga2O3-2D graphene structure may possess potential applications.

Double-shot MeV electron diffraction and microscopy

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

Musumeci, P.; Cesar, D.; Maxson, J.

Here in this paper, we study by numerical simulations a time-resolved MeV electron scattering mode where two consecutive electron pulses are used to capture the evolution of a material sample on 10 ps time scales. The two electron pulses are generated by illuminating a photocathode in a radiofrequency photogun by two short laser pulses with adjustable delay. A streak camera/deflecting cavity is used after the sample to project the two electron bunches on two well separated regions of the detector screen. By using sufficiently short pulses, the 2D spatial information from each snapshot can be preserved. This “double-shot” technique enablesmore » the efficient capture of irreversible dynamics in both diffraction and imaging modes. Finally, in this work, we demonstrate both modes in start-to-end simulations of the UCLA Pegasus MeV microscope column.« less

Double-shot MeV electron diffraction and microscopy

DOE PAGES

Musumeci, P.; Cesar, D.; Maxson, J.

2017-05-19

Here in this paper, we study by numerical simulations a time-resolved MeV electron scattering mode where two consecutive electron pulses are used to capture the evolution of a material sample on 10 ps time scales. The two electron pulses are generated by illuminating a photocathode in a radiofrequency photogun by two short laser pulses with adjustable delay. A streak camera/deflecting cavity is used after the sample to project the two electron bunches on two well separated regions of the detector screen. By using sufficiently short pulses, the 2D spatial information from each snapshot can be preserved. This “double-shot” technique enablesmore » the efficient capture of irreversible dynamics in both diffraction and imaging modes. Finally, in this work, we demonstrate both modes in start-to-end simulations of the UCLA Pegasus MeV microscope column.« less

Anisotropic high-harmonic generation in bulk crystals

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

You, Yong Sing; Reis, David A.; Ghimire, Shambhu

2016-11-21

The microscopic valence electron density determines the optical, electronic, structural and thermal properties of materials. However, current techniques for measuring this electron charge density are limited: for example, scanning tunnelling microscopy is confined to investigations at the surface, and electron diffraction requires very thin samples to avoid multiple scattering. Therefore, an optical method is desirable for measuring the valence charge density of bulk materials. Since the discovery of high-harmonic generation (HHG) in solids, there has been growing interest in using HHG to probe the electronic structure of solids. Here, using single-crystal MgO, we demonstrate that high-harmonic generation in solids ismore » sensitive to interatomic bonding. We find that harmonic efficiency is enhanced (diminished) for semi-classical electron trajectories that connect (avoid) neighbouring atomic sites in the crystal. Finally, these results indicate the possibility of using materials’ own electrons for retrieving the interatomic potential and thus the valence electron density, and perhaps even wavefunctions, in an all-optical setting.« less

Phthalocyanine adsorption to graphene on Ir(111): Evidence for decoupling from vibrational spectroscopy

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

Endlich, M., E-mail: michael.endlich@tu-ilmenau.de; Gozdzik, S.; Néel, N.

2014-11-14

Phthalocyanine molecules have been adsorbed to Ir(111) and to graphene on Ir(111). From a comparison of scanning tunneling microscopy images of individual molecules adsorbed to the different surfaces alone it is difficult to discern potential differences in the molecular adsorption geometry. In contrast, vibrational spectroscopy using inelastic electron scattering unequivocally hints at strong molecule deformations on Ir(111) and at a planar adsorption geometry on graphene. The spectroscopic evidence for the different adsorption configurations is supported by density functional calculations.

Fabrication and study of properties of magnetite nanoparticles in hybrid micelles of polystyrene-block-polyethylene oxide and sodium dodecyl sulfate

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

Loginova, T. P., E-mail: tlg@ineos.ac.ru; Timofeeva, G. I.; Lependina, O. L.

2016-01-15

Magnetite nanoparticles have been formed for the first time in hybrid micelles of polystyrene-block-polyethylene oxide and sodium dodecyl sulfate in water by ultrasonic treatment at room temperature. An analysis by small-angle X-ray scattering and transmission electron microscopy (TEM) showed that magnetite nanoparticles in hybrid micelles of block copolymer and sodium dodecyl sulfate are polydesperse (have sizes from 0.5 to 20 nm). The specific magnetization of solid samples has been measured.

Dynamical diffraction imaging (topography) with X-ray synchrotron radiation

NASA Technical Reports Server (NTRS)

Kuriyama, M.; Steiner, B. W.; Dobbyn, R. C.

1989-01-01

By contrast to electron microscopy, which yields information on the location of features in small regions of materials, X-ray diffraction imaging can portray minute deviations from perfect crystalline order over larger areas. Synchrotron radiation-based X-ray optics technology uses a highly parallel incident beam to eliminate ambiguities in the interpretation of image details; scattering phenomena previously unobserved are now readily detected. Synchrotron diffraction imaging renders high-resolution, real-time, in situ observations of materials under pertinent environmental conditions possible.

Effect of abrasive water jet on the structure of the surface layer of Al-Mg alloy

NASA Astrophysics Data System (ADS)

Tabatchikova, T. I.; Tereshchenko, N. A.; Yakovleva, I. L.; Gudnev, N. Z.

2017-09-01

Optical, scanning, and transmission electron microscopy methods, and X-ray diffraction analysis have been used to study the changes in the structure and the microhardness in the surface layer of the Al-Mg (5.8-6.8 wt %) alloy after water jet cutting. The dislocation density, the sizes of coherent scattering regions, and microdistortions have been determined. The transformation of the fine structure has been revealed in the displacement from the alloy volume to the abrasive-waterjet cutting surface.

Transport properties of bismuth telluride compound prepared by mechanical alloying

NASA Astrophysics Data System (ADS)

Khade, Poonam; Bagwaiya, Toshi; Bhattacharya, Shovit; Rayaprol, Sudhindra; Sahu, Ashok K.; Shelke, Vilas

2017-05-01

We have synthesized bismuth telluride compound using mechanical alloying and hot press sintering method. The phase formation, crystal structure was evaluated by X-ray diffraction and Raman spectroscopy. The scanning electron microscopy images indicated sub-micron sized grains. We observed low value of thermal conductivity 0.39 W/mK at room temperature as a result of grain size reduction by increasing deformation. The performance of the samples can be improved by reducing the grain size, which increases the grain boundary scattering.

Effect of intermetallic phases on the anodic oxidation and corrosion of 5A06 aluminum alloy

NASA Astrophysics Data System (ADS)

Li, Song-mei; Li, Ying-dong; Zhang, You; Liu, Jian-hua; Yu, Mei

2015-02-01

Intermetallic phases were found to influence the anodic oxidation and corrosion behavior of 5A06 aluminum alloy. Scattered intermetallic particles were examined by scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) after pretreatment. The anodic film was investigated by transmission electron microscopy (TEM), and its corrosion resistance was analyzed by electrochemical impedance spectroscopy (EIS) and Tafel polarization in NaCl solution. The results show that the size of Al-Fe-Mg-Mn particles gradually decreases with the iron content. During anodizing, these intermetallic particles are gradually dissolved, leading to the complex porosity in the anodic film beneath the particles. After anodizing, the residual particles are mainly silicon-containing phases, which are embedded in the anodic film. Electrochemical measurements indicate that the porous anodic film layer is easily penetrated, and the barrier plays a dominant role in the overall protection. Meanwhile, self-healing behavior is observed during the long immersion time.

Growth process optimization of ZnO thin film using atomic layer deposition

NASA Astrophysics Data System (ADS)

Weng, Binbin; Wang, Jingyu; Larson, Preston; Liu, Yingtao

2016-12-01

The work reports experimental studies of ZnO thin films grown on Si(100) wafers using a customized thermal atomic layer deposition. The impact of growth parameters including H2O/DiethylZinc (DEZn) dose ratio, background pressure, and temperature are investigated. The imaging results of scanning electron microscopy and atomic force microscopy reveal that the dose ratio is critical to the surface morphology. To achieve high uniformity, the H2O dose amount needs to be at least twice that of DEZn per each cycle. If the background pressure drops below 400 mTorr, a large amount of nanoflower-like ZnO grains would emerge and increase surface roughness significantly. In addition, the growth temperature range between 200 °C and 250 °C is found to be the optimal growth window. And the crystal structures and orientations are also strongly correlated to the temperature as proved by electron back-scattering diffraction and x-ray diffraction results.

Fabrication of Metal and Metal Oxide Nanoparticles by Algae and their Toxic Effects

NASA Astrophysics Data System (ADS)

Siddiqi, Khwaja Salahuddin; Husen, Azamal

2016-08-01

Of all the aquatic organisms, algae are a good source of biomolecules. Since algae contain pigments, proteins, carbohydrates, fats, nucleic acids and secondary metabolites such as alkaloids, some aromatic compounds, macrolides, peptides and terpenes, they act as reducing agents to produce nanoparticles from metal salts without producing any toxic by-product. Once the algal biomolecules are identified, the nanoparticles of desired shape or size may be fabricated. The metal and metal oxide nanoparticles thus synthesized have been investigated for their antimicrobial activity against several gram-positive and gram-negative bacterial strains and fungi. Their dimension is controlled by temperature, incubation time, pH and concentration of the solution. In this review, we have attempted to update the procedure of nanoparticle synthesis from algae, their characterization by UV-vis, Fourier transform infrared spectroscopy, transmission electron microscopy, scanning electron microscopy, x-ray diffraction, energy-dispersive x-ray spectroscopy, dynamic light scattering and application in cutting-edge areas.

Bulk and Surface Morphologies of ABC Miktoarm Star Terpolymers Composed of PDMS, PI, and PMMA Arms

DOE PAGES

Chernyy, Sergey; Kirkensgaard, Jacob Judas Kain; Mahalik, Jyoti P.; ...

2018-02-02

DIM miktoarm star copolymers, composed of polydimethylsiloxane [D], poly(1,4-isoprene) [I], and poly(methyl methacrylate) [M], were synthesized using a newly developed linking methodology with 4-allyl-1,1-diphenylethylene as a linking agent. The equilibrium bulk morphologies of the DIM stars were found to range from [6.6.6] tiling patterns to alternating lamellar and alternating cylindrical morphologies, as determined experimentally by small-angle X-ray scattering and transmission electron microscopy and confirmed by dissipative particle dynamics and self-consistent field theory based arguments. The thin film morphologies, which differ from those found in the bulk, were identified by scanning electron microscopy, coupled with oxygen plasma etching. Finally, square arraysmore » of the PDMS nanodots and empty core cylinders were formed on silica after oxygen plasma removal of the poly(1,4-isoprene) and poly(methyl methacrylate) which generated nanostructured substrates decorated with these features readily observable.« less

A biocompatible synthesis of gold nanoparticles by Tris(hydroxymethyl)aminomethane

NASA Astrophysics Data System (ADS)

Chen, Feng; Wang, Yanwei; Ma, Jun; Yang, Guangcan

2014-05-01

Gold nanoparticles' novel properties are widely realized in catalysis, plasmonics, electronics, and biomedical applications. For biomedical application, one challenge is to find a non-toxic chemical and/or physical method of functionalizing gold nanoparticles with biomolecular compounds that can promote efficient binding, clearance, and biocompatibility and to assess their safety to other biological systems and their long-term effects on human health and reproduction. In the present study, we describe a new method by using Tris(hydroxymethyl)aminomethane (Tris), a widely used buffer solvent of nucleic acid and proteins, as the reducing agent for synthesizing gold nanoparticles by one step. It is found that Tris carries out the reduction reactions in relatively mild conditions for biomacromolecules. Particularly, it can be used to modify the DNA during the process of preparation of gold nanoparticles. The morphology and size distribution of gold nanoparticles are consistent and were confirmed by many different approaches including dynamic light scattering (DLS), UV-visible (UV-vis) spectrophotometry, atomic force microscopy (AFM), and transmission electron microscopy (TEM).

Bulk and Surface Morphologies of ABC Miktoarm Star Terpolymers Composed of PDMS, PI, and PMMA Arms

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

Chernyy, Sergey; Kirkensgaard, Jacob Judas Kain; Mahalik, Jyoti P.

DIM miktoarm star copolymers, composed of polydimethylsiloxane [D], poly(1,4-isoprene) [I], and poly(methyl methacrylate) [M], were synthesized using a newly developed linking methodology with 4-allyl-1,1-diphenylethylene as a linking agent. The equilibrium bulk morphologies of the DIM stars were found to range from [6.6.6] tiling patterns to alternating lamellar and alternating cylindrical morphologies, as determined experimentally by small-angle X-ray scattering and transmission electron microscopy and confirmed by dissipative particle dynamics and self-consistent field theory based arguments. The thin film morphologies, which differ from those found in the bulk, were identified by scanning electron microscopy, coupled with oxygen plasma etching. Finally, square arraysmore » of the PDMS nanodots and empty core cylinders were formed on silica after oxygen plasma removal of the poly(1,4-isoprene) and poly(methyl methacrylate) which generated nanostructured substrates decorated with these features readily observable.« less

Kinetic control of block copolymer self-assembly into multicompartment and novel geometry nanoparticles

NASA Astrophysics Data System (ADS)

Chen, Yingchao; Wang, Xiaojun; Zhang, Ke; Wooley, Karen; Mays, Jimmy; Percec, Virgil; Pochan, Darrin

2012-02-01

Micelles with the segregation of hydrophobic blocks trapped in the same nanoparticle core have been produced through co-self-assembly of two block copolymers in THF/water dilute solution. The dissolution of two block copolymer sharing the same polyacrylic acid PAA blocks in THF undergoes consequent aggregation and phase separation through either slow water titration or quick water addition that triggers the micellar formation. The combination and comparison of the two water addition kinetic pathways are the keys of forming multicompartment structures at high water content. Importantly, the addition of organic diamine provides for acid-base complexation with the PAA side chains which, in turn, plays the key role of trapping unlike hydrophobic blocks from different block copolymers into one nanoparticle core. The kinetic control of solution assembly can be applied to other molecular systems such as dendrimers as well as other block copolymer molecules. Transmission electron microscopy, cryogenic transmission electron microscopy, light scattering have been applied to characterize the micelle structures.

Structure of the Full-length VEGFR-1 Extracellular Domain in Complex with VEGF-A.

PubMed

Markovic-Mueller, Sandra; Stuttfeld, Edward; Asthana, Mayanka; Weinert, Tobias; Bliven, Spencer; Goldie, Kenneth N; Kisko, Kaisa; Capitani, Guido; Ballmer-Hofer, Kurt

2017-02-07

Vascular endothelial growth factors (VEGFs) regulate blood and lymph vessel development upon activation of three receptor tyrosine kinases: VEGFR-1, -2, and -3. Partial structures of VEGFR/VEGF complexes based on single-particle electron microscopy, small-angle X-ray scattering, and X-ray crystallography revealed the location of VEGF binding and domain arrangement of individual receptor subdomains. Here, we describe the structure of the full-length VEGFR-1 extracellular domain in complex with VEGF-A at 4 Å resolution. We combined X-ray crystallography, single-particle electron microscopy, and molecular modeling for structure determination and validation. The structure reveals the molecular details of ligand-induced receptor dimerization, in particular of homotypic receptor interactions in immunoglobulin homology domains 4, 5, and 7. Functional analyses of ligand binding and receptor activation confirm the relevance of these homotypic contacts and identify them as potential therapeutic sites to allosterically inhibit VEGFR-1 activity. Copyright © 2017 Elsevier Ltd. All rights reserved.

Electrodeposition of Au/Ag bimetallic dendrites assisted by Faradaic AC-electroosmosis flow

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

Ji, Jianlong; Li, Pengwei; Sang, Shengbo, E-mail: sbsang@tyut.edu.cn

2014-03-15

Au/Ag bimetallic dendrites were synthesized successfully from the corresponding aqueous solution via the AC electrodeposition method. Both of the morphologies and compositions could be tuned by the electrolyte concentration and AC frequency. The prepared bimetallic dendrites were characterized by scanning electron microscopy (SEM), energy dispersive X-ray spectrometer (EDS), transmission electron microscopy (TEM) and UV–vis spectroscopy. The underlying dendrite growth mechanism was then proposed in the context of the Directed Electrochemical Nanowires Assembly (DENA) models. Owing to the unscreened voltage dropping in the electrolyte bulk, electromigration dominates the species flux process, and cations tend to accumulate in areas with strong electricmore » field intensity, such as electrode edges. Moreover, Faradaic AC-electro-osmosis (ACEO) flow could increase the effective diffusion layer thickness in these areas during the electrochemical reaction, and leads to dendrite growth. Further Micro-Raman observations illustrated that the Au/Ag bimetallic dendrites exhibited pronounced surface-enhanced Raman scattering (SERS) activity, using 4-mercaptopyridine (4-MP) as model molecules.« less

Enhanced light element imaging in atomic resolution scanning transmission electron microscopy.

PubMed

Findlay, S D; Kohno, Y; Cardamone, L A; Ikuhara, Y; Shibata, N

2014-01-01

We show that an imaging mode based on taking the difference between signals recorded from the bright field (forward scattering region) in atomic resolution scanning transmission electron microscopy provides an enhancement of the detectability of light elements over existing techniques. In some instances this is an enhancement of the visibility of the light element columns relative to heavy element columns. In all cases explored it is an enhancement in the signal-to-noise ratio of the image at the light column site. The image formation mechanisms are explained and the technique is compared with earlier approaches. Experimental data, supported by simulation, are presented for imaging the oxygen columns in LaAlO₃. Case studies looking at imaging hydrogen columns in YH₂ and lithium columns in Al₃Li are also explored through simulation, particularly with respect to the dependence on defocus, probe-forming aperture angle and detector collection aperture angles. © 2013 Elsevier B.V. All rights reserved.

Solid lipid nanoparticles mediate non-viral delivery of plasmid DNA to dendritic cells

NASA Astrophysics Data System (ADS)

Penumarthi, Alekhya; Parashar, Deepti; Abraham, Amanda N.; Dekiwadia, Chaitali; Macreadie, Ian; Shukla, Ravi; Smooker, Peter M.

2017-06-01

There is an increasing demand for novel DNA vaccine delivery systems, mainly for the non-viral type as they are considered relatively safe. Therefore, solid lipid nanoparticles (SLNs) were investigated for their suitability as a non-viral DNA vaccine delivery system. SLNs were synthesised by a modified solvent-emulsification method in order to study their potential to conjugate with plasmid DNA and deliver them in vitro to dendritic cells using eGFP as the reporter plasmid. The DNA-SLN complexes were characterised by electron microscopy, gel retardation assays and dynamic light scattering. The cytotoxicity assay data supported their biocompatibility and was used to estimate safe threshold concentration resulting in high transfection rate. The transfection efficiency of these complexes in a dendritic cell line was shown to increase significantly compared to plasmid alone, and was comparable to that mediated by lipofectamine. Transmission electron microscopy studies delineated the pathway of cellular uptake. Endosomal escape was observed supporting the mechanism of transfection.

Synthesis of highly-monodisperse spherical titania particles with diameters in the submicron range.

PubMed

Tanaka, Shunsuke; Nogami, Daisuke; Tsuda, Natsuki; Miyake, Yoshikazu

2009-06-15

Monodisperse titania spheres with particle diameters in the range 380-960 nm were successfully synthesized by hydrolysis and condensation of titanium tetraisopropoxide. The preparation was performed using ammonia or dodecylamine (DDA) as a catalyst in methanol/acetonitrile co-solvent at room temperature. The samples were characterized by powder X-ray diffraction, scanning electron microscopy, transmission electron microscopy, dynamic light scattering, and nitrogen sorption measurement. The use of DDA was effective for the synthesis of monodisperse titania spheres with low coefficient of variation. When the titania spherical particles with coefficient of variation less than 4% were obtained, the colloidal crystallization easily occurred simply by centrifugation. The monodispersity was maintained even after crystallization of the particles by high temperature annealing. The titania particles prepared using DDA had mesopores near the surface of the spheres, providing high pore accessibility to the sphere from the surface-air interface. The particle size uniformity and photocatalytic reactivity of the titania prepared using DDA were higher than those of the titania prepared using ammonia.

The role of gas in determining image quality and resolution during in situ scanning transmission electron microscopy experiments

DOE PAGES

Zhu, Yuanyuan; Browning, Nigel D.

2017-05-24

As gas-solid heterogeneous catalytic reactions are molecular in nature, a full mechanistic understanding of the process requires atomic scale characterization under realistic operating conditions. While atomic resolution imaging has become a routine in modern high-vacuum (scanning) transmission electron microscopy ((S)TEM), both image quality and resolution nominally degrade when reaction gases are introduced. In this work, we systematically assess the effects of different gases at various pressures on the quality and resolution of images obtained at room temperature in the annular dark field STEM imaging mode using a differentially pumped (DP) gas cell. This imaging mode is largely free from inelasticmore » scattering effects induced by the presence of gases and retains good imaging properties over a wide range of gas mass/pressures. Furthermore, we demonstrate the application of the ESTEM with atomic resolution images of a complex oxide alkane oxidation catalyst MoVNbTeOx (M1) immersed in light and heavy gas environments.« less

Isotope effect in heavy/light water suspensions of optically active gold nanoparticles

NASA Astrophysics Data System (ADS)

Kutsenko, V. Y.; Artykulnyi, O. P.; Petrenko, V. I.; Avdeev, M. V.; Marchenko, O. A.; Bulavin, L. A.; Snegir, S. V.

2018-04-01

Aqueous suspensions of optically active gold nanoparticles coated with trisodium citrate were synthesized in light (H2O) water and mixture of light and heavy (H2O/D2O) water using the modified Turkevich protocol. The objective of the paper was to verify sensitivity of neutron scattering methods (in particular, neutron reflectometry) to the potential isotope H/D substitution in the stabilizing organic shell around particles in colloidal solutions. First, the isotope effect was studied with respect to the changes in the structural properties of metal particles (size, shape, crystalline morphology) in solutions by electron microscopy including high-resolution transmission electron microscopy from dried systems. The structural factors determining the variation in the adsorption spectra in addition to the change in the optical properties of surrounding medium were discussed. Then, neutron reflectometry was applied to the layered nanoparticles anchored on a silicon wafer via 3-aminopropyltriethoxysilane molecules to reveal the presence of deuterated water molecules in the shell presumably formed by citrate molecules around the metallic core.

Single Molecule Spectroelectrochemistry of Interfacial Charge Transfer Dynamics In Hybrid Organic Solar Cell

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

Pan, Shanlin

2014-11-16

Our research under support of this DOE grant is focused on applied and fundamental aspects of model organic solar cell systems. Major accomplishments are: 1) we developed a spectroelectorchemistry technique of single molecule single nanoparticle method to study charge transfer between conjugated polymers and semiconductor at the single molecule level. The fluorescence of individual fluorescent polymers at semiconductor surfaces was shown to exhibit blinking behavior compared to molecules on glass substrates. Single molecule fluorescence excitation anisotropy measurements showed the conformation of the polymer molecules did not differ appreciably between glass and semiconductor substrates. The similarities in molecular conformation suggest thatmore » the observed differences in blinking activity are due to charge transfer between fluorescent polymer and semiconductor, which provides additional pathways between states of high and low fluorescence quantum efficiency. Similar spectroelectrochemistry work has been done for small organic dyes for understand their charge transfer dynamics on various substrates and electrochemical environments; 2) We developed a method of transferring semiconductor nanoparticles (NPs) and graphene oxide (GO) nanosheets into organic solvent for a potential electron acceptor in bulk heterojunction organic solar cells which employed polymer semiconductor as the electron donor. Electron transfer from the polymer semiconductor to semiconductor and GO in solutions and thin films was established through fluorescence spectroscopy and electroluminescence measurements. Solar cells containing these materials were constructed and evaluated using transient absorption spectroscopy and dynamic fluorescence techniques to understand the charge carrier generation and recombination events; 3) We invented a spectroelectorchemistry technique using light scattering and electroluminescence for rapid size determination and studying electrochemistry of single NPs in an electrochemical cell. For example, we are able to use this technique to track electroluminescence of single Au NPs, and the electrodeposition of individual Ag NPs in-situ. These metallic NPs are useful to enhance light harvesting in organic photovoltaic systems. The scattering at the surface of an indium tin oxide (ITO) working electrode was measured during a potential sweep. Utilizing Mie scattering theory and high resolution scanning electron microscopy (SEM), the scattering data were used to calculate current-potential curves depicting the electrodeposition of individual Ag NPs. The oxidation of individual presynthesized and electrodeposited Ag NPs was also investigated using fluorescence and DFS microscopies. Our work has produced 1 US provisional patent, 15 published manuscripts, 1 submitted and two additional in-writing manuscripts. 5 graduate students, 1 postdoctoral student, 1 visiting professor, and two undergraduate students have received research training in the area of electrochemistry and optical spectroscopy under support of this award.« less

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.

Rare-earth-doped nanophosphors for multicolor cathodoluminescence nanobioimaging using scanning transmission electron microscopy.

PubMed

Furukawa, Taichi; Fukushima, Shoichiro; Niioka, Hirohiko; Yamamoto, Naoki; Miyake, Jun; Araki, Tsutomu; Hashimoto, Mamoru

2015-05-01

We describe rare-earth-doped nanophosphors (RE-NPs) for biological imaging using cathodoluminescence(CL) microscopy based on scanning transmission electron microscopy (STEM). We report the first demonstration of multicolor CL nanobioimaging using STEM with nanophosphors. The CL spectra of the synthesized nanophosphors (Y2O3∶Eu, Y2O3∶Tb) were sufficiently narrow to be distinguished. From CL images of RE-NPs on an elastic carbon-coated copper grid, the spatial resolution was beyond the diffraction limit of light.Y2O3∶Tb and Y2O3∶Eu RE-NPs showed a remarkable resistance against electron beam exposure even at high acceleration voltage (80 kV) and retained a CL intensity of more than 97% compared with the initial intensity for 1 min. In biological CL imaging with STEM, heavy-metal-stained cell sections containing the RE-NPs were prepared,and both the CL images of RE-NPs and cellular structures, such as mitochondria, were clearly observed from STEM images with high contrast. The cellular CL imaging using RE-NPs also had high spatial resolution even though heavy-metal-stained cells are normally regarded as highly scattering media. Moreover, since theRE-NPs exhibit photoluminescence (PL) excited by UV light, they are useful for multimodal correlative imaging using CL and PL.

Microstructure, texture, and mechanical properties of friction stir welded commercial brass alloy

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

Heidarzadeh, A., E-mail: ak.hz62@gmail.com

Microstructural evolution during friction stir welding of single-phase brass and corresponding mechanical properties were investigated. For this purpose, 2 mm thick brass plate was friction stir welded at a rotational speed of 450 rpm and traverse speed of 100 mm/min. The microstructure of the joint was studied using optical microscopy, scanning electron microscopy equipped with electron back scattered diffraction system, and scanning transmission electron microscopy. The mechanical properties were measured using hardness and tensile tests. The formation of subgrains and their transformation into new grains in conjunction with existence of A{sub 1}{sup ⁎}, A{sub 2}{sup ⁎} and C texture componentsmore » revealed that the continuous dynamic recrystallization plays a dominant role in the microstructural evolution. However, grain boundary bulging, along with the formation of twin boundaries, and presence of the G texture component showed that the discontinues dynamic recrystallization may participate in the new grain formation. Furthermore, the different strengthening mechanisms, which caused the higher strength of the joint, were discussed. - Highlights: •Microstructural evolution during FSW of a single phase brass was investigated. •CDRX and DDRX were the main mechanisms of the grain structure formation during FSW. •GDRX and SRX were not contributed in grain structure formation. •The lamellas TBs were formed in the SZ of the joints. •Grain boundary, dislocation, and texture effects resulted in higher strength.« less

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.

Differential dynamic microscopy of weakly scattering and polydisperse protein-rich clusters

NASA Astrophysics Data System (ADS)

Safari, Mohammad S.; Vorontsova, Maria A.; Poling-Skutvik, Ryan; Vekilov, Peter G.; Conrad, Jacinta C.

2015-10-01

Nanoparticle dynamics impact a wide range of biological transport processes and applications in nanomedicine and natural resource engineering. Differential dynamic microscopy (DDM) was recently developed to quantify the dynamics of submicron particles in solutions from fluctuations of intensity in optical micrographs. Differential dynamic microscopy is well established for monodisperse particle populations, but has not been applied to solutions containing weakly scattering polydisperse biological nanoparticles. Here we use bright-field DDM (BDDM) to measure the dynamics of protein-rich liquid clusters, whose size ranges from tens to hundreds of nanometers and whose total volume fraction is less than 10-5. With solutions of two proteins, hemoglobin A and lysozyme, we evaluate the cluster diffusion coefficients from the dependence of the diffusive relaxation time on the scattering wave vector. We establish that for weakly scattering populations, an optimal thickness of the sample chamber exists at which the BDDM signal is maximized at the smallest sample volume. The average cluster diffusion coefficient measured using BDDM is consistently lower than that obtained from dynamic light scattering at a scattering angle of 90∘. This apparent discrepancy is due to Mie scattering from the polydisperse cluster population, in which larger clusters preferentially scatter more light in the forward direction.

Coherent Raman scattering microscopy for label-free imaging of live amphioxus

NASA Astrophysics Data System (ADS)

Yu, Zhilong; Chen, Tao; Zhang, Xiannian; Shen, Jie; Chen, Junyuan; Huang, Yanyi

2012-03-01

The existence of notochord distinguishes chordates from other phyla. Amphioxus is the only animal that keeps notochord during the whole life. Notochord is a unique organ for amphioxus, with its vertically arranged muscular notochordal plates, which is different from notochords in embryos of other chordates. We use stimulated Raman scattering (SRS) microscopy as a non-invasive technique to image the chemical components in amphioxus notochord. SRS provides chemical specificity as spontaneous Raman does and offers a higher sensitivity for fast acquisition. Unlike coherent anti- Stokes Raman scattering (CARS) microscopy, SRS microscopy doesn't have non-resonant background and can better differentiate different components in the specimen. We verify that the notochord is a protein-rich organ, which agrees well with the result of conventional staining methods. Detailed structures in notochordal plates and notochordal sheath are revealed by SRS microscopy with diffraction limited resolution. Our experiment shows that SRS microscopy is an excellent imaging tool for biochemical research with its intrinsic chemical selectivity, high spatiotemporal resolution and native 3D optical sectioning ability.

Wide field fluorescence epi-microscopy behind a scattering medium enabled by speckle correlations

NASA Astrophysics Data System (ADS)

Hofer, Matthias; Soeller, Christian; Brasselet, Sophie; Bertolotti, Jacopo

2018-04-01

Fluorescence microscopy is widely used in biological imaging, however scattering from tissues strongly limits its applicability to a shallow depth. In this work we adapt a methodology inspired from stellar speckle interferometry, and exploit the optical memory effect to enable fluorescence microscopy through a turbid layer. We demonstrate efficient reconstruction of micrometer-size fluorescent objects behind a scattering medium in epi-microscopy, and study the specificities of this imaging modality (magnification, field of view, resolution) as compared to traditional microscopy. Using a modified phase retrieval algorithm to reconstruct fluorescent objects from speckle images, we demonstrate robust reconstructions even in relatively low signal to noise conditions. This modality is particularly appropriate for imaging in biological media, which are known to exhibit relatively large optical memory ranges compatible with tens of micrometers size field of views, and large spectral bandwidths compatible with emission fluorescence spectra of tens of nanometers widths.

Three-dimensional structure determination protocol for noncrystalline biomolecules using x-ray free-electron laser diffraction imaging.

PubMed

Oroguchi, Tomotaka; Nakasako, Masayoshi

2013-02-01

Coherent and intense x-ray pulses generated by x-ray free-electron laser (XFEL) sources are paving the way for structural determination of noncrystalline biomolecules. However, due to the small scattering cross section of electrons for x rays, the available incident x-ray intensity of XFEL sources, which is currently in the range of 10(12)-10(13) photons/μm(2)/pulse, is lower than that necessary to perform single-molecule diffraction experiments for noncrystalline biomolecules even with the molecular masses of megadalton and submicrometer dimensions. Here, we propose an experimental protocol and analysis method for visualizing the structure of those biomolecules by the combined application of coherent x-ray diffraction imaging and three-dimensional reconstruction methods. To compensate the small scattering cross section of biomolecules, in our protocol, a thin vitreous ice plate containing several hundred biomolecules/μm(2) is used as sample, a setup similar to that utilized by single-molecule cryoelectron microscopy. The scattering cross section of such an ice plate is far larger than that of a single particle. The images of biomolecules contained within irradiated areas are then retrieved from each diffraction pattern, and finally provide the three-dimensional electron density model. A realistic atomic simulation using large-scale computations proposed that the three-dimensional structure determination of the 50S ribosomal subunit embedded in a vitreous ice plate is possible at a resolution of 0.8 nm when an x-ray beam of 10(16) photons/500×500 nm(2)/pulse is available.

Development of In-situ Resonant Soft X-ray Scattering for Soft Materials at Advanced Light Source

NASA Astrophysics Data System (ADS)

Wang, Cheng; Hexemer, Alexander; Young, Anthony; Padmore, Howard

2014-03-01

Resonant Soft X-ray Scattering was developed at ALS over the past a few years. It combines soft x-ray spectroscopy with x-ray scattering and offers statistical information for 3D chemical morphology over a large sample area. Its unique chemical sensitivity, large accessible size scale, polarization control and high coherence make it a powerful tool for mesoscale chemical/morphological structure characterization for many classes of materials. However, in order to study sciences in naturally occurring conditions, we need to overcome the sample limitations set by the low penetration depth of soft x-rays and requirement of high vacuum. Adapting to the evolving environmental cell designs utilized increasingly in the Electron Microscopy community, we will report our development of customize design liquid/gas environmental cells that will enable soft x-ray scattering experiments on biological, electro-chemical, self-assembly, and hierarchical functional systems in both static and dynamic fashion. Initial RSoXS result of solar fuel membrane assembly/fuel-cell membrane structure in wet cell will be presented.

Mass-specific scattering coefficient for natural minerogenic particle populations: particle size distribution effect and closure analyses.

PubMed

Peng, Feng; Effler, Steve W

2012-05-01

The relationship between the particulate scattering coefficient (b(p)) and the concentration of suspended particulate matter (SPM), as represented by the mass-specific scattering coefficient of particulates (b(p)*=b(p)/SPM), depends on particle size distribution (PSD). This dependence is quantified for minerogenic particle populations in this paper through calculations of b(p)* for common minerals as idealized populations (monodispersed spheres); contemporaneous measurements of b(p), SPM, and light-scattering attributes of mineral particles with scanning electron microscopy interfaced with automated image and x-ray analyses (SAX), for a connected stream-reservoir system where minerogenic particles dominate b(p); and estimates of b(p) and its size dependency (through SAX results-driven Mie theory calculations), particle volume concentration, and b(p)*. Modest changes in minerogenic PSDs are shown to result in substantial variations in b(p)*. Good closure of the SAX-based estimates of b(p) and particle volume concentration with bulk measurements is demonstrated. Converging relationships between b(p)* and particle size, developed from three approaches, were well described by power law expressions.

Differential dynamic microscopy of bidisperse colloidal suspensions.

PubMed

Safari, Mohammad S; Poling-Skutvik, Ryan; Vekilov, Peter G; Conrad, Jacinta C

2017-01-01

Research tasks in microgravity include monitoring the dynamics of constituents of varying size and mobility in processes such as aggregation, phase separation, or self-assembly. We use differential dynamic microscopy, a method readily implemented with equipment available on the International Space Station, to simultaneously resolve the dynamics of particles of radius 50 nm and 1 μm in bidisperse aqueous suspensions. Whereas traditional dynamic light scattering fails to detect a signal from the larger particles at low concentrations, differential dynamic microscopy exhibits enhanced sensitivity in these conditions by accessing smaller wavevectors where scattering from the large particles is stronger. Interference patterns due to scattering from the large particles induce non-monotonic decay of the amplitude of the dynamic correlation function with the wavevector. We show that the position of the resulting minimum contains information on the vertical position of the particles. Together with the simple instrumental requirements, the enhanced sensitivity of differential dynamic microscopy makes it an appealing alternative to dynamic light scattering to characterize samples with complex dynamics.

The contribution of grain boundary and defects to the resistivity in the ferromagnetic state of polycrystalline manganites

NASA Astrophysics Data System (ADS)

Sagdeo, P. R.; Anwar, Shahid; Lalla, N. P.; Patil, S. I.

2006-11-01

In the present study we report the precise resistivity measurements for the polycrystalline bulk sample as well as highly oriented thin-films of La 0.8Ca 0.2MnO 3. The poly crystalline sample was prepared by standard solid-state reaction route and the oriented thin film was prepared by pulsed laser deposition (PLD). The phase purity of these samples was confirmed by X-ray diffraction and the back-scattered electron imaging using scanning electron microscopy (SEM). The oxygen stoichiometry analysis was done by iodimetry titration. The resistivities of these samples were carried out with four-probe resistivity measurement setup. The observed temperature dependence of resistivity data for both the samples was fitted using the polaron model. We have found that polaronic model fits well with the experimental data of both polycrystalline and single crystal samples. A new phenomenological model is proposed and used to estimate contribution to the resistivity due to grain boundary in the ferromagnetic state of polycrystalline manganites and it has been shown that the scattering of electrons from the grain boundary (grain surface) is a function of temperature and controlled by the effective grain resistance at that temperature.

Electrospun Conjugated Polymer/Fullerene Hybrid Fibers: Photoactive Blends, Conductivity through Tunneling-AFM, Light Scattering, and Perspective for Their Use in Bulk-Heterojunction Organic Solar Cells

DOE PAGES

Yang, Zhenhua; Moffa, Maria; Liu, Ying; ...

2018-01-25

Hybrid conjugated polymer/fullerene filaments based on MEH-PPV/PVP/PCBM were prepared by electrospinning, and their properties were assessed by scanning electron, atomic and lateral-force, tunneling, and confocal microscopies, as well as by attenuated-total-reflection Fourier transform infrared spectroscopy, photoluminescence quantum yield, and spatially resolved fluorescence. Highlighted features include the ribbon shape of the realized fibers and the persistence of a network serving as a template for heterogeneous active layers in solar cell devices. A set of favorable characteristics is evidenced in this way in terms of homogeneous charge-transport behavior and formation of effective interfaces for diffusion and dissociation of photogenerated excitons. The interactionmore » of the organic filaments with light, exhibiting specific light-scattering properties of the nanofibrous mat, might also contribute to spreading incident radiation across the active layers, thus potentially enhancing photovoltaic performance. Finally, this method might be applied to other electron donor–electron acceptor material systems for the fabrication of solar cell devices enhanced by nanofibrillar morphologies embedding conjugated polymers and fullerene compounds.« less

Electrospun Conjugated Polymer/Fullerene Hybrid Fibers: Photoactive Blends, Conductivity through Tunneling-AFM, Light Scattering, and Perspective for Their Use in Bulk-Heterojunction Organic Solar Cells

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

Yang, Zhenhua; Moffa, Maria; Liu, Ying

Hybrid conjugated polymer/fullerene filaments based on MEH-PPV/PVP/PCBM were prepared by electrospinning, and their properties were assessed by scanning electron, atomic and lateral-force, tunneling, and confocal microscopies, as well as by attenuated-total-reflection Fourier transform infrared spectroscopy, photoluminescence quantum yield, and spatially resolved fluorescence. Highlighted features include the ribbon shape of the realized fibers and the persistence of a network serving as a template for heterogeneous active layers in solar cell devices. A set of favorable characteristics is evidenced in this way in terms of homogeneous charge-transport behavior and formation of effective interfaces for diffusion and dissociation of photogenerated excitons. The interactionmore » of the organic filaments with light, exhibiting specific light-scattering properties of the nanofibrous mat, might also contribute to spreading incident radiation across the active layers, thus potentially enhancing photovoltaic performance. Finally, this method might be applied to other electron donor–electron acceptor material systems for the fabrication of solar cell devices enhanced by nanofibrillar morphologies embedding conjugated polymers and fullerene compounds.« less

Scattering of surface electrons by isolated steps versus periodic step arrays

NASA Astrophysics Data System (ADS)

Ortega, J. E.; Lobo-Checa, J.; Peschel, G.; Schirone, S.; Abd El-Fattah, Z. M.; Matena, M.; Schiller, F.; Borghetti, P.; Gambardella, P.; Mugarza, A.

2013-03-01

We investigate the scattering of electrons belonging to Shockley states of (111)-oriented noble metal surfaces using angle-resolved photoemission (ARPES) and scanning tunneling microscopy (STM). Both ARPES and STM indicate that monatomic steps on a noble metal surface may act either as strongly repulsive or highly transmissive barriers for surface electrons, depending on the coherence of the step lattice, and irrespectively of the average step spacing. By measuring curved crystal surfaces with terrace length ranging from 30 to 180 Å, we show that vicinal surfaces of Au and Ag with periodic step arrays exhibit a remarkable wave function coherence beyond 100 Å step spacings, well beyond the Fermi wavelength limit and independently of the projection of the bulk band gap on the vicinal plane. In contrast, the analysis of transmission resonances investigated by STM shows that a pair of isolated parallel steps defining a 58 Å wide terrace confines and decouples the surface state of the small terrace from that of the (111) surface. We conclude that the formation of laterally confined quantum well states in vicinal surfaces as opposed to propagating superlattice states depends on the loss of coherence driven by imperfection in the superlattice order.

Electron back-scattered diffraction and nanoindentation analysis of nanostructured Al tubes processed by multipass tubular-channel angular pressing

NASA Astrophysics Data System (ADS)

Mesbah, Mohsen; Faraji, Ghader; Bushroa, A. R.

2016-03-01

Microstructural evolution and mechanical properties of nanostructured 1060 aluminum alloy tubes processed by tubular-channel angular pressing (TCAP) process were investigated using electron back-scattered diffraction (EBSD), transmission electron microscopy (TEM) and nanoindentation analyzes. EBSD scans revealed a homogeneous ultrafine grained microstructure after the third passes of the TCAP process. Apart from that the mean grain sizes of the TCAP processed tubes were refined to 566 nm, 500 nm and 480 nm respectively after the first, second and third passes. The results showed that after the three TCAP passes, the grain boundaries with a high angle comprised 78% of all the boundaries. This is in comparison to the first pass processed sample that includes approximately 20% HAGBs. The TEM inspection afforded an appreciation of the role of very low-angle misorientation boundaries in the process of refining microstructure. Nanoindentation results showed that hardness was the smallest form of an unprocessed sample while the largest form of the processed sample after the three passes of TCAP indicated the highest resistant of the material. In addition, the module of elasticity of the TCAP processed samples was greater from that of the unprocessed sample.

Evaluation of drug delivery to intact and porated skin by coherent Raman scattering and fluorescence microscopies.

PubMed

Belsey, Natalie A; Garrett, Natalie L; Contreras-Rojas, L Rodrigo; Pickup-Gerlaugh, Adam J; Price, Gareth J; Moger, Julian; Guy, Richard H

2014-01-28

Stimulated Raman scattering microscopy was used to assess the permeation of topically applied drugs and formulation excipients into porcine skin. This chemically selective technique generates high-resolution 3D images, from which semi-quantitative information may be elucidated. Ibuprofen, applied as a close-to-saturated solution in propylene glycol, was directly observed to crystallise in/on the skin, as the co-solvent permeated more rapidly, resulting in precipitation of the drug. Coherent Raman scattering microscopy is also an excellent tool, in conjunction with more conventional confocal fluorescence microscopy, with which to image micro/nanoparticle-based formulations. Specifically, the uptake of particles into thermal ablation transport pathways in the skin has been examined. Copyright © 2013 Elsevier B.V. All rights reserved.

Hepatic Subcellular Compartmentation of Cytoplasmic Phosphoenolpyruvate Carboxykinase Determined by Immunogold Electron Microscopy

NASA Astrophysics Data System (ADS)

Gao, Kuixiong; Cardell, Emma Lou; Morris, Randal E.; Giffin, Bruce F.; Cardell, Robert R.

1995-08-01

Phosphoenolpyruvate carboxykinase (PEPCK) is the rate-limiting gluconeogenic enzyme and in liver occurs in a lobular gradient from periportal to pericentral regions. The subcellular distribution of cytoplasmic PEPCK molecules within hepatocytes and its relationship to organelles have not been determined previously. In this study, we have used immunogold electron microscopy to evaluate the subcellar distribution of the enzyme, in addition to brightfield and epipolarized light microscopy. Cryosections (10 [mu]m) of perfusion-fixed rat liver were collected on silanated slides and immunostained using goat anti-rat PEPCK followed by 5-nm gold-labeled secondary and tertiary antibodies. Additionally, free-floating vibratome sections (25, 50, and 100 [mu]m) of perfusion-immersion-fixed rat liver were immunogold stained using goat anti-rat PEPCK and 5-nm gold-labeled secondary antibody, with and without silver enhancement. The immunogold labeled sections from both procedures were embedded in epoxy resin for the preparation of thin sections for electron microscopy. The results showed that the gold-labeled antibodies penetrated the entire thickness of cryosections, resulting in a high signal for PEPCK, but membranes in general, the smooth endoplasmic reticulum in particular, were not identifiable as electron dense unit membranes. On the other hand, the vibratome sections of well-fixed tissue allowed good visualization of the ultrastructure of cellular organelles, with the smooth endoplasmic reticulum appearing as vesicles and tubules with electron dense unit membranes; however, the penetration of the gold-labeled antibody was limited to cells at the surface of the vibratome sections. In both procedures, PEPCK, as indicated by gold particles, is predominantly in the glycogen areas of the cytosome and not in mitochondria, nuclei, Golgi apparatus, or other cell organelles. Hepatocytes in periportal regions have a compact subcellular distribution of PEPCK shown by gold particles; hepatocytes in pericentral regions have a diffuse subcellular distribution of PEPCK and thus more scattered gold particles. When normal serum replaced the first antibody in the immunogold staining procedures, the background was very low.

Nanoscale imaging of fundamental Li battery chemistry: solid-electrolyte interphase formation and preferential growth of lithium metal nanoclusters

DOE PAGES

Sacci, Robert L; Black, Jennifer M.; Wisinger, Nina; ...

2015-02-23

The performance characteristics of Li-ion batteries are intrinsically linked to evolving nanoscale interfacial electrochemical reactions. To probe the mechanisms of solid electrolyte interphase formation and Li electrodeposition from a standard battery electrolyte, we use in situ electrochemical scanning transmission electron microscopy for controlled potential sweep-hold electrochemical measurements with simultaneous BF and ADF STEM image acquisition. Through a combined quantitative electrochemical measurement and quantitative STEM imaging approach, based upon electron scattering theory, we show that chemically sensitive ADF STEM imaging can be used to estimate the density of evolving SEI constituents and distinguish contrast mechanisms of Li-bearing components in the liquidmore » cell.« less

Mechanisms of grain refinement in aluminum alloys in the process of severe plastic deformation

NASA Astrophysics Data System (ADS)

Kaibyshev, R. O.; Mazurina, I. A.; Gromov, D. A.

2006-01-01

A study of the mechanisms of grain refinement in the process of severe plastic deformation of two aluminum alloys, i.e., 2219 bearing nanometric particles of Al3Zr and low-alloy Al-3% Cu, is described. The alloys are deformed by the method of equal channel angular pressing at 250°C to a maximum strain degree of about 12. The angles of (sub)grain boundaries in alloy 2219 are determined with the help of transmission electron microscopy by the method of Kikuchi lines. The evolution of the microstructure in alloy Al-3% Cu is studied with the help of grain-boundary maps obtained by the method of electron back-scattered diffraction.

Breaking the diffraction barrier using coherent anti-Stokes Raman scattering difference microscopy.

PubMed

Wang, Dong; Liu, Shuanglong; Chen, Yue; Song, Jun; Liu, Wei; Xiong, Maozhen; Wang, Guangsheng; Peng, Xiao; Qu, Junle

2017-05-01

We propose a method to improve the resolution of coherent anti-Stokes Raman scattering microscopy (CARS), and present a theoretical model. The proposed method, coherent anti-Stokes Raman scattering difference microscopy (CARS-D), is based on the intensity difference between two differently acquired images. One being the conventional CARS image, and the other obtained when the sample is illuminated by a doughnut shaped spot. The final super-resolution CARS-D image is constructed by intensity subtraction of these two images. However, there is a subtractive factor between them, and the theoretical model sets this factor to obtain the best imaging effect.

A simple and selective resonance Rayleigh scattering-energy transfer spectral method for determination of trace neomycin sulfate using Cu2O particle as probe

NASA Astrophysics Data System (ADS)

Ouyang, Huixiang; Liang, Aihui; Jiang, Zhiliang

2018-02-01

The stable Cu2O nanocubic (Cu2ONC) sol was prepared, based on graphene oxide (GO) catalysis of glucose-Fehling's reagent reaction, and its absorption and resonance Rayleigh scattering (RRS) spectra, transmission electron microscopy (TEM) and energy dispersive spectroscopy (EDS) were examined. Using the as-prepared Cu2ONC as RRS probe, and coupling with the neomycin sulfate (NEO) complex reaction, a new, simple, sensitive and selective RRS-energy transfer (RRS-ET) method was established for detection of neomycin sulfate, with a linear range of 1.4-112 μM and a detection limit of 0.4 μM. The method has been applied to the detection of neomycin sulfate in samples with satisfactory results.

Dispersed SiC nanoparticles in Ni observed by ultra-small-angle X-ray scattering

DOE PAGES

Xie, R.; Ilavsky, J.; Huang, H. F.; ...

2016-11-24

In this paper, a metal-ceramic composite, nickel reinforced with SiC nanoparticles, was synthesized and characterized for its potential application in next-generation molten salt nuclear reactors. Synchrotron ultra-small-angle X-ray scattering (USAXS) measurements were conducted on the composite. The size distribution and number density of the SiC nanoparticles in the material were obtained through data modelling. Scanning and transmission electron microscopy characterization were performed to substantiate the results of the USAXS measurements. Tensile tests were performed on the samples to measure the change in their yield strength after doping with the nanoparticles. Finally, the average interparticle distance was calculated from the USAXSmore » results and is related to the increased yield strength of the composite.« less

Characterization of oligomerization of a peptide from the ebola virus glycoprotein by small-angle neutron scattering

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

Egorov, V. V., E-mail: vlaegur@omrb.pnpi.spb.ru; Gorshkov, A. N.; Murugova, T. N.

2016-01-15

Transmission electron microscopy (TEM) and small-angle neutron scattering (SANS) studies showed that model peptides QNALVCGLRQ (G33) and QNALVCGLRG (G31) corresponding to region 551–560 of the GP protein of the Sudan Ebola virus are prone to oligomerization in solution. Both peptides can form amyloid-like fibrills. The G33 peptide forms fibrils within one day of incubation, whereas the fibrillogenesis of the G31 peptide is observed only after incubation for several months. The possible role of the observed processes in the pathogenesis and the possibility of applying a combination of the TEM and SANS techniques to search for new compounds that are ablemore » to influence the protein oligomerization are discussed.« less

Theranostic reduction-sensitive gemcitabine prodrug micelles for near-infrared imaging and pancreatic cancer therapy

NASA Astrophysics Data System (ADS)

Han, Haijie; Wang, Haibo; Chen, Yangjun; Li, Zuhong; Wang, Yin; Jin, Qiao; Ji, Jian

2015-12-01

A biodegradable and reduction-cleavable gemcitabine (GEM) polymeric prodrug with in vivo near-infrared (NIR) imaging ability was reported. This theranostic GEM prodrug PEG-b-[PLA-co-PMAC-graft-(IR820-co-GEM)] was synthesized by ring-opening polymerization and ``click'' reaction. The as-prepared reduction-sensitive prodrug could self-assemble into prodrug micelles in aqueous solution confirmed by dynamic light scattering (DLS) and transmission electron microscopy (TEM). In vitro drug release studies showed that these prodrug micelles were able to release GEM in an intracellular-mimicking reductive environment. These prodrug micelles could be effectively internalized by BxPC-3 pancreatic cancer cells, which were observed by confocal laser scanning microscopy (CLSM). Meanwhile, a methyl thiazolyl tetrazolium (MTT) assay demonstrated that this prodrug exhibited high cytotoxicity against BxPC-3 cells. The in vivo whole-animal near-infrared (NIR) imaging results showed that these prodrug micelles could be effectively accumulated in tumor tissue and had a longer blood circulation time than IR820-COOH. The endogenous reduction-sensitive gemcitabine prodrug micelles with the in vivo NIR imaging ability might have great potential in image-guided pancreatic cancer therapy.A biodegradable and reduction-cleavable gemcitabine (GEM) polymeric prodrug with in vivo near-infrared (NIR) imaging ability was reported. This theranostic GEM prodrug PEG-b-[PLA-co-PMAC-graft-(IR820-co-GEM)] was synthesized by ring-opening polymerization and ``click'' reaction. The as-prepared reduction-sensitive prodrug could self-assemble into prodrug micelles in aqueous solution confirmed by dynamic light scattering (DLS) and transmission electron microscopy (TEM). In vitro drug release studies showed that these prodrug micelles were able to release GEM in an intracellular-mimicking reductive environment. These prodrug micelles could be effectively internalized by BxPC-3 pancreatic cancer cells, which were observed by confocal laser scanning microscopy (CLSM). Meanwhile, a methyl thiazolyl tetrazolium (MTT) assay demonstrated that this prodrug exhibited high cytotoxicity against BxPC-3 cells. The in vivo whole-animal near-infrared (NIR) imaging results showed that these prodrug micelles could be effectively accumulated in tumor tissue and had a longer blood circulation time than IR820-COOH. The endogenous reduction-sensitive gemcitabine prodrug micelles with the in vivo NIR imaging ability might have great potential in image-guided pancreatic cancer therapy. Electronic supplementary information (ESI) available. See DOI: 10.1039/c5nr06734k

Improvement of electron mobility in La:BaSnO{sub 3} thin films by insertion of an atomically flat insulating (Sr,Ba)SnO{sub 3} buffer layer

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

Shiogai, Junichi, E-mail: junichi.shiogai@imr.tohoku.ac.jp; Nishihara, Kazuki; Sato, Kazuhisa

One perovskite oxide, ASnO{sub 3} (A = Sr, Ba), is a candidate for use as a transparent conductive oxide with high electron mobility in single crystalline form. However, the electron mobility of films grown on SrTiO{sub 3} substrates does not reach the bulk value, probably because of dislocation scattering that originates from the large lattice mismatch. This study investigates the effect of insertion of bilayer BaSnO{sub 3} / (Sr,Ba)SnO{sub 3} for buffering this large lattice mismatch between La:BaSnO{sub 3} and SrTiO{sub 3} substrate. The insertion of 200-nm-thick BaSnO{sub 3} on (Sr,Ba)SnO{sub 3} bilayer buffer structures reduces the number of dislocationsmore » and improves surface smoothness of the films after annealing as proved respectively by scanning transmission electron microscopy and atomic force microscopy. A systematic investigation of BaSnO{sub 3} buffer layer thickness dependence on Hall mobility of the electron transport in La:BaSnO{sub 3} shows that the highest obtained value of mobility is 78 cm{sup 2}V{sup −1}s{sup −1} because of its fewer dislocations. High electron mobility films based on perovskite BaSnO{sub 3} can provide a good platform for transparent-conducting-oxide electronic devices and for creation of fascinating perovskite heterostructures.« less

Through a Window, Brightly: A Review of Selected Nanofabricated Thin-Film Platforms for Spectroscopy, Imaging, and Detection.

PubMed

Dwyer, Jason R; Harb, Maher

2017-09-01

We present a review of the use of selected nanofabricated thin films to deliver a host of capabilities and insights spanning bioanalytical and biophysical chemistry, materials science, and fundamental molecular-level research. We discuss approaches where thin films have been vital, enabling experimental studies using a variety of optical spectroscopies across the visible and infrared spectral range, electron microscopies, and related techniques such as electron energy loss spectroscopy, X-ray photoelectron spectroscopy, and single molecule sensing. We anchor this broad discussion by highlighting two particularly exciting exemplars: a thin-walled nanofluidic sample cell concept that has advanced the discovery horizons of ultrafast spectroscopy and of electron microscopy investigations of in-liquid samples; and a unique class of thin-film-based nanofluidic devices, designed around a nanopore, with expansive prospects for single molecule sensing. Free-standing, low-stress silicon nitride membranes are a canonical structural element for these applications, and we elucidate the fabrication and resulting features-including mechanical stability, optical properties, X-ray and electron scattering properties, and chemical nature-of this material in this format. We also outline design and performance principles and include a discussion of underlying material preparations and properties suitable for understanding the use of alternative thin-film materials such as graphene.

The architecture of amyloid-like peptide fibrils revealed by X-ray scattering, diffraction and electron microscopy

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

Langkilde, Annette E., E-mail: annette.langkilde@sund.ku.dk; Morris, Kyle L.; Serpell, Louise C.

The aggregation process and the fibril state of an amyloidogenic peptide suggest monomer addition to be the prevailing mechanism of elongation and a model of the peptide packing in the fibrils has been obtained. Structural analysis of protein fibrillation is inherently challenging. Given the crucial role of fibrils in amyloid diseases, method advancement is urgently needed. A hybrid modelling approach is presented enabling detailed analysis of a highly ordered and hierarchically organized fibril of the GNNQQNY peptide fragment of a yeast prion protein. Data from small-angle X-ray solution scattering, fibre diffraction and electron microscopy are combined with existing high-resolution X-raymore » crystallographic structures to investigate the fibrillation process and the hierarchical fibril structure of the peptide fragment. The elongation of these fibrils proceeds without the accumulation of any detectable amount of intermediate oligomeric species, as is otherwise reported for, for example, glucagon, insulin and α-synuclein. Ribbons constituted of linearly arranged protofilaments are formed. An additional hierarchical layer is generated via the pairing of ribbons during fibril maturation. Based on the complementary data, a quasi-atomic resolution model of the protofilament peptide arrangement is suggested. The peptide structure appears in a β-sheet arrangement reminiscent of the β-zipper structures evident from high-resolution crystal structures, with specific differences in the relative peptide orientation. The complexity of protein fibrillation and structure emphasizes the need to use multiple complementary methods.« less

Hyaluronan degrading silica nanoparticles for skin cancer therapy

NASA Astrophysics Data System (ADS)

Scodeller, P.; Catalano, P. N.; Salguero, N.; Duran, H.; Wolosiuk, A.; Soler-Illia, G. J. A. A.

2013-09-01

We report the first nanoformulation of Hyaluronidase (Hyal) and its enhanced adjuvant effect over the free enzyme. Hyaluronic acid (HA) degrading enzyme Hyal was immobilized on 250 nm silica nanoparticles (SiNP) maintaining specific activity of the enzyme via the layer-by-layer self-assembly technique. This process was characterized by dynamic light scattering (DLS), zeta potential, infrared and UV-Vis spectroscopy, transmission electron microscopy (TEM) and enzymatic activity measurements. The nanoparticles were tested in vivo as adjuvants of carboplatin (CP), peritumorally injected in A375 human melanoma bearing mice and compared with the non-immobilized enzyme, on the basis of equal enzymatic activity. Alcian Blue staining of A375 tumors indicated large overexpression of hyaluronan. At the end of the experiment, tumor volume reduction with SiNP-immobilized Hyal was significantly enhanced compared to non-immobilized Hyal. Field emission scanning electron microscopy (FE-SEM) images together with energy dispersive X-ray spectroscopy (EDS) spectra confirmed the presence of SiNP on the tumor. We mean a proof of concept: this extracellular matrix (ECM) degrading enzyme, immobilized on SiNP, is a more effective local adjuvant of cancer drugs than the non-immobilized enzyme. This could prove useful in future therapies using other or a combination of ECM degrading enzymes.We report the first nanoformulation of Hyaluronidase (Hyal) and its enhanced adjuvant effect over the free enzyme. Hyaluronic acid (HA) degrading enzyme Hyal was immobilized on 250 nm silica nanoparticles (SiNP) maintaining specific activity of the enzyme via the layer-by-layer self-assembly technique. This process was characterized by dynamic light scattering (DLS), zeta potential, infrared and UV-Vis spectroscopy, transmission electron microscopy (TEM) and enzymatic activity measurements. The nanoparticles were tested in vivo as adjuvants of carboplatin (CP), peritumorally injected in A375 human melanoma bearing mice and compared with the non-immobilized enzyme, on the basis of equal enzymatic activity. Alcian Blue staining of A375 tumors indicated large overexpression of hyaluronan. At the end of the experiment, tumor volume reduction with SiNP-immobilized Hyal was significantly enhanced compared to non-immobilized Hyal. Field emission scanning electron microscopy (FE-SEM) images together with energy dispersive X-ray spectroscopy (EDS) spectra confirmed the presence of SiNP on the tumor. We mean a proof of concept: this extracellular matrix (ECM) degrading enzyme, immobilized on SiNP, is a more effective local adjuvant of cancer drugs than the non-immobilized enzyme. This could prove useful in future therapies using other or a combination of ECM degrading enzymes. Electronic supplementary information (ESI) available. See DOI: 10.1039/c3nr02787b

Biological imaging with coherent Raman scattering microscopy: a tutorial

PubMed Central

Alfonso-García, Alba; Mittal, Richa; Lee, Eun Seong; Potma, Eric O.

2014-01-01

Abstract. Coherent Raman scattering (CRS) microscopy is gaining acceptance as a valuable addition to the imaging toolset of biological researchers. Optimal use of this label-free imaging technique benefits from a basic understanding of the physical principles and technical merits of the CRS microscope. This tutorial offers qualitative explanations of the principles behind CRS microscopy and provides information about the applicability of this nonlinear optical imaging approach for biological research. PMID:24615671

Crystallographic orientation inhomogeneity and crystal splitting in biogenic calcite

PubMed Central

Checa, Antonio G.; Bonarski, Jan T.; Willinger, Marc G.; Faryna, Marek; Berent, Katarzyna; Kania, Bogusz; González-Segura, Alicia; Pina, Carlos M.; Pospiech, Jan; Morawiec, Adam

2013-01-01

The calcitic prismatic units forming the outer shell of the bivalve Pinctada margaritifera have been analysed using scanning electron microscopy–electron back-scatter diffraction, transmission electron microscopy and atomic force microscopy. In the initial stages of growth, the individual prismatic units are single crystals. Their crystalline orientation is not consistent but rather changes gradually during growth. The gradients in crystallographic orientation occur mainly in a direction parallel to the long axis of the prism, i.e. perpendicular to the shell surface and do not show preferential tilting along any of the calcite lattice axes. At a certain growth stage, gradients begin to spread and diverge, implying that the prismatic units split into several crystalline domains. In this way, a branched crystal, in which the ends of the branches are independent crystalline domains, is formed. At the nanometre scale, the material is composed of slightly misoriented domains, which are separated by planes approximately perpendicular to the c-axis. Orientational gradients and splitting processes are described in biocrystals for the first time and are undoubtedly related to the high content of intracrystalline organic molecules, although the way in which these act to induce the observed crystalline patterns is a matter of future research. PMID:23804442

Electrical characterization of HgTe nanowires using conductive atomic force microscopy

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

Gundersen, P.; Department of Physics, Norwegian University of Science and Technology, NO-7491 Trondheim; Kongshaug, K. O.

Self-organized HgTe nanowires grown by molecular beam epitaxy (MBE) have been characterized using conductive atomic force microscopy. As HgTe will degrade or evaporate at normal baking temperatures for electron beam lithography (EBL) resists, an alternative method was developed. Using low temperature optical lithography processes, large Au contacts were deposited on a sample covered with randomly oriented, lateral HgTe nanowires. Nanowires partly covered by the large electrodes were identified with a scanning electron microscope and then localized in the atomic force microscope (AFM). The conductive tip of the AFM was then used as a movable electrode to measure current-voltage curves atmore » several locations on HgTe nanowires. The measurements revealed that polycrystalline nanowires had diffusive electron transport, with resistivities two orders of magnitude larger than that of an MBE-grown HgTe film. The difference can be explained by scattering at the rough surface walls and at the grain boundaries in the wires. The method can be a solution when EBL is not available or requires too high temperature, or when measurements at several positions along a wire are required.« less

Electronic, vibrational, Raman, and scanning tunneling microscopy signatures of two-dimensional boron nanomaterials

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

Massote, Daniel V. P.; Liang, Liangbo; Kharche, Neerav

Compared to graphene, the synthesis of large area atomically thin boron materials is particularly challenging, owing to the electronic shell structure of B, which does not lend itself to the straightforward assembly of pure B materials. This difficulty is evidenced by the fact that the first synthesis of a pure two-dimensional boron was only very recently reported, using silver as a growing substrate. In addition to experimentally observed 2D boron allotropes, a number of other stable and metastable 2D boron materials are predicted to exist, depending on growth conditions and the use of a substrate during growth. This first-principles studymore » based on density functional theory aims at providing guidelines for the identification of these materials. To this end, this report presents a comparative description of a number of possible 2D B allotropes. Electronic band structures, phonon dispersion curves, Raman scattering spectra, and scanning tunneling microscopy images are simulated to highlight the differences between five distinct realizations of these B systems. In conclusion, this study demonstrates the existence of clear experimental signatures that constitute a solid basis for the unambiguous experimental identification of layered B materials.« less

Electronic, vibrational, Raman, and scanning tunneling microscopy signatures of two-dimensional boron nanomaterials

DOE PAGES

Massote, Daniel V. P.; Liang, Liangbo; Kharche, Neerav; ...

2016-11-11

Compared to graphene, the synthesis of large area atomically thin boron materials is particularly challenging, owing to the electronic shell structure of B, which does not lend itself to the straightforward assembly of pure B materials. This difficulty is evidenced by the fact that the first synthesis of a pure two-dimensional boron was only very recently reported, using silver as a growing substrate. In addition to experimentally observed 2D boron allotropes, a number of other stable and metastable 2D boron materials are predicted to exist, depending on growth conditions and the use of a substrate during growth. This first-principles studymore » based on density functional theory aims at providing guidelines for the identification of these materials. To this end, this report presents a comparative description of a number of possible 2D B allotropes. Electronic band structures, phonon dispersion curves, Raman scattering spectra, and scanning tunneling microscopy images are simulated to highlight the differences between five distinct realizations of these B systems. In conclusion, this study demonstrates the existence of clear experimental signatures that constitute a solid basis for the unambiguous experimental identification of layered B materials.« less

Microstructure, crystallography and nucleation mechanism of NANOBAIN steel

NASA Astrophysics Data System (ADS)

Huang, Yao; Zhao, Ai-min; He, Jian-guo; Wang, Xiao-pei; Wang, Zhi-gang; Qi, Liang

2013-12-01

The microstructure of bainite ferrite in NANOBAIN steel transformed at different temperatures was investigated by scanning electron microscopy, transmission electron microscopy, electron back-scattered diffraction, and vickers hardness tester in detail. It is found that the average width of bainitic ferrite (BF) plates can be refined to be thinner with the reduction of temperature (473-573 K), and the bainitic ferrite plates can reach up to 20-74 nm at 473 K. Crystallographic analysis reveals that the bainitic ferrite laths are close to the Nishiyama-Wasserman orientation relationship with their parent austenite. Temperature shows a significant effect on the variant selection, and a decrease in temperature generally weakens the variant selection. Thermodynamic analyses indicates that the Lacher, Fowler and Guggenheim (LFG) model is more suitable than the Kaufman, Radcliffe and Cohen (KRC) model dealing with NANOBAIN steel at a low temperature range. The free energy change Δ G γ→BF is about -1500 J·mol-1 at 473 K, which indicates that nucleation in NANOBAIN steel is the shear mechanism. Finally, the formation of carbon poor regions is thermodynamically possible, and the existence of carbon poor regions can greatly increase the possibility of the shear mechanism.

Ag/CuO nanoparticles prepared from a novel trinuclear compound [Cu(Imdz)4(Ag(CN)2)2] (Imdz = imidazole) by a pyrolysis display excellent antimicrobial activity

NASA Astrophysics Data System (ADS)

Adhikary, Jaydeep; Das, Balaram; Chatterjee, Sourav; Dash, Sandeep Kumar; Chattopadhyay, Sourav; Roy, Somenath; Chen, Jeng-Wei; Chattopadhyay, Tanmay

2016-06-01

One copper and two silver containing one hetero tri-nuclear precursor compound [Cu(Imdz)4(Ag(CN)2)2] (1) (Imdz = Imidazole) has been synthesized and characterized by single crystal X-ray diffraction. Simple pyrolysis of the complex at 550 °C for 4 h afforded Ag/CuO nanoparticles (NPs). The synthesized nanoparticles were characterized by ultraviolet-visible (UV-Vis), Fourier transform infrared (FT-IR), X-ray powder diffraction (XRPD), dynamic light scattering (DLS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray (EDX) and X-ray photo electron spectroscopy (XPS). Staphylococcus aureus (S. aureus) and Escherichia coli (E. coli) have been employed as model microbial species to study the anti-microbial activity of the synthesized NPs. The NPs showed potent anti-microbial activity evidenced from the Minimum Inhibitory Concentration (MIC) and Minimum Bactericidal Concentration (MBC) values. Very high level of cell uptake and then generation of reactive oxygen species (ROS) are the origin of such strong antimicrobial activity for the NPs. However, the cytotoxicity level of the NPs towards normal human cell is very low.

Structural evolution of detonation carbon in composition B by X-ray scattering

DOE PAGES

Firestone, Millicent A.; Dattelbaum, Dana M.; Podlesak, David W.; ...

2015-01-01

Products evolved during the detonation of high explosives are primarily a collection of molecular gases and solid carbon condensates. Electron microscopy studies have revealed that detonation carbon (soot) can contain a variety of unique carbon particles possessing novel morphologies, such as carbon onions and ribbons. Despite these observations very little is known about the conditions that leads to the production of these novel carbon nanoparticles. A fuller understanding on conditions that generate such nanoparticles would greatly benefit from time-resolved studies that probe particle formation and evolution through and beyond the chemical reaction zone. Herein, we report initial results employing time-resolvedmore » X-ray scattering (TRSAXS) measurements to monitor nanosecond time-scale carbon products formed from detonating Composition B (60% TNT, 40% RDX). These studies were performed at the Dynamic Compression Sector (DCS, Sector 35) at the Advanced Photon Source (Argonne National Laboratory). Lastly, analysis of the collected scattering patterns reveals the presence of fractal multi-layered carbon condensates.« less

Effect of annealing conditions on the microstructure and magnetic properties of sintered Nd-Fe-B magnets as seen by magnetic small-angle neutron scattering

NASA Astrophysics Data System (ADS)

Périgo, Élio A.; Titov, Ivan; Weber, Raoul; Mettus, Denis; Peral, Inma; Vallcorba, Oriol; Honecker, Dirk; Feoktystov, Artem; Michels, Andreas

2018-03-01

We have investigated the effect of the annealing conditions (heating rate and temperature) on the magnetic microstructure of sintered Nd-Fe-B magnets by means of magnetometry, scanning electron microscopy, high-energy synchrotron x-ray diffraction, and small-angle neutron scattering (SANS). While the temperature treatment has a strong effect on the coercivity (reduction by about 50% on annealing), the associated changes in the microstructure do surprisingly not show up (or at best only very weakly) in the neutron-scattering signal, which probes a mesoscopic real-space length scale ranging between about 1–300 nm. On the other hand, the x-ray data reveal microstructural changes in the Nd-rich phases, presumably due to modifications in grain-boundary regions. Moreover, we observe an unusual diamond-shaped angular anisotropy in the SANS cross section, which strongly points towards the existence of texture in the nuclear microstructure.

Structural evolution of detonation carbon in composition B by X-ray scattering

NASA Astrophysics Data System (ADS)

Firestone, Millicent A.; Dattelbaum, Dana M.; Podlesak, David W.; Gustavsen, Richard L.; Huber, Rachel C.; Ringstrand, Bryan S.; Watkins, Erik B.; Jensen, Brian; Willey, Trevor; Lauderbauch, Lisa; Hodgin, Ralph; Bagge-Hansen, Michael; van Buuren, Tony; Seifert, Sönke; Graber, Timothy

2017-01-01

Products evolved during the detonation of high explosives are primarily a collection of molecular gases and solid carbon condensates. Electron microscopy studies have revealed that detonation carbon (soot) can contain a variety of unique carbon particles possessing novel morphologies, such as carbon onions and ribbons. Despite these observations very little is known about the conditions that leads to the production of these novel carbon nanoparticles. A fuller understanding on conditions that generate such nanoparticles would greatly benefit from time-resolved studies that probe particle formation and evolution through and beyond the chemical reaction zone. Herein, we report initial results employing time-resolved X-ray scattering (TRSAXS) measurements to monitor nanosecond time-scale carbon products formed from detonating Composition B (60% TNT, 40% RDX). These studies were performed at the Dynamic Compression Sector (DCS, Sector 35) at the Advanced Photon Source (Argonne National Laboratory). Analysis of the collected scattering patterns reveals the presence of fractal multi-layered carbon condensates.

Resolution of ab initio shapes determined from small-angle scattering.

PubMed

Tuukkanen, Anne T; Kleywegt, Gerard J; Svergun, Dmitri I

2016-11-01

Spatial resolution is an important characteristic of structural models, and the authors of structures determined by X-ray crystallography or electron cryo-microscopy always provide the resolution upon publication and deposition. Small-angle scattering of X-rays or neutrons (SAS) has recently become a mainstream structural method providing the overall three-dimensional structures of proteins, nucleic acids and complexes in solution. However, no quantitative resolution measure is available for SAS-derived models, which significantly hampers their validation and further use. Here, a method is derived for resolution assessment for ab initio shape reconstruction from scattering data. The inherent variability of the ab initio shapes is utilized and it is demonstrated how their average Fourier shell correlation function is related to the model resolution. The method is validated against simulated data for proteins with known high-resolution structures and its efficiency is demonstrated in applications to experimental data. It is proposed that henceforth the resolution be reported in publications and depositions of ab initio SAS models.

Resolution of ab initio shapes determined from small-angle scattering

PubMed Central

Tuukkanen, Anne T.; Kleywegt, Gerard J.; Svergun, Dmitri I.

2016-01-01

Spatial resolution is an important characteristic of structural models, and the authors of structures determined by X-ray crystallography or electron cryo-microscopy always provide the resolution upon publication and deposition. Small-angle scattering of X-rays or neutrons (SAS) has recently become a mainstream structural method providing the overall three-dimensional structures of proteins, nucleic acids and complexes in solution. However, no quantitative resolution measure is available for SAS-derived models, which significantly hampers their validation and further use. Here, a method is derived for resolution assessment for ab initio shape reconstruction from scattering data. The inherent variability of the ab initio shapes is utilized and it is demonstrated how their average Fourier shell correlation function is related to the model resolution. The method is validated against simulated data for proteins with known high-resolution structures and its efficiency is demonstrated in applications to experimental data. It is proposed that henceforth the resolution be reported in publications and depositions of ab initio SAS models. PMID:27840683

Electric field imaging of single atoms

PubMed Central

Shibata, Naoya; Seki, Takehito; Sánchez-Santolino, Gabriel; Findlay, Scott D.; Kohno, Yuji; Matsumoto, Takao; Ishikawa, Ryo; Ikuhara, Yuichi

2017-01-01

In scanning transmission electron microscopy (STEM), single atoms can be imaged by detecting electrons scattered through high angles using post-specimen, annular-type detectors. Recently, it has been shown that the atomic-scale electric field of both the positive atomic nuclei and the surrounding negative electrons within crystalline materials can be probed by atomic-resolution differential phase contrast STEM. Here we demonstrate the real-space imaging of the (projected) atomic electric field distribution inside single Au atoms, using sub-Å spatial resolution STEM combined with a high-speed segmented detector. We directly visualize that the electric field distribution (blurred by the sub-Å size electron probe) drastically changes within the single Au atom in a shape that relates to the spatial variation of total charge density within the atom. Atomic-resolution electric field mapping with single-atom sensitivity enables us to examine their detailed internal and boundary structures. PMID:28555629

Red-luminescent europium (III) doped silica nanoshells: synthesis, characterization, and their interaction with HeLa cells

NASA Astrophysics Data System (ADS)

Yang, Jian; Sandoval, Sergio; Alfaro, Jesus G.; Aschemeyer, Sharraya; Liberman, Alex; Martin, David T.; Makale, Milan; Kummel, Andrew C.; Trogler, William C.

2011-06-01

A simple method to fabricate Eu3+ doped silica nanoshells particles with 100 and 200 nm diameters is reported. Amino polystyrene beads were used as templates, and an 8 to 10 nm thick silica gel coating was formed by the sol-gel reaction. After removing the template by calcination, porous dehydrated silica gel nanoshells of uniform size were obtained. The Eu3+ doped silica nanoshells exhibited a red emission at 615 nm on UV excitation. The porous structure of the silica shell wall was characterized by transmission electron microscopy measurements, while particle size and zeta potentials of the particles suspended in aqueous solution were characterized by dynamic light scattering. Two-photon microscopy was used to image the nanoshells after assimilation by HeLa cancer cells.

Atomic oxygen effects on thin film space coatings studied by spectroscopic ellipsometry, atomic force microscopy, and laser light scattering

NASA Technical Reports Server (NTRS)

Synowicki, R. A.; Hale, Jeffrey S.; Woollam, John A.

1992-01-01

The University of Nebraska is currently evaluating Low Earth Orbit (LEO) simulation techniques as well as a variety of thin film protective coatings to withstand atomic oxygen (AO) degradation. Both oxygen plasma ashers and an electron cyclotron resonance (ECR) source are being used for LEO simulation. Thin film coatings are characterized by optical techniques including Variable Angle Spectroscopic Ellipsometry, Optical spectrophotometry, and laser light scatterometry. Atomic Force Microscopy (AFM) is also used to characterize surface morphology. Results on diamondlike carbon (DLC) films show that DLC degrades with simulated AO exposure at a rate comparable to Kapton polyimide. Since DLC is not as susceptible to environmental factors such as moisture absorption, it could potentially provide more accurate measurements of AO fluence on short space flights.

Microscopy and microRaman study of periodically poled domains in deeply thinned lithium niobate wafers

NASA Astrophysics Data System (ADS)

Bullen, P. S.; Huang, H.-C.; Yang, H.; Dadap, J. I.; Kymissis, I.; Osgood, R. M.

2016-07-01

The domain structure of poled deeply thinned lithium niobate is investigated as a function of sample thickness. Free-standing samples of thickness from 25 to 500 μm are prepared by a multiple-cycle polish and annealing procedure and then periodically poled. Using these samples and employing micro-Raman scattering and scanning electron, atomic force, and optical microscopy together, the domain broadening and poling voltage are found to vary in a regular and significant manner. The poled domains show a reduction in width spreading of 38% as the sample thickness is reduced from 500 to 25 μm. Micro-Raman probe measurements verify the quality and the uniformity of the poled domains and provide insight into their thickness-dependent poling contrast.

Cations Modulate Actin Bundle Mechanics, Assembly Dynamics, and Structure.

PubMed

Castaneda, Nicholas; Zheng, Tianyu; Rivera-Jacquez, Hector J; Lee, Hyun-Ju; Hyun, Jaekyung; Balaeff, Alexander; Huo, Qun; Kang, Hyeran

2018-04-12

Actin bundles are key factors in the mechanical support and dynamic reorganization of the cytoskeleton. High concentrations of multivalent counterions promote bundle formation through electrostatic attraction between actin filaments that are negatively charged polyelectrolytes. In this study, we evaluate how physiologically relevant divalent cations affect the mechanical, dynamic, and structural properties of actin bundles. Using a combination of total internal reflection fluorescence microscopy, transmission electron microscopy, and dynamic light scattering, we demonstrate that divalent cations modulate bundle stiffness, length distribution, and lateral growth. Molecular dynamics simulations of an all-atom model of the actin bundle reveal specific actin residues coordinate cation-binding sites that promote the bundle formation. Our work suggests that specific cation interactions may play a fundamental role in the assembly, structure, and mechanical properties of actin bundles.

Synthesis of strongly fluorescent molybdenum disulfide nanosheets for cell-targeted labeling.

PubMed

Wang, Nan; Wei, Fang; Qi, Yuhang; Li, Hongxiang; Lu, Xin; Zhao, Guoqiang; Xu, Qun

2014-11-26

MoS2 nanosheets with polydispersity of the lateral dimensions from natural mineral molybdenite have been prepared in the emulsions microenvironment built by the water/surfactant/CO2 system. The size, thickness, and atomic structure are characterized by transmission electron microscopy (TEM), atomic force microscopy (AFM), and laser-scattering particle size analysis. Meanwhile, by the analysis of photoluminescence spectroscopy and microscope, the MoS2 nanosheets with smaller lateral dimensions exhibit extraordinary photoluminescence properties different from those with relatively larger lateral dimensions. The discovery of the excitation dependent photoluminescence for MoS2 nanosheets makes them potentially of interests for the applications in optoelectronics and biology. Moreover, we demonstrate that the fabricated MoS2 nanosheets can be a nontoxic fluorescent label for cell-targeted labeling application.

Synthesis of poly(3-hydroxybutyrate) nanospheres and deposition thereof into porous thin film

NASA Astrophysics Data System (ADS)

Abid, S.; Raza, Z. A.; Rehman, A.

2016-10-01

Polymeric nanostructures have gained importance in medical science as drug delivery carriers due to their biocompatibility and biodegradability. Polyhydroxybutyrate (PHB) is one of the natural biodegradable polymers used to deliver drugs in the form of nano/microcapsules. In this study, solvent evaporation method has been used for the synthesis of PHB nanospheres using poly(vinyl) alcohol (PVA) both as emulsifier and stabilizer. The produced PHB nanospheres were analyzed using dynamic light scattering and scanning electron microscopy. The size of nanospheres decreased whereas the zeta potential increased on increasing the concentration of emulsifier. The PHB nanospheres were then deposited into porous thin film on a glass surface and characterized against bulk PHB film by using atomic force microscopy, contact angle measurement and x-ray diffraction.

Raman enhancement by graphene-Ga2O3 2D bilayer film

PubMed Central

2014-01-01

2D β-Ga2O3 flakes on a continuous 2D graphene film were prepared by a one-step chemical vapor deposition on liquid gallium surface. The composite was characterized by optical microscopy, scanning electron microscopy, Raman spectroscopy, energy dispersive spectroscopy, and X-ray photoelectron spectroscopy (XPS). The experimental results indicate that Ga2O3 flakes grew on the surface of graphene film during the cooling process. In particular, tenfold enhancement of graphene Raman scattering signal was detected on Ga2O3 flakes, and XPS indicates the C-O bonding between graphene and Ga2O3. The mechanism of Raman enhancement was discussed. The 2D Ga2O3-2D graphene structure may possess potential applications. PMID:24472433

Reversible Stabilization of Vesicles: Redox-Responsive Polymer Nanocontainers for Intracellular Delivery.

PubMed

de Vries, Wilke C; Grill, David; Tesch, Matthias; Ricker, Andrea; Nüsse, Harald; Klingauf, Jürgen; Studer, Armido; Gerke, Volker; Ravoo, Bart Jan

2017-08-01

We present the self-assembly of redox-responsive polymer nanocontainers comprising a cyclodextrin vesicle core and a thin reductively cleavable polymer shell anchored via host-guest recognition on the vesicle surface. The nanocontainers are of uniform size, show high stability, and selectively respond to a mild reductive trigger as revealed by dynamic light scattering, transmission electron microscopy, atomic force microscopy, a quantitative thiol assay, and fluorescence spectroscopy. Live cell imaging experiments demonstrate a specific redox-responsive release and cytoplasmic delivery of encapsulated hydrophilic payloads, such as the pH-probe pyranine, and the fungal toxin phalloidin. Our results show the high potential of these stimulus-responsive nanocontainers for cell biological applications requiring a controlled delivery. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Lung cancer diagnosis with quantitative DIC microscopy and support vector machine

NASA Astrophysics Data System (ADS)

Zheng, Longfei; Cai, Shuangshuang; Zeng, Bixin; Xu, Min

2017-01-01

We report the study of lung squamous cell carcinoma diagnosis using the TI-DIC microscopy and the scattering-phase theorem. The spatially resolved optical properties of tissue are computed from the 2D phase map via the scattering-phase theorem. The scattering coefficient, the reduced scattering coefficient, and the anisotropy factor are all found to increase with the grade of lung cancer. The retrieved optical parameters are shown to distinguish cancer cases from the normal cases with high accuracy. This label-free microscopic approach applicable to fresh tissues may be promising for in situ rapid cancer diagnosis.

Coherent Raman Scattering Microscopy in Biology and Medicine.

PubMed

Zhang, Chi; Zhang, Delong; Cheng, Ji-Xin

2015-01-01

Advancements in coherent Raman scattering (CRS) microscopy have enabled label-free visualization and analysis of functional, endogenous biomolecules in living systems. When compared with spontaneous Raman microscopy, a key advantage of CRS microscopy is the dramatic improvement in imaging speed, which gives rise to real-time vibrational imaging of live biological samples. Using molecular vibrational signatures, recently developed hyperspectral CRS microscopy has improved the readout of chemical information available from CRS images. In this article, we review recent achievements in CRS microscopy, focusing on the theory of the CRS signal-to-noise ratio, imaging speed, technical developments, and applications of CRS imaging in bioscience and clinical settings. In addition, we present possible future directions that the use of this technology may take.

Coherent Raman Scattering Microscopy in Biology and Medicine

PubMed Central

Zhang, Chi; Zhang, Delong; Cheng, Ji-Xin

2016-01-01

Advancements in coherent Raman scattering (CRS) microscopy have enabled label-free visualization and analysis of functional, endogenous biomolecules in living systems. When compared with spontaneous Raman microscopy, a key advantage of CRS microscopy is the dramatic improvement in imaging speed, which gives rise to real-time vibrational imaging of live biological samples. Using molecular vibrational signatures, recently developed hyperspectral CRS microscopy has improved the readout of chemical information available from CRS images. In this article, we review recent achievements in CRS microscopy, focusing on the theory of the CRS signal-to-noise ratio, imaging speed, technical developments, and applications of CRS imaging in bioscience and clinical settings. In addition, we present possible future directions that the use of this technology may take. PMID:26514285

Live-cell stimulated Raman scattering imaging of alkyne-tagged biomolecules.

PubMed

Hong, Senlian; Chen, Tao; Zhu, Yuntao; Li, Ang; Huang, Yanyi; Chen, Xing

2014-06-02

Alkynes can be metabolically incorporated into biomolecules including nucleic acids, proteins, lipids, and glycans. In addition to the clickable chemical reactivity, alkynes possess a unique Raman scattering within the Raman-silent region of a cell. Coupling this spectroscopic signature with Raman microscopy yields a new imaging modality beyond fluorescence and label-free microscopies. The bioorthogonal Raman imaging of various biomolecules tagged with an alkyne by a state-of-the-art Raman imaging technique, stimulated Raman scattering (SRS) microscopy, is reported. This imaging method affords non-invasiveness, high sensitivity, and molecular specificity and therefore should find broad applications in live-cell imaging. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Biophysical characterization of influenza virus subpopulations using field flow fractionation and multiangle light scattering: correlation of particle counts, size distribution and infectivity.

PubMed

Wei, Ziping; McEvoy, Matt; Razinkov, Vladimir; Polozova, Alla; Li, Elizabeth; Casas-Finet, Jose; Tous, Guillermo I; Balu, Palani; Pan, Alfred A; Mehta, Harshvardhan; Schenerman, Mark A

2007-09-01

Adequate biophysical characterization of influenza virions is important for vaccine development. The influenza virus vaccines are produced from the allantoic fluid of developing chicken embryos. The process of viral replication produces a heterogeneous mixture of infectious and non-infectious viral particles with varying states of aggregation. The study of the relative distribution and behavior of different subpopulations and their inter-correlation can assist in the development of a robust process for a live virus vaccine. This report describes a field flow fractionation and multiangle light scattering (FFF-MALS) method optimized for the analysis of size distribution and total particle counts. The FFF-MALS method was compared with several other methods such as transmission electron microscopy (TEM), atomic force microscopy (AFM), size exclusion chromatography followed by MALS (SEC-MALS), quantitative reverse transcription polymerase chain reaction (RT Q-PCR), median tissue culture dose (TCID(50)), and the fluorescent focus assay (FFA). The correlation between the various methods for determining total particle counts, infectivity and size distribution is reported. The pros and cons of each of the analytical methods are discussed.

High quality gold nanorods and nanospheres for surface-enhanced Raman scattering detection of 2,4-dichlorophenoxyacetic acid

NASA Astrophysics Data System (ADS)

Jia, Jin-Liang; Xu, Han-Hong; Zhang, Gui-Rong; Hu, Zhun; Xu, Bo-Qing

2012-12-01

Nearly monodisperse Au nanorods (NRs) with different aspect ratios were separated from home-synthesized polydisperse samples using a gradient centrifugation method. The morphology, size and its distribution, and photo-absorption property were analyzed by transmission electron microscopy, atomic force microscopy and UV-visible spectroscopy. Subsequently, using colloidal Au NRs (36.2 nm ×10.7 nm) with 97.4% yield after centrifugation and Au nanospheres (NSs) (22.9 ± 1.0 nm in diameter) with 97.6% yield as Au substrates, surface-enhanced Raman scattering (SERS) spectra of 2,4-dichlorophenoxyacetic acid (2,4-D) were recorded using laser excitation at 632.8 nm. Results show that surface enhancement factors (EF) for Au NRs and NSs are 6.2 × 105 and 5.7 × 104 using 1.0 × 10-6 M 2,4-D, respectively, illustrating that EF value is a factor of ˜10 greater for Au NRs substrates than for Au NSs substrates. As a result, large EF are a mainly result of chemical enhancement mechanisms. Thus, it is expected that Au NPs can find a comprehensive SERS application in the trace detection of pesticide residues.

High quality gold nanorods and nanospheres for surface-enhanced Raman scattering detection of 2,4-dichlorophenoxyacetic acid.

PubMed

Jia, Jin-Liang; Xu, Han-Hong; Zhang, Gui-Rong; Hu, Zhun; Xu, Bo-Qing

2012-12-14

Nearly monodisperse Au nanorods (NRs) with different aspect ratios were separated from home-synthesized polydisperse samples using a gradient centrifugation method. The morphology, size and its distribution, and photo-absorption property were analyzed by transmission electron microscopy, atomic force microscopy and UV-visible spectroscopy. Subsequently, using colloidal Au NRs (36.2 nm ×10.7 nm) with 97.4% yield after centrifugation and Au nanospheres (NSs) (22.9 ± 1.0 nm in diameter) with 97.6% yield as Au substrates, surface-enhanced Raman scattering (SERS) spectra of 2,4-dichlorophenoxyacetic acid (2,4-D) were recorded using laser excitation at 632.8 nm. Results show that surface enhancement factors (EF) for Au NRs and NSs are 6.2 × 10(5) and 5.7 × 10(4) using 1.0 × 10(-6) M 2,4-D, respectively, illustrating that EF value is a factor of ~10 greater for Au NRs substrates than for Au NSs substrates. As a result, large EF are a mainly result of chemical enhancement mechanisms. Thus, it is expected that Au NPs can find a comprehensive SERS application in the trace detection of pesticide residues.

Application of different analytical methods for the characterization of non-spherical micro- and nanoparticles.

PubMed

Mathaes, Roman; Winter, Gerhard; Engert, Julia; Besheer, Ahmed

2013-09-10

Non-spherical micro- and nanoparticles have recently gained considerable attention due to their surprisingly different interaction with biological systems compared to their spherical counterparts, opening new opportunities for drug delivery and vaccination. Up till now, electron microscopy is the only method to quantitatively identify the critical quality attributes (CQAs) of non-spherical particles produced by film-stretching; namely size, morphology and the quality of non-spherical particles (degree of contamination with spherical ones). However, electron microscopy requires expensive instrumentation, demanding sample preparation and non-trivial image analysis. To circumvent these drawbacks, the ability of different particle analysis methods to quantitatively identify the CQA of spherical and non-spherical poly(1-phenylethene-1,2-diyl (polystyrene) particles over a wide size range (40 nm, 2 μm and 10 μm) was investigated. To this end, light obscuration, image-based analysis methods (Microflow imaging, MFI, and Vi-Cell XR Coulter Counter) and flow cytometry were used to study particles in the micron range, while asymmetric flow field fractionation (AF4) coupled to multi-angle laser scattering (MALS) and quasi elastic light scattering (QELS) was used for particles in the nanometer range, and all measurements were benchmarked against electron microscopy. Results show that MFI can reliably identify particle size and aspect ratios of the 10 μm particles, but not the 2 μm ones. Meanwhile, flow cytometry was able to differentiate between spherical and non-spherical 10 or 2 μm particles, and determine the amount of impurities in the sample. As for the nanoparticles, AF4 coupled to MALS and QELS allowed the measurement of the geometric (rg) and hydrodynamic (rh) radii of the particles, as well as their shape factors (rg/rh), confirming their morphology. While this study shows the utility of MFI, flow cytometry and AF4 for quantitative evaluation of the CQA of non-spherical particles over a wide size range, the limitations of the methods are discussed. The use of orthogonal characterization methods can provide a complete picture about the CQA of non-spherical particles over a wide size range. Copyright © 2013 Elsevier B.V. All rights reserved.

Histological and morphological observations on tongue of Scincella tsinlingensis (Reptilia, Squamata, Scincidae).

PubMed

Yang, Chun; Wang, Limin

2016-01-01

The histology and morphology characteristics of the tongue in Scincella tsinlingensis were studied by light and electronic microscopy. Under light microscopy, the tongue consists of tip, lingual body and radix in sequence. Numerous lingual papillae widely distribute on the surface of the dorsal and ventral flanks in the tongue, in addition to some regions of the tip. The papillae's surface is covered with the epithelial layer. The lamina propria and dense connective tissue are distinct existing under the epithelial layer. There are many lingual glands spread over the lamina propria. Tongue muscle is developed and composed of distinct intrinsic muscle, hyoglossus and genioglossus. By scanning electron microscopy, at higher magnification, the epithelial cells of the dorsal surface in the divaricate tongue tips show numerous microvilli, micro-ridges and micro-pores. The surface of dorsal side of the papillae in lingual body is covered with abundant of micro-ridges and taste bud lacuna. On the surface of the papillae in radix, micro-facets and micro-ridges are compactly distributed, as well as scattered mucilage-pores. The lingual epithelium is divided into four layers observed by the transmission electron microscope. Cells of basal layer are irregularly elliptical in shape, with sparse organelles in the cytoplasm. The deep intermediate layer is not always distinct. Small numbers of organelles are scattered into the cytoplasm. The cells of the superficial intermediate layer gradually flatten, as do their nuclei. The cytoplasm contains many keratohyalin granules. Cell membranes are formed processes around cells and joined by abundant desmosomes to the cell membranes of adjacent cells. The cells located on the extreme free-surface side of the keratinized layer have fallen off. The basal lamina is intercalated between the basal layer and the lamina propria. The lamina propria of lingual body contains lingual gland. A large part of the cytoplasm is occupied by mucus granules which located in the distal part of the cell. The connective tissue contains myelinated nerve fibers, vessel and muscle cells. Copyright © 2015 Elsevier Ltd. All rights reserved.

Electron scattering by molecules. II - Experimental methods and data

NASA Technical Reports Server (NTRS)

Trajmar, S.; Chutjian, A.; Register, D. F.

1983-01-01

Experimental techniques for measuring electron-molecule collision cross sections are briefly summarized. A survey of the available experimental cross section data is presented. The emphasis here is on elastic scattering, rotational, vibrational and electronic excitations, total electron scattering, and momentum transfer in the few eV to few hundred eV impact energy range. Reference is made to works concerned with high energy electron scattering, innershell and multi-electron excitations, conicidence methods and electron scattering in laser fields.

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.

Simulation of transmission electron microscope images of biological specimens.

PubMed

Rullgård, H; Ofverstedt, L-G; Masich, S; Daneholt, B; Oktem, O

2011-09-01

We present a new approach to simulate electron cryo-microscope images of biological specimens. The framework for simulation consists of two parts; the first is a phantom generator that generates a model of a specimen suitable for simulation, the second is a transmission electron microscope simulator. The phantom generator calculates the scattering potential of an atomic structure in aqueous buffer and allows the user to define the distribution of molecules in the simulated image. The simulator includes a well defined electron-specimen interaction model based on the scalar Schrödinger equation, the contrast transfer function for optics, and a noise model that includes shot noise as well as detector noise including detector blurring. To enable optimal performance, the simulation framework also includes a calibration protocol for setting simulation parameters. To test the accuracy of the new framework for simulation, we compare simulated images to experimental images recorded of the Tobacco Mosaic Virus (TMV) in vitreous ice. The simulated and experimental images show good agreement with respect to contrast variations depending on dose and defocus. Furthermore, random fluctuations present in experimental and simulated images exhibit similar statistical properties. The simulator has been designed to provide a platform for development of new instrumentation and image processing procedures in single particle electron microscopy, two-dimensional crystallography and electron tomography with well documented protocols and an open source code into which new improvements and extensions are easily incorporated. © 2011 The Authors Journal of Microscopy © 2011 Royal Microscopical Society.

Merging single-shot XFEL diffraction data from inorganic nanoparticles: a new approach to size and orientation determination

DOE PAGES

Li, Xuanxuan; Spence, John C. H.; Hogue, Brenda G.; ...

2017-09-22

X-ray free-electron lasers (XFELs) provide new opportunities for structure determination of biomolecules, viruses and nanomaterials. With unprecedented peak brilliance and ultra-short pulse duration, XFELs can tolerate higher X-ray doses by exploiting the femtosecond-scale exposure time, and can thus go beyond the resolution limits achieved with conventional X-ray diffraction imaging techniques. Using XFELs, it is possible to collect scattering information from single particles at high resolution, however particle heterogeneity and unknown orientations complicate data merging in three-dimensional space. Using the Linac Coherent Light Source (LCLS), synthetic inorganic nanocrystals with a core–shell architecture were used as a model system for proof-of-principle coherentmore » diffractive single-particle imaging experiments. To deal with the heterogeneity of the core–shell particles, new computational methods have been developed to extract the particle size and orientation from the scattering data to assist data merging. The size distribution agrees with that obtained by electron microscopy and the merged data support a model with a core–shell architecture.« less

Merging single-shot XFEL diffraction data from inorganic nanoparticles: a new approach to size and orientation determination

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

Li, Xuanxuan; Spence, John C. H.; Hogue, Brenda G.

X-ray free-electron lasers (XFELs) provide new opportunities for structure determination of biomolecules, viruses and nanomaterials. With unprecedented peak brilliance and ultra-short pulse duration, XFELs can tolerate higher X-ray doses by exploiting the femtosecond-scale exposure time, and can thus go beyond the resolution limits achieved with conventional X-ray diffraction imaging techniques. Using XFELs, it is possible to collect scattering information from single particles at high resolution, however particle heterogeneity and unknown orientations complicate data merging in three-dimensional space. Using the Linac Coherent Light Source (LCLS), synthetic inorganic nanocrystals with a core–shell architecture were used as a model system for proof-of-principle coherentmore » diffractive single-particle imaging experiments. To deal with the heterogeneity of the core–shell particles, new computational methods have been developed to extract the particle size and orientation from the scattering data to assist data merging. The size distribution agrees with that obtained by electron microscopy and the merged data support a model with a core–shell architecture.« less

Structural and electronic properties of graphene nanoflakes on Au(111) and Ag(111)

PubMed Central

Tesch, Julia; Leicht, Philipp; Blumenschein, Felix; Gragnaniello, Luca; Fonin, Mikhail; Marsoner Steinkasserer, Lukas Eugen; Paulus, Beate; Voloshina, Elena; Dedkov, Yuriy

2016-01-01

We investigate the electronic properties of graphene nanoflakes on Ag(111) and Au(111) surfaces by means of scanning tunneling microscopy and spectroscopy as well as density functional theory calculations. Quasiparticle interference mapping allows for the clear distinction of substrate-derived contributions in scattering and those originating from graphene nanoflakes. Our analysis shows that the parabolic dispersion of Au(111) and Ag(111) surface states remains unchanged with the band minimum shifted to higher energies for the regions of the metal surface covered by graphene, reflecting a rather weak interaction between graphene and the metal surface. The analysis of graphene-related scattering on single nanoflakes yields a linear dispersion relation E(k), with a slight p-doping for graphene/Au(111) and a larger n-doping for graphene/Ag(111). The obtained experimental data (doping level, band dispersions around EF, and Fermi velocity) are very well reproduced within DFT-D2/D3 approaches, which provide a detailed insight into the site-specific interaction between graphene and the underlying substrate. PMID:27002297

Spall damage of a Ta particle-reinforced metallic glass matrix composite under high strain rate loading

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

Tang, X. C.; Jian, W. R.; Huang, J. Y.

We investigate deformation and damage of a Zr-based bulk metallic glass (BMG) and its Ta particle-reinforced composite (MGMC) under impact loading, as well as quasi-static tension for comparison. Yield strength, spall strength, and damage accumulation rate are obtained from free-surface velocity histories, and MGMC appears to be more damage-resistant. Scanning electron microscopy, electron back scattering diffraction and x-ray computed tomography, are utilized for characterizing microstructures, which show features consistent with macroscopic measurements. Different damage and fracture modes are observed for BMG and MGMC. Multiple well-defined spall planes are observed in BMG, while isolated and scattered cracking around reinforced particles dominatesmore » fracture of MGMC. Particle–matrix interface serves as the source and barrier to crack nucleation and propagation under both quasi-static and impact loading. Finally, deformation twinning and grain refinement play a key role in plastic deformation during shock loading but not in quasi-static loading. In addition, 3D cup-cone structures are resolved in BMG, but not in MGMC due to its heterogeneous stress field.« less

A Mott insulator continuously connected to iron pnictide superconductors

DOE PAGES

Song, Yu; Yamani, Zahra; Cao, Chongde; ...

2016-12-19

Iron-based superconductivity develops near an antiferromagnetic order and out of a bad-metal normal state, which has been interpreted as originating from a proximate Mott transition. Whether an actual Mott insulator can be realized in the phase diagram of the iron pnictides remains an open question. Here we use transport, transmission electron microscopy, X-ray absorption spectroscopy, resonant inelastic X-ray scattering and neutron scattering to demonstrate that NaFe 1-xCu xAs near x≈0.5 exhibits real space Fe and Cu ordering, and are antiferromagnetic insulators with the insulating behaviour persisting above the Néel temperature, indicative of a Mott insulator. On decreasing x from 0.5,more » the antiferromagnetic-ordered moment continuously decreases, yielding to superconductivity ~x=0.05. Our discovery of a Mott-insulating state in NaFe 1-xCu xAs thus makes it the only known Fe-based material, in which superconductivity can be smoothly connected to the Mott-insulating state, highlighting the important role of electron correlations in the high-T c superconductivity.« less

A Mott insulator continuously connected to iron pnictide superconductors

PubMed Central

Song, Yu; Yamani, Zahra; Cao, Chongde; Li, Yu; Zhang, Chenglin; Chen, Justin S.; Huang, Qingzhen; Wu, Hui; Tao, Jing; Zhu, Yimei; Tian, Wei; Chi, Songxue; Cao, Huibo; Huang, Yao-Bo; Dantz, Marcus; Schmitt, Thorsten; Yu, Rong; Nevidomskyy, Andriy H.; Morosan, Emilia; Si, Qimiao; Dai, Pengcheng

2016-01-01

Iron-based superconductivity develops near an antiferromagnetic order and out of a bad-metal normal state, which has been interpreted as originating from a proximate Mott transition. Whether an actual Mott insulator can be realized in the phase diagram of the iron pnictides remains an open question. Here we use transport, transmission electron microscopy, X-ray absorption spectroscopy, resonant inelastic X-ray scattering and neutron scattering to demonstrate that NaFe1−xCuxAs near x≈0.5 exhibits real space Fe and Cu ordering, and are antiferromagnetic insulators with the insulating behaviour persisting above the Néel temperature, indicative of a Mott insulator. On decreasing x from 0.5, the antiferromagnetic-ordered moment continuously decreases, yielding to superconductivity ∼x=0.05. Our discovery of a Mott-insulating state in NaFe1−xCuxAs thus makes it the only known Fe-based material, in which superconductivity can be smoothly connected to the Mott-insulating state, highlighting the important role of electron correlations in the high-Tc superconductivity. PMID:27991514

Spall damage of a Ta particle-reinforced metallic glass matrix composite under high strain rate loading

DOE PAGES

Tang, X. C.; Jian, W. R.; Huang, J. Y.; ...

2017-11-11

We investigate deformation and damage of a Zr-based bulk metallic glass (BMG) and its Ta particle-reinforced composite (MGMC) under impact loading, as well as quasi-static tension for comparison. Yield strength, spall strength, and damage accumulation rate are obtained from free-surface velocity histories, and MGMC appears to be more damage-resistant. Scanning electron microscopy, electron back scattering diffraction and x-ray computed tomography, are utilized for characterizing microstructures, which show features consistent with macroscopic measurements. Different damage and fracture modes are observed for BMG and MGMC. Multiple well-defined spall planes are observed in BMG, while isolated and scattered cracking around reinforced particles dominatesmore » fracture of MGMC. Particle–matrix interface serves as the source and barrier to crack nucleation and propagation under both quasi-static and impact loading. Finally, deformation twinning and grain refinement play a key role in plastic deformation during shock loading but not in quasi-static loading. In addition, 3D cup-cone structures are resolved in BMG, but not in MGMC due to its heterogeneous stress field.« less

The Effect of a Two-Stage Heat-Treatment on the Microstructural and Mechanical Properties of a Maraging Steel

PubMed Central

Sun, Lin; Galvin, Deri Rhys; Hill, Paul; Rawson, Martin; Gilbert, Elliot Paul; Bhadeshia, Harshad; Perkins, Karen

2017-01-01

Maraging steels gain many of their beneficial properties from heat treatments which induce the precipitation of intermetallic compounds. We consider here a two-stage heat-treatment, first involving austenitisation, followed by quenching to produce martensite and then an ageing treatment at a lower temperature to precipitation harden the martensite of a maraging steel. It is shown that with a suitable choice of the initial austenitisation temperature, the steel can be heat treated to produce enhanced toughness, strength and creep resistance. A combination of small angle neutron scattering, scanning electron microscopy, electron back-scattered diffraction, and atom probe tomography were used to relate the microstructural changes to mechanical properties. It is shown that such a combination of characterisation methods is necessary to quantify this complex alloy, and relate these microstructural changes to mechanical properties. It is concluded that a higher austenitisation temperature leads to a greater volume fraction of smaller Laves phase precipitates formed during ageing, which increase the strength and creep resistance but reduces toughness. PMID:29168800

Synthesis and characterization of PEG-P(MAA-SS-VCL) nanoparticles

NASA Astrophysics Data System (ADS)

Yu, L. L.; Yang, K.; Mu, R. H.; Zhang, N.; Su, L.

2016-07-01

The PEG-P(MAA-SS-VCL) nanoparticles were obtained using disulfide containing dimethacrylate (SS) as cross-linking agent, using polyethylene glycol methyl acrylate (PEGMA), N-Vinyl-ε-caprolactam (VCL), and methacrylic acid (MAA) as monomers via homogeneous polymerization in aqueous. The PEG-P(MAA-SS-VCL) nanoparticles were characterized by FT-IR and TGA. The particle size and morphology variation in different environments were detected by dynamic light scattering (DLS) and scanning electron microscopy (SEM). It is the very method that PEG-P(MAA-SS-VCL) nanoparticles can be obtained in this study.

On the crystallization of amorphous germanium films

NASA Astrophysics Data System (ADS)

Edelman, F.; Komem, Y.; Bendayan, M.; Beserman, R.

1993-06-01

The incubation time for crystallization of amorphous Ge (a-Ge) films, deposited by e-gun, was studied as a function of temperature between 150 and 500°C by means of both in situ transmission electron microscopy and Raman scattering spectroscopy. The temperature dependence of t0 follows an Arrhenius curve with an activation energy of 2.0 eV for free-sustained a-Ge films. In the case where the a-Ge films were on Si 3N 4 substrate, the activation energy of the incubation process was 1.3 eV.

Design of titania nanotube structures by focused laser beam direct writing

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

Enachi, Mihai; Stevens-Kalceff, Marion A.; Sarua, Andrei

In this work, we report on electrochemical fabrication of titania films consisting of nanotubes (NTs) and their treatment by focused laser beam. The results of sample characterization by optical and scanning electron microscopy, cathodoluminescence imaging, and Raman scattering scanning spectroscopy are compared to those inherent to specimens subjected to thermal treatment in a furnace. The obtained data demonstrate possibilities for controlling crystallographic structure of TiO{sub 2} NTs by focused laser beam direct writing. These findings open new prospects for the design and fabrication of spatial architectures based on titania nanotubes.

Structure, transport and photoconductance of PbS quantum dot monolayers functionalized with a copper phthalocyanine derivative.

PubMed

André, A; Theurer, C; Lauth, J; Maiti, S; Hodas, M; Samadi Khoshkhoo, M; Kinge, S; Meixner, A J; Schreiber, F; Siebbeles, L D A; Braun, K; Scheele, M

2017-01-31

We simultaneously surface-functionalize PbS nanocrystals with Cu 4,4',4'',4'''-tetraaminophthalocyanine and assemble this hybrid material into macroscopic monolayers. Electron microscopy and X-ray scattering reveal a granular mesocrystalline structure with strong coherence between the atomic lattice and the superlattice of nanocrystals within each domain. Terahertz spectroscopy and field-effect transistor measurements indicate efficient coupling of holes throughout the hybrid thin film, in conjunction with a pronounced photoresponse. We demonstrate the potential of this material for optoelectronic applications by fabricating a light-effect transistor.

Corrosion and degradation of a polyurethane/Co-Ni-Cr-Mo pacemaker lead

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

Sung, P.; Fraker, A.C.

1987-12-01

An investigation to study changes in the metal surfaces and the polyurethane insulation of heart pacemaker leads under controlled in vitro conditions was conducted. A polyurethane (Pellethane 2363-80A)/Co-Ni-Cr-Mo (MP35N) wire lead was exposed in Hanks' physiological saline solution for 14 months and then analyzed using scanning electron microscopy, x-ray energy dispersive analysis, and small angle x-ray scattering. Results showed that some leakage of solution into the lead had occurred and changes were present on both the metal and the polyurethane surfaces.

Axonal inclusions in the crab Hemigrapsus nudus.

PubMed

Smith, R S

1978-10-01

Light microscopic examination of living giant axons from the walking legs of Hemigrapsus nudus revealed intra-axonal inclusions which were usually several tens of micrometers long and about 5 micron wide. The inclusions were filled with small light-scattering particles. The inclusions were shown, by thin section electron microscopy, to be composed largely 68% by volume) of mitochondria. Each inclusion was surrounded by membrane bounded spaces which are presumed to represent a part of the smooth endoplasmic reticulum. Similar inclusions were not found in the leg axons of a variety of other decapod crustaceans.

International Conference (4th) on Nanostructured Materials Held in Stockholm, Sweden on 14-19 June 1998. Special Volume - Part A. Volume 12, Numbers 1-4, 1999

DTIC Science & Technology

1998-06-19

correlation was found between the X - ray grain size and the TEM grain size. Table 2 contains the hardness and density data for the nanocrystalline 5083...temperature with a Neophot hardness tester and a load of 0.2 N. RESULTS AND DISCUSSION X - ray diffraction and transmission electron microscopy combined with...For Single- Wall Carbon Nanotubes by Raman Scattering Technique Microstructure Change in Co46AI19035 Granular Thin Films by Annealing X - Ray

Shape-dependent bactericidal activity of copper oxide nanoparticle mediated by DNA and membrane damage

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

Laha, Dipranjan; Pramanik, Arindam; Laskar, Aparna

Highlights: • Spherical and sheet shaped copper oxide nanoparticles were synthesized. • Physical characterizations of these nanoparticles were done by TEM, DLS, XRD, FTIR. • They showed shape dependent antibacterial activity on different bacterial strain. • They induced both membrane damage and ROS mediated DNA damage in bacteria. - Abstract: In this work, we synthesized spherical and sheet shaped copper oxide nanoparticles and their physical characterizations were done by the X-ray diffraction, fourier transform infrared spectroscopy, transmission electron microscopy and dynamic light scattering. The antibacterial activity of these nanoparticles was determined on both gram positive and gram negative bacterial. Sphericalmore » shaped copper oxide nanoparticles showed more antibacterial property on gram positive bacteria where as sheet shaped copper oxide nanoparticles are more active on gram negative bacteria. We also demonstrated that copper oxide nanoparticles produced reactive oxygen species in both gram negative and gram positive bacteria. Furthermore, they induced membrane damage as determined by atomic force microscopy and scanning electron microscopy. Thus production of and membrane damage are major mechanisms of the bactericidal activity of these copper oxide nanoparticles. Finally it was concluded that antibacterial activity of nanoparticles depend on physicochemical properties of copper oxide nanoparticles and bacterial strain.« less

Nanogel-based natural polymers as smart carriers for the controlled delivery of Timolol Maleate through the cornea for glaucoma.

PubMed

Ilka, Roya; Mohseni, Mojdeh; Kianirad, Mehran; Naseripour, Masood; Ashtari, Khadijeh; Mehravi, Bita

2018-04-01

Despite frequent scientific efforts, efficient ocular drug delivery is a major challenge for pharmaceutical scientists. Poor bioavailability of ophthalmic solutions can be overcome by using smart ophthalmic drug-delivery systems. In this research, loading and delivery of Timolol Maleate (TM) through the cornea by synthesized nanoparticles based on biopolymers (chitosan-alginate) were studied. The physico-chemical properties of these nanoparticles were characterized using scanning electron microscopy (SEM), transmission electron microscopy (TEM) and dynamic light scattering (DLS). Loading and release were evaluated by a UV-vis spectrometer and the ex vivo permeation study was carried out using the Franz Diffusion Cell and fluorescent microscopy studies. The results indicated that morphology and size of nanoparticles were spherical and in the range of 80-100nm. The loading capacity and encapsulation efficiency were about 42% and 94% respectively. They illustrated a burst release in the first hour followed by a slower and more sustained drug release during the next 24h. Also, the results indicated that the cornea penetration of TM loaded in nanoparticles was twice than that of TM. Hence, this nanocarrier can be considered as a suitable candidate for controlled TM delivery and release through the cornea. Copyright © 2017 Elsevier B.V. All rights reserved.

Nano titania aided clustering and adhesion of beneficial bacteria to plant roots to enhance crop growth and stress management.

PubMed

Palmqvist, N G M; Bejai, S; Meijer, J; Seisenbaeva, G A; Kessler, V G

2015-05-13

A novel use of Titania nanoparticles as agents in the nano interface interaction between a beneficial plant growth promoting bacterium (Bacillus amyloliquefaciens UCMB5113) and oilseed rape plants (Brassica napus) for protection against the fungal pathogen Alternaria brassicae is presented. Two different TiO2 nanoparticle material were produced by the Sol-Gel approach, one using the patented Captigel method and the other one applying TiBALDH precursor. The particles were characterized by transmission electron microscopy, thermogravimetric analysis, X-ray diffraction, dynamic light scattering and nano particle tracking analysis. Scanning electron microscopy showed that the bacterium was living in clusters on the roots and the combined energy-dispersive X-ray spectroscopy analysis revealed that titanium was present in these cluster formations. Confocal laser scanning microscopy further demonstrated an increased bacterial colonization of Arabidopsis thaliana roots and a semi-quantitative microscopic assay confirmed an increased bacterial adhesion to the roots. An increased amount of adhered bacteria was further confirmed by quantitative fluorescence measurements. The degree of infection by the fungus was measured and quantified by real-time-qPCR. Results showed that Titania nanoparticles increased adhesion of beneficial bacteria on to the roots of oilseed rape and protected the plants against infection.

Nano titania aided clustering and adhesion of beneficial bacteria to plant roots to enhance crop growth and stress management

NASA Astrophysics Data System (ADS)

Palmqvist, N. G. M.; Bejai, S.; Meijer, J.; Seisenbaeva, G. A.; Kessler, V. G.

2015-05-01

A novel use of Titania nanoparticles as agents in the nano interface interaction between a beneficial plant growth promoting bacterium (Bacillus amyloliquefaciens UCMB5113) and oilseed rape plants (Brassica napus) for protection against the fungal pathogen Alternaria brassicae is presented. Two different TiO2 nanoparticle material were produced by the Sol-Gel approach, one using the patented Captigel method and the other one applying TiBALDH precursor. The particles were characterized by transmission electron microscopy, thermogravimetric analysis, X-ray diffraction, dynamic light scattering and nano particle tracking analysis. Scanning electron microscopy showed that the bacterium was living in clusters on the roots and the combined energy-dispersive X-ray spectroscopy analysis revealed that titanium was present in these cluster formations. Confocal laser scanning microscopy further demonstrated an increased bacterial colonization of Arabidopsis thaliana roots and a semi-quantitative microscopic assay confirmed an increased bacterial adhesion to the roots. An increased amount of adhered bacteria was further confirmed by quantitative fluorescence measurements. The degree of infection by the fungus was measured and quantified by real-time-qPCR. Results showed that Titania nanoparticles increased adhesion of beneficial bacteria on to the roots of oilseed rape and protected the plants against infection.

Nano titania aided clustering and adhesion of beneficial bacteria to plant roots to enhance crop growth and stress management

PubMed Central

Palmqvist, N. G. M.; Bejai, S.; Meijer, J.; Seisenbaeva, G. A.; Kessler, V. G.

2015-01-01

A novel use of Titania nanoparticles as agents in the nano interface interaction between a beneficial plant growth promoting bacterium (Bacillus amyloliquefaciens UCMB5113) and oilseed rape plants (Brassica napus) for protection against the fungal pathogen Alternaria brassicae is presented. Two different TiO2 nanoparticle material were produced by the Sol-Gel approach, one using the patented Captigel method and the other one applying TiBALDH precursor. The particles were characterized by transmission electron microscopy, thermogravimetric analysis, X-ray diffraction, dynamic light scattering and nano particle tracking analysis. Scanning electron microscopy showed that the bacterium was living in clusters on the roots and the combined energy-dispersive X-ray spectroscopy analysis revealed that titanium was present in these cluster formations. Confocal laser scanning microscopy further demonstrated an increased bacterial colonization of Arabidopsis thaliana roots and a semi-quantitative microscopic assay confirmed an increased bacterial adhesion to the roots. An increased amount of adhered bacteria was further confirmed by quantitative fluorescence measurements. The degree of infection by the fungus was measured and quantified by real-time-qPCR. Results showed that Titania nanoparticles increased adhesion of beneficial bacteria on to the roots of oilseed rape and protected the plants against infection. PMID:25970693

Enzymatic formation of gold nanoparticles by submerged culture of the basidiomycete Lentinus edodes.

PubMed

Vetchinkina, Elena P; Loshchinina, Ekaterina A; Burov, Andrey M; Dykman, Lev A; Nikitina, Valentina E

2014-07-20

We report for the first time that the medicinal basidiomycete Lentinus edodes can reduce Au(III) from chloroauric acid (HAuCl4) to elemental Au [Au(0)], forming nanoparticles. Several methods, including transmission electron microscopy, electron energy loss spectroscopy, X-ray fluorescence, and dynamic light scattering, were used to show that when the fungus was grown submerged, colloidal gold accumulated on the surface of and inside the mycelial hyphae as electron-dense particles mostly spherical in shape, with sizes ranging from 5 to 50nm. Homogeneous proteins (the fungal enzymes laccase, tyrosinase, and Mn-peroxidase) were found for the first time to be involved in the reduction of Au(III) to Au(0) from HAuCl4. A possible mechanism forming Au nanoparticles is discussed. Copyright © 2014 Elsevier B.V. All rights reserved.

In Situ and In Vivo Molecular Analysis by Coherent Raman Scattering Microscopy

PubMed Central

Liao, Chien-Sheng; Cheng, Ji-Xin

2017-01-01

Coherent Raman scattering (CRS) microscopy is a high-speed vibrational imaging platform with the ability to visualize the chemical content of a living specimen by using molecular vibrational fingerprints. We review technical advances and biological applications of CRS microscopy. The basic theory of CRS and the state-of-the-art instrumentation of a CRS microscope are presented. We further summarize and compare the algorithms that are used to separate the Raman signal from the nonresonant background, to denoise a CRS image, and to decompose a hyperspectral CRS image into concentration maps of principal components. Important applications of single-frequency and hyperspectral CRS microscopy are highlighted. Potential directions of CRS microscopy are discussed. PMID:27306307

Nanocapsules: The Weapons for Novel Drug Delivery Systems

PubMed Central

Kothamasu, Pavankumar; Kanumur, Hemanth; Ravur, Niranjan; Maddu, Chiranjeevi; Parasuramrajam, Radhika; Thangavel, Sivakumar

2012-01-01

Introduction Nanocapsules, existing in miniscule size, range from 10 nm to 1000 nm. They consist of a liquid/solid core in which the drug is placed into a cavity, which is surrounded by a distinctive polymer membrane made up of natural or synthetic polymers. They have attracted great interest, because of the protective coating, which are usually pyrophoric and easily oxidized and delay the release of active ingredients. Methods Various technical approaches are utilized for obtaining the nanocapsules; however, the methods of interfacial polymerization for monomer and the nano-deposition for preformed polymer are chiefly preferred. Most important characteristics in their preparation is particle size and size distribution which can be evaluated by using various techniques like X-ray diffraction, scanning electron microscopy, transmission electron microscopy, high-resolu¬tion transmission electron microscopy, X-ray photoelectron spectroscopy, superconducting quantum interference device, multi angle laser light scattering and other spectroscopic techniques. Results Nanocapsules possessing extremely high reproducibility have a broad range of life science applications. They may be applied in agrochemicals, genetic engineering, cosmetics, cleansing products, wastewater treatments, adhesive component applications, strategic delivery of the drug in tumors, nanocapsule bandages to fight infec¬tion, in radiotherapy and as liposomal nanocapsules in food science and agriculture. In addition, they can act as self-healing materials. Conclusion The enhanced delivery of bio¬active molecules through the targeted delivery by means of a nanocapsule opens numerous challenges and opportunities for the research and future development of novel improved therapies. PMID:23678444

Nanocapsules: the weapons for novel drug delivery systems.

PubMed

Kothamasu, Pavankumar; Kanumur, Hemanth; Ravur, Niranjan; Maddu, Chiranjeevi; Parasuramrajam, Radhika; Thangavel, Sivakumar

2012-01-01

Nanocapsules, existing in miniscule size, range from 10 nm to 1000 nm. They consist of a liquid/solid core in which the drug is placed into a cavity, which is surrounded by a distinctive polymer membrane made up of natural or synthetic polymers. They have attracted great interest, because of the protective coating, which are usually pyrophoric and easily oxidized and delay the release of active ingredients. Various technical approaches are utilized for obtaining the nanocapsules; however, the methods of interfacial polymerization for monomer and the nano-deposition for preformed polymer are chiefly preferred. Most important characteristics in their preparation is particle size and size distribution which can be evaluated by using various techniques like X-ray diffraction, scanning electron microscopy, transmission electron microscopy, high-resolu¬tion transmission electron microscopy, X-ray photoelectron spectroscopy, superconducting quantum interference device, multi angle laser light scattering and other spectroscopic techniques. Nanocapsules possessing extremely high reproducibility have a broad range of life science applications. They may be applied in agrochemicals, genetic engineering, cosmetics, cleansing products, wastewater treatments, adhesive component applications, strategic delivery of the drug in tumors, nanocapsule bandages to fight infec¬tion, in radiotherapy and as liposomal nanocapsules in food science and agriculture. In addition, they can act as self-healing materials. The enhanced delivery of bio¬active molecules through the targeted delivery by means of a nanocapsule opens numerous challenges and opportunities for the research and future development of novel improved therapies.

Profiling of back-scattered electrons in opposed magnetic field of a Twin Electron Beam Gun

NASA Astrophysics Data System (ADS)

Sethi, S.; Gupta, Anchal; Dileep Kumar, V.; Mukherjee, Jaya; Gantayet, L. M.

2012-11-01

Electron gun is extensively used in material processing, physical vapour deposition and atomic vapour based laser processes. In these processes where the electron beam is incident on the substrate, a significant fraction of electron beam gets back-scattered from the target surface. The trajectory of this back scattered electron beam depends on the magnetic field in the vicinity. The fraction of back-scattered depends on the atomic number of the target metal and can be as high as ~40% of the incident beam current. These back-scattered electrons can cause undesired hot spots and also affect the overall process. Hence, the study of the trajectory of these back-scattered electrons is important. This paper provides the details of experimentally mapped back-scattered electrons of a 2×20kW Twin Electron Beam Gun (TEBG) in opposed magnetic field i.e. with these guns placed at 180° to each other.

Resonant antenna probes for tip-enhanced infrared near-field microscopy.

PubMed

Huth, Florian; Chuvilin, Andrey; Schnell, Martin; Amenabar, Iban; Krutokhvostov, Roman; Lopatin, Sergei; Hillenbrand, Rainer

2013-03-13

We report the development of infrared-resonant antenna probes for tip-enhanced optical microscopy. We employ focused-ion-beam machining to fabricate high-aspect ratio gold cones, which replace the standard tip of a commercial Si-based atomic force microscopy cantilever. Calculations show large field enhancements at the tip apex due to geometrical antenna resonances in the cones, which can be precisely tuned throughout a broad spectral range from visible to terahertz frequencies by adjusting the cone length. Spectroscopic analysis of these probes by electron energy loss spectroscopy, Fourier transform infrared spectroscopy, and Fourier transform infrared near-field spectroscopy corroborates their functionality as resonant antennas and verifies the broad tunability. By employing the novel probes in a scattering-type near-field microscope and imaging a single tobacco mosaic virus (TMV), we experimentally demonstrate high-performance mid-infrared nanoimaging of molecular absorption. Our probes offer excellent perspectives for optical nanoimaging and nanospectroscopy, pushing the detection and resolution limits in many applications, including nanoscale infrared mapping of organic, molecular, and biological materials, nanocomposites, or nanodevices.

Determining the size of nanoparticles in the example of magnetic iron oxide core-shell systems

NASA Astrophysics Data System (ADS)

Jarzębski, Maciej; Kościński, Mikołaj; Białopiotrowicz, Tomasz

2017-08-01

The size of nanoparticles is one of the most important factors for their possible applications. Various techniques for the nanoparticle size characterization are available. In this paper selected techniques will be considered base on the prepared core-shell magnetite nanoparticles. Magnetite is one of the most investigated and developed magnetic material. It shows interesting magnetic properties which can be used for biomedical applications, such as drug delivery, hypothermia and also as a contrast agent. To reduce the toxic effects of Fe3O4, magnetic core was covered by dextran and gelatin. Moreover, the shell was doped by fluorescent dye for confocal microscopy investigation. The main investigation focused on the methods for particles size determination of modified magnetite nanoparticles prepared with different techniques. The size distribution were obtained by nanoparticle tracking analysis, dynamic light scattering and transmission electron microscopy. Furthermore, fluorescent correlation spectroscopy (FCS) and confocal microscopy were used to compare the results for particle size determination of core-shell systems.

Spatiotemporal focusing-based widefield multiphoton microscopy for fast optical sectioning of thick tissues

NASA Astrophysics Data System (ADS)

Cheng, Li-Chung; Chang, Chia-Yuan; Yen, Wei-Chung; Chen, Shean-Jen

2012-10-01

Conventional multiphoton microscopy employs beam scanning; however, in this study a microscope based on spatiotemporal focusing offering widefield multiphoton excitation has been developed to provide fast optical sectioning images. The microscope integrates a 10 kHz repetition rate ultrafast amplifier featuring strong instantaneous peak power (maximum 400 μJ/pulse at 90 fs pulse width) with a TE-cooled, ultra-sensitive photon detecting, electron multiplying charge-coupled device camera. This configuration can produce multiphoton excited images with an excitation area larger than 200 × 100 μm2 at a frame rate greater than 100 Hz. Brownian motions of fluorescent microbeads as small as 0.5 μm have been instantaneously observed with a lateral spatial resolution of less than 0.5 μm and an axial resolution of approximately 3.5 μm. Moreover, we combine the widefield multiphoton microscopy with structure illuminated technique named HiLo to reject the background scattering noise to get better quality for bioimaging.

Determination of the mean inner potential of cadmium telluride via electron holography

NASA Astrophysics Data System (ADS)

Cassidy, C.; Dhar, A.; Shintake, T.

2017-04-01

Mean inner potential is a fundamental material parameter in solid state physics and electron microscopy and has been experimentally measured in CdTe, a technologically important semiconductor. As a first step, the inelastic mean free path for electron scattering in CdTe was determined, using electron energy loss spectroscopy, to enable precise thickness mapping of thin CdTe lamellae. The obtained value was λi(CdTe, 300 kV) = 192 ± 10 nm. This value is relatively large, given the high density of the material, and is discussed in the text. Next, electron diffraction and specimen tilting were employed to identify weakly diffracting lattice orientations, to enable the straightforward measurement of the electron phase shift. Finally, electron holography was utilized to quantitatively map the phase shift experienced by electron waves passing through a CdTe crystal, with several different propagation vectors. Utilization of both thickness and phase data allowed computation of mean inner potential as V0 (CdTe) = 14.0 ± 0.9 V, within the range of previous theoretical estimates.

Effect of particle size on the UV pulsed-laser scribing in computational fluid dynamics-based simulations

NASA Astrophysics Data System (ADS)

Park, Kwan-Woo; Na, Suck-Joo

2010-06-01

A computational model for UV pulsed-laser scribing of silicon target is presented and compared with experimental results. The experiments were performed with a high-power Q-switched diode-pumped solid state laser which was operated at 355 nm. They were conducted on n-type 500 μm thick silicon wafers. The scribing width and depth were measured using scanning electron microscopy. The model takes into account major physics, such as heat transfer, evaporation, multiple reflections, and Rayleigh scattering. It also considers the attenuation and redistribution of laser energy due to Rayleigh scattering. Especially, the influence of the average particle sizes in the model is mainly investigated. Finally, it is shown that the computational model describing the laser scribing of silicon is valid at an average particle size of about 10 nm.

Transformation from Multilamellar to Unilamellar Vesicles by Addition of a Cationic Lipid to PEGylated Liposomes Explored with Synchrotron Small Angle X-ray Scattering

NASA Astrophysics Data System (ADS)

Sakuragi, Mina; Koiwai, Kazunori; Nakamura, Kouji; Masunaga, Hiroyasu; Ogawa, Hiroki; Sakurai, Kazuo

2011-01-01

PEGylated liposomes composed of a benzamidine derivative (TRX), hydrogenated soybean phosphatidylcholine (HSPC), and N-(monomethoxy-polyethyleneglycolcarbamyl) distearoyl phosphatidylethanolamine (PEG-PE) were examined in terms of how the addition of TRX affects their structures with small angle x-ray scattering (SAXS) as well as transmission electron microscopy (TEM). TEM images showed the presence of unilamella vesicles for both with and without TRX, though a small amount of multilamella vesicles were observed in absence of TRX. We analyzed SAXS profiles at contained TRX composition combined with contrast variation technique by adding PEG solution and unilamella vesicle model could be reproduced. Subsequently, we analyzed SAXS profiles at no TRX composition. The mixture model of unilamella and multilamella vesicle was reconstructed and we estimated about 10 % multilamella vesicles from a fitting parameter.

Specific physical and chemical properties of two modifications of poly(N-vinylcaprolcatam)

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

Chihacheva, I. P.; Timaeva, O. I.; Kuz’micheva, G. M., E-mail: galina-kuzmicheva@list.ru

2016-05-15

Two modifications of poly(N-vinylcaprolactam)—PVCL25 and PVCL40 (drying of a PVCL solution at 25 and 40°C, respectively)—as powdered films and their solutions were systematically investigated for the first time. Powders were studied by X-ray diffraction, IR spectroscopy, scanning electron microscopy, low-temperature krypton adsorption, and differential scanning calorimetry. Solutions were studied by smallangle X-ray scattering and dynamic light scattering. It was demonstrated that powders of PVCL25 and PVCL40 differ in the characteristics of the sub- and microstructure and in the water content and the solutions differ in the particle size. The relationships between the characteristics of the systems in the solid andmore » liquid state and between the hydrodynamic diameter of PVCL particles in solution and their coagulation time were found.« less

Acceptor Percolation Determines How Electron-Accepting Additives Modify Transport of Ambipolar Polymer Organic Field-Effect Transistors.

PubMed

Ford, Michael J; Wang, Ming; Bustillo, Karen C; Yuan, Jianyu; Nguyen, Thuc-Quyen; Bazan, Guillermo C

2018-06-18

Organic field-effect transistors (OFETs) that utilize ambipolar polymer semiconductors can benefit from the ability of both electron and hole conduction, which is necessary for complementary circuits. However, simultaneous hole and electron transport in organic field-effect transistors result in poor ON/OFF ratios, limiting potential applications. Solution processing methods have been developed to control charge transport properties and transform ambipolar conduction to hole-only conduction. The electron-acceptor phenyl-C61-butyric acid methyl ester (PC 61 BM), when mixed in solution with an ambipolar semiconducting polymer, can reduce electron conduction. Unipolar p-type OFETs with high, well-defined ON/OFF ratios and without detrimental effects on hole conduction are achieved for a wide range of blend compositions, from 95:5 to 5:95 wt % semiconductor polymer:PC 61 BM. When introducing the alternative acceptor N, N'-bis(1-ethylpropyl)-3,4:9,10-perylenediimide (PDI), high ON/OFF ratios are achieved for 95:5 wt % semiconductor polymer:PDI; however, electron conduction increases for 50:50 and 5:95 wt % semiconductor polymer:PDI. As described within, we show that electron conduction is practically eliminated when additive domains do not percolate across the OFET channel, that is, electrons are "morphologically trapped". Morphologies were characterized by optical, electron, and atomic force microscopy as well as X-ray scattering techniques. PC 61 BM was substituted with an endohedral Lu 3 N fullerene, which enhanced contrast in electron microscopy and allowed for more detailed insight into the blend morphologies. Blends with alternative, nonfullerene acceptors further emphasize the importance of morphology and acceptor percolation, providing insights for such blends that control ambipolar transport and ON/OFF ratios.

Some strategies for quantitative scanning Auger electron microscopy

NASA Technical Reports Server (NTRS)

Browning, R.; Peacock, D. C.; Prutton, M.

1985-01-01

The general applicability of power law forms of the background in electron spectra is pointed out and exploited for background removal from under Auger peaks. This form of B(E) is found to be extremely sensitive to instrumental alignment and to fault-free construction - an observation which can be used to set up analyser configurations in an accurate way. Also, differences between N(E) and B(E) can be used to derive a spectrometer transmission function T(E). The questions of information density in an energy-analysing spatially-resolving instrument are addressed after reliable instrumental characterization has been established. Strategies involving ratio histograms, showing the population distribution of the ratio of a pair of Auger peak heights, composition scatter diagrams and windowed imaging are discussed and illustrated.

Optimizing Nanoscale Quantitative Optical Imaging of Subfield Scattering Targets

PubMed Central

Henn, Mark-Alexander; Barnes, Bryan M.; Zhou, Hui; Sohn, Martin; Silver, Richard M.

2016-01-01

The full 3-D scattered field above finite sets of features has been shown to contain a continuum of spatial frequency information, and with novel optical microscopy techniques and electromagnetic modeling, deep-subwavelength geometrical parameters can be determined. Similarly, by using simulations, scattering geometries and experimental conditions can be established to tailor scattered fields that yield lower parametric uncertainties while decreasing the number of measurements and the area of such finite sets of features. Such optimized conditions are reported through quantitative optical imaging in 193 nm scatterfield microscopy using feature sets up to four times smaller in area than state-of-the-art critical dimension targets. PMID:27805660

Room-temperature mobility above 2200 cm{sup 2}/V·s of two-dimensional electron gas in a sharp-interface AlGaN/GaN heterostructure

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

Chen, Jr-Tai, E-mail: jrche@ifm.liu.se; Persson, Ingemar; Nilsson, Daniel

A high mobility of 2250 cm{sup 2}/V·s of a two-dimensional electron gas (2DEG) in a metalorganic chemical vapor deposition-grown AlGaN/GaN heterostructure was demonstrated. The mobility enhancement was a result of better electron confinement due to a sharp AlGaN/GaN interface, as confirmed by scanning transmission electron microscopy analysis, not owing to the formation of a traditional thin AlN exclusion layer. Moreover, we found that the electron mobility in the sharp-interface heterostructures can sustain above 2000 cm{sup 2}/V·s for a wide range of 2DEG densities. Finally, it is promising that the sharp-interface AlGaN/GaN heterostructure would enable low contact resistance fabrication, less impurity-related scattering, andmore » trapping than the AlGaN/AlN/GaN heterostructure, as the high-impurity-contained AlN is removed.« less

Comparative analysis of characteristic electron energy loss spectra and inelastic scattering cross-section spectra of Fe

NASA Astrophysics Data System (ADS)

Parshin, A. S.; Igumenov, A. Yu.; Mikhlin, Yu. L.; Pchelyakov, O. P.; Zhigalov, V. S.

2016-05-01

The inelastic electron scattering cross section spectra of Fe have been calculated based on experimental spectra of characteristic reflection electron energy loss as dependences of the product of the inelastic mean free path by the differential inelastic electron scattering cross section on the electron energy loss. It has been shown that the inelastic electron scattering cross-section spectra have certain advantages over the electron energy loss spectra in the analysis of the interaction of electrons with substance. The peaks of energy loss in the spectra of characteristic electron energy loss and inelastic electron scattering cross sections have been determined from the integral and differential spectra. It has been shown that the energy of the bulk plasmon is practically independent of the energy of primary electrons in the characteristic electron energy loss spectra and monotonically increases with increasing energy of primary electrons in the inelastic electron scattering cross-section spectra. The variation in the maximum energy of the inelastic electron scattering cross-section spectra is caused by the redistribution of intensities over the peaks of losses due to various excitations. The inelastic electron scattering cross-section spectra have been analyzed using the decomposition of the spectra into peaks of the energy loss. This method has been used for the quantitative estimation of the contributions from different energy loss processes to the inelastic electron scattering cross-section spectra of Fe and for the determination of the nature of the energy loss peaks.

Electron-molecule scattering in a strong laser field: Two-center interference effects

NASA Astrophysics Data System (ADS)

Dakić, J.; Habibović, D.; Čerkić, A.; Busuladžić, M.; Milošević, D. B.

2017-10-01

Laser-assisted scattering of electrons on diatomic molecules is considered using the S -matrix theory within the second Born approximation. The first term of the expansion in powers of the scattering potential corresponds to the direct or single laser-assisted scattering of electrons on molecular targets, while the second term of this expansion corresponds to the laser-assisted rescattering or double scattering. The rescattered electrons may have considerably higher energies in the final state than those that scattered only once. For multicenter polyatomic molecules scattering and rescattering may happen at any center and in any order. All these cases contribute to the scattering amplitude and the interference of different contributions leads to an increase or a decrease of the differential cross section in particular electron energy regions. For diatomic molecules there are two such contributions for single scattering and four contributions for double scattering. Analyzing the spectra of the scattered electrons, we find two interesting effects. For certain molecular orientations, the plateaus in the electron energy spectrum, characteristic of laser-assisted electron-atom scattering, are replaced by a sequence of gradually declining maxima, caused by the two-center interference effects. The second effect is the appearance of symmetric U -shaped structures in the angle-resolved energy spectra, which are described very well by the analytical formulas we provide.

Morphology, mechanical, cross-linking, thermal, and tribological properties of nitrile and hydrogenated nitrile rubber/multi-walled carbon nanotubes composites prepared by melt compounding: The effect of acrylonitrile content and hydrogenation

NASA Astrophysics Data System (ADS)

Likozar, Blaž; Major, Zoltan

2010-11-01

The purpose of this work was to prepare nanocomposites by mixing multi-walled carbon nanotubes (MWCNT) with nitrile and hydrogenated nitrile elastomers (NBR and HNBR). Utilization of transmission electronic microscopy (TEM), scanning electron microscopy (SEM), and small- and wide-angle X-ray scattering techniques (SAXS and WAXS) for advanced morphology observation of conducting filler-reinforced nitrile and hydrogenated nitrile rubber composites is reported. Principal results were increases in hardness (maximally 97 Shore, type A), elastic modulus (maximally 981 MPa), tensile strength (maximally 27.7 MPa), elongation at break (maximally 216%), cross-link density (maximally 7.94 × 1028 m-3), density (maximally 1.16 g cm-3), and tear strength (11.2 kN m-1), which were clearly visible at particular acrylonitrile contents both for unhydrogenated and hydrogenated polymers due to enhanced distribution of carbon nanotubes (CNT) and their aggregated particles in the applied rubber matrix. Conclusion was that multi-walled carbon nanotubes improved the performance of nitrile and hydrogenated nitrile rubber nanocomposites prepared by melt compounding.

From Nano to Macro: Studying the Hierarchical Structure of the Corneal Extracellular Matrix

PubMed Central

Quantock, Andrew J.; Winkler, Moritz; Parfitt, Geraint J.; Young, Robert D.; Brown, Donald J.; Boote, Craig; Jester, James V.

2014-01-01

In this review, we discuss current methods for studying ocular extracellular matrix (ECM) assembly from the ‘nano’ to the ‘macro’ levels of hierarchical organization. Since collagen is the major structural protein in the eye, providing mechanical strength and controlling ocular shape, the methods presented focus on understanding the molecular assembly of collagen at the nanometer level using x-ray scattering through to the millimeter to centimeter level using nonlinear optical (NLO) imaging of second harmonic generated (SHG) signals. Three-dimensional analysis of ECM structure is also discussed, including electron tomography, serial block face scanning electron microscopy (SBF-SEM) and digital image reconstruction. Techniques to detect non-collagenous structural components of the ECM are also presented, and these include immunoelectron microscopy and staining with cationic dyes. Together, these various approaches are providing new insights into the structural blueprint of the ocular ECM, and in particular that of the cornea, which impacts upon our current understanding of the control of corneal shape, pathogenic mechanisms underlying ectatic disorders of the cornea and the potential for corneal tissue engineering. PMID:25819457

As-prepared MoS2 quantum dot as a facile fluorescent probe for long-term tracing of live cells

NASA Astrophysics Data System (ADS)

Zhou, Kai; Zhang, Yue; Xia, Zhining; Wei, Weili

2016-07-01

Recently, the newly emerged two-dimensional nanomaterials, layered transition metal dichalcogenide (e.g. MoS2) nanosheets, have drawn tremendous attentions due to their extraordinary electronic and optical properties, and MoS2 quantum dots (MoS2 QDs) with lateral sizes less than 10 nm have been found to be highly luminescent. In the present study, a facile approach for large-scale preparation of MoS2 QDs by Na intercalation reaction without using any toxic organic reagents is proposed. MoS2 QDs were carefully characterized by various techniques including transmission electron microscopy, atomic force microscopy, dynamic light scattering, spectroscopy, in vitro cytotoxicology, and capillary electrophoresis. The as-prepared MoS2 QDs were strongly fluorescent, highly photo-stable, low in cytotoxicity, and readily reactive to thiols. These inherent properties of MoS2 QDs make them excellent fluorescent probes for long-term live cell tracing. The results of live cells imaging indicated that MoS2 QD stained cells remained highly fluorescent after long-term culture, and could be easily traced from other co-cultured cell lines.

Stability of colloidal silver nanoparticles trapped in lipid bilayer: effect of lecithin concentration and applied temperature.

PubMed

Barani, Hossein; Montazer, Majid; Braun, Hans-Georg; Dutschk, Victoria

2014-12-01

The use of silver nanoparticle on various substrates has been widespread because of its good antibacterial properties that directly depend on the stability of the silver nanoparticles in a colloidal suspension. In this study, the colloidal solutions of the silver nanoparticles were synthesised by a simple and safe method by using lecithin as a stabilising agent and their stability was examined at various temperatures. The effect of the lecithin concentrations on the stability of the synthesised silver nanoparticles was examined from 25 to 80°C at 5°C intervals, by recording the changes in the UV-vis absorption spectra, the hydrodynamic diameter and the light scattering intensity of the silver nanoparticles. In addition, the morphology of the synthesised silver nanoparticles was investigated with the low-voltage scanning electron microscopy and transmission electron microscopy. The results indicated that increasing temperature caused different changes in the size of the stabilised and the unstabilised silver nanoparticles. The size of the stabilised silver nanoparticles reduced from 38 to 36 nm during increasing temperature, which confirmed good stability.

Studies on microstructure, mechanical and corrosion properties of high nitrogen stainless steel shielded metal arc welds

NASA Astrophysics Data System (ADS)

Mohammed, Raffi; Madhusudhan Reddy, G.; Srinivasa Rao, K.

2018-03-01

The present work is aimed at studying the microstructure, mechanical and corrosion properties of high nitrogen stainless steel shielded metal arc (SMA) welds made with Cromang-N electrode. Basis for selecting this electrode is to increase the solubility of nitrogen in weld metal due to high chromium and manganese content. Microstructures of the welds were characterized using optical microscopy (OM), field emission scanning electron microscopy (FESEM) and electron back scattered diffraction (EBSD) mainly to determine the morphology, phase analysis, grain size and orientation image mapping. Hardness, tensile and ductility bend tests were carried out to determine mechanical properties. Potentio-dynamic polarization testing was carried out to study the pitting corrosion resistance using a GillAC basic electrochemical system. Constant load type testing was carried out to study stress corrosion cracking (SCC) behaviour of welds. The investigation results shown that the selected Cr–Mn–N type electrode resulted in favourable microstructure and completely solidified as single phase coarse austenite. Mechanical properties of SMA welds are found to be inferior when compared to that of base metal and is due to coarse and dendritic structure.

Nano-hybrid carboxymethyl-hexanoyl chitosan modified with (3-aminopropyl)triethoxysilane for camptothecin delivery.

PubMed

Hsiao, Meng-Hsuan; Tung, Tsan-Hua; Hsiao, Chi-Sheng; Liu, Dean-Mo

2012-06-20

Silane-modified amphiphilic chitosan was synthesized by anchoring a silane coupling agent, (3-aminopropyl)triethoxysilane, to a novel amphiphilic carboxymethyl-hexanoyl chitosan (CHC). The chemical structure of this new organic-inorganic hybrid molecule was characterized by FTIR and 13C-, 29Si-nuclear magnetic resonance, while the structural evolution was examined using scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), and dynamic light scattering (DLS). Experimental results indicated a self-assembly behaviour of molecules into nanoparticles with a stable polygonal geometry, consisting of ordered silane layers of 6 nm in thickness. The self-assembly property was found to be influenced by chemical composition and concentration of silane incorporated, while the size can be varied by the amount of anchored silane. It was also demonstrated that such vesicle exhibited excellent cytocompatibility and cellular internalization capability in ARPE-19 cell line, and presented well-controlled encapsulation and release profiles for (S)-(+)-camptothecin. These unique properties render it as a potential drug delivery nanosystem. Copyright © 2012 Elsevier Ltd. All rights reserved.