Instrumental development of a quasi-relativistic ultrashort electron beam source for electron diffractions and spectroscopies

NASA Astrophysics Data System (ADS)

Shin, Young-Min; Figora, Michael

2017-10-01

A stable femtosecond electron beam system has been configured for time-resolved pump-probe experiments. The ultrafast electron diffraction (UED) system is designed with a sub-MeV photoelectron beam source pulsed by a femtosecond UV laser and nondispersive beamline components, including a bunch compressor—a pulsed S-band klystron is installed and fully commissioned with 5.5 MW peak power in a 2.5 μs pulse length. A single-cell RF photo-gun is designed to produce 1.6-16 pC electron bunches in a photoemission mode with 150 fs pulse duration at 0.5-1 MeV. The measured RF system jitters are within 1% in magnitude and 0.2° in phase, which would induce 3.4 keV and 0.25 keV of ΔE, corresponding to 80 fs and 5 fs of Δt, respectively. Our particle-in-cell simulations indicate that the designed bunch compressor reduces the time-of-arrival jitter by about an order of magnitude. The transport and focusing optics of the designed beamline with the bunch compressor enables an energy spread within 10-4 and a bunch length (electron probe) within <500 fs. In this paper, the design analysis and instrumental test results are presented along with the development of the quasi-relativistic UED system.

Instrumental development of a quasi-relativistic ultrashort electron beam source for electron diffractions and spectroscopies.

PubMed

Shin, Young-Min; Figora, Michael

2017-10-01

A stable femtosecond electron beam system has been configured for time-resolved pump-probe experiments. The ultrafast electron diffraction (UED) system is designed with a sub-MeV photoelectron beam source pulsed by a femtosecond UV laser and nondispersive beamline components, including a bunch compressor-a pulsed S-band klystron is installed and fully commissioned with 5.5 MW peak power in a 2.5 μs pulse length. A single-cell RF photo-gun is designed to produce 1.6-16 pC electron bunches in a photoemission mode with 150 fs pulse duration at 0.5-1 MeV. The measured RF system jitters are within 1% in magnitude and 0.2° in phase, which would induce 3.4 keV and 0.25 keV of ΔE, corresponding to 80 fs and 5 fs of Δt, respectively. Our particle-in-cell simulations indicate that the designed bunch compressor reduces the time-of-arrival jitter by about an order of magnitude. The transport and focusing optics of the designed beamline with the bunch compressor enables an energy spread within 10 -4 and a bunch length (electron probe) within <500 fs. In this paper, the design analysis and instrumental test results are presented along with the development of the quasi-relativistic UED system.

On the temperature dependence of H-U{sub iso} in the riding hydrogen model

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

Lübben, Jens; Volkmann, Christian; Grabowsky, Simon

The temperature dependence of hydrogen U{sub iso} and parent U{sub eq} in the riding hydrogen model is investigated by neutron diffraction, aspherical-atom refinements and QM/MM and MO/MO cluster calculations. Fixed values of 1.2 or 1.5 appear to be underestimated, especially at temperatures below 100 K. The temperature dependence of H-U{sub iso} in N-acetyl-l-4-hydroxyproline monohydrate is investigated. Imposing a constant temperature-independent multiplier of 1.2 or 1.5 for the riding hydrogen model is found to be inaccurate, and severely underestimates H-U{sub iso} below 100 K. Neutron diffraction data at temperatures of 9, 150, 200 and 250 K provide benchmark results for thismore » study. X-ray diffraction data to high resolution, collected at temperatures of 9, 30, 50, 75, 100, 150, 200 and 250 K (synchrotron and home source), reproduce neutron results only when evaluated by aspherical-atom refinement models, since these take into account bonding and lone-pair electron density; both invariom and Hirshfeld-atom refinement models enable a more precise determination of the magnitude of H-atom displacements than independent-atom model refinements. Experimental efforts are complemented by computing displacement parameters following the TLS+ONIOM approach. A satisfactory agreement between all approaches is found.« less

Ultrafast electron microscopy in materials science, biology, and chemistry

NASA Astrophysics Data System (ADS)

King, Wayne E.; Campbell, Geoffrey H.; Frank, Alan; Reed, Bryan; Schmerge, John F.; Siwick, Bradley J.; Stuart, Brent C.; Weber, Peter M.

2005-06-01

The use of pump-probe experiments to study complex transient events has been an area of significant interest in materials science, biology, and chemistry. While the emphasis has been on laser pump with laser probe and laser pump with x-ray probe experiments, there is a significant and growing interest in using electrons as probes. Early experiments used electrons for gas-phase diffraction of photostimulated chemical reactions. More recently, scientists are beginning to explore phenomena in the solid state such as phase transformations, twinning, solid-state chemical reactions, radiation damage, and shock propagation. This review focuses on the emerging area of ultrafast electron microscopy (UEM), which comprises ultrafast electron diffraction (UED) and dynamic transmission electron microscopy (DTEM). The topics that are treated include the following: (1) The physics of electrons as an ultrafast probe. This encompasses the propagation dynamics of the electrons (space-charge effect, Child's law, Boersch effect) and extends to relativistic effects. (2) The anatomy of UED and DTEM instruments. This includes discussions of the photoactivated electron gun (also known as photogun or photoelectron gun) at conventional energies (60-200 keV) and extends to MeV beams generated by rf guns. Another critical aspect of the systems is the electron detector. Charge-coupled device cameras and microchannel-plate-based cameras are compared and contrasted. The effect of various physical phenomena on detective quantum efficiency is discussed. (3) Practical aspects of operation. This includes determination of time zero, measurement of pulse-length, and strategies for pulse compression. (4) Current and potential applications in materials science, biology, and chemistry. UEM has the potential to make a significant impact in future science and technology. Understanding of reaction pathways of complex transient phenomena in materials science, biology, and chemistry will provide fundamental knowledge for discovery-class science.

Biosynthesis of silver nanoparticles using fresh extracts of Tridax procumbens linn.

PubMed

Bhati-Kushwaha, Himakshi

2014-04-01

A simple and eco-friendly method for the synthesis of biogenic nanoparticles (NP's) using an aqueous solution of T. procumbens fresh plant extract (leaf and stem) as a bioreductant is reported. The prepared biogenic nanoparticles were well characterized using U.V. visible spectroscopy, scanning electron microscopy, X-ray diffraction and Fourier-transform infrared spectroscopy. The particles were confirmed to be elemental crystal by X-ray diffraction. The potential applications of biosynthesized nanoparticles as antimicrobial (antibacterial and antifungal) against pathogens Escherichia coli, Vibrio cholerae, Aspergillus niger and Aspergillusflavus were demonstrated.

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

Interdiffusion behavior of U3Si2 with FeCrAl via diffusion couple studies

NASA Astrophysics Data System (ADS)

Hoggan, Rita E.; He, Lingfeng; Harp, Jason M.

2018-04-01

Uranium silicide (U3Si2) is a candidate to replace uranium oxide (UO2) as light water reactor (LWR) fuel because of its higher thermal conductivity and higher fissile density relative to the current standard, UO2. A class of Fe, Cr, Al alloys collectively known as FeCrAl alloys that have superior mechanical and oxidation resistance are being considered as an alternative to the standard Zirconium based LWR cladding. The interdiffusion behavior between FeCrAl and U3Si2 is investigated in this study. Commercially available FeCrAl, along with U3Si2 pellets were placed in diffusion couples. Individual tests were ran at temperatures ranging from 500 °C to 1000 °C for 30 h and 100 h. The interdiffusion was analyzed with an optical microscope, scanning electron microscope, and transmission electron microscope. Uniform and planar interdiffusion layers along the material interface were illustrated with backscatter electron micrographs and energy-dispersive X-ray spectroscopy. Electron diffraction was used to validate phases present in the system, including distinct U2Fe3Si/UFe2 and UFeSi layers at the material interface. U and Fe diffused far into the FeCrAl and U3Si2 matrix, respectively, in the higher temperature tests. No interaction was observed at 500 °C for 30 h.

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

Jana, S.; Devaraj, A.; Kovarik, L.

Transformation kinetics of metastable body-centered cubic γ-UMo phase in U-10 wt.percent Mo alloy during annealing at sub-eutectoid temperatures of 500C and 400C has been determined as a function of time using detailed microstructural characterization by scanning electron microscopy, X-ray diffraction analysis, scanning transmission electron microscopy, and atom probe tomography. Based on the results, we found that the phase transformation is initiated by cellular transformation at both the temperatures, which results in formation of a lamellar microstructure along prior γ-UMo grain boundaries.

Uranium Redox Transformations after U(VI) Coprecipitation with Magnetite Nanoparticles.

PubMed

Pidchenko, Ivan; Kvashnina, Kristina O; Yokosawa, Tadahiro; Finck, Nicolas; Bahl, Sebastian; Schild, Dieter; Polly, Robert; Bohnert, Elke; Rossberg, André; Göttlicher, Jörg; Dardenne, Kathy; Rothe, Jörg; Schäfer, Thorsten; Geckeis, Horst; Vitova, Tonya

2017-02-21

Uranium redox states and speciation in magnetite nanoparticles coprecipitated with U(VI) for uranium loadings varying from 1000 to 10 000 ppm are investigated by X-ray absorption spectroscopy (XAS). It is demonstrated that the U M 4 high energy resolution X-ray absorption near edge structure (HR-XANES) method is capable to clearly characterize U(IV), U(V), and U(VI) existing simultaneously in the same sample. The contributions of the three different uranium redox states are quantified with the iterative transformation factor analysis (ITFA) method. U L 3 XAS and transmission electron microscopy (TEM) reveal that initially sorbed U(VI) species recrystallize to nonstoichiometric UO 2+x nanoparticles within 147 days when stored under anoxic conditions. These U(IV) species oxidize again when exposed to air. U M 4 HR-XANES data demonstrate strong contribution of U(V) at day 10 and that U(V) remains stable over 142 days under ambient conditions as shown for magnetite nanoparticles containing 1000 ppm U. U L 3 XAS indicates that this U(V) species is protected from oxidation likely incorporated into octahedral magnetite sites. XAS results are supported by density functional theory (DFT) calculations. Further characterization of the samples include powder X-ray diffraction (pXRD), scanning electron microscopy (SEM) and Fe 2p X-ray photoelectron spectroscopy (XPS).

High pressure effects on U L 3 x-ray absorption in partial fluorescence yield mode and single crystal x-ray diffraction in the heavy fermion compound UCd 11

DOE PAGES

Nasreen, Farzana; Antonio, Daniel; VanGennep, Derrick; ...

2016-02-15

© 2016 IOP Publishing Ltd. We report a study of high pressure x-ray absorption (XAS) performed in the partial fluorescence yield mode (PFY) at the U L 3 edge (0-28.2 GPa) and single crystal x-ray diffraction (SXD) (0-20 GPa) on the UCd 11 heavy fermion compound at room temperature. Under compression, the PFY-XAS results show that the white line is shifted by +4.1(3) eV at the highest applied pressure of 28.2 GPa indicating delocalization of the 5f electrons. The increase in full width at half maxima and decrease in relative amplitude of the white line with respect to the edgemore » jump point towards 6d band broadening under high pressure. A bulk modulus of K 0 = 62(1) GPa and its pressure derivative, = 4.9(2) was determined from high pressure SXD results. Both the PFY-XAS and diffraction results do not show any sign of a structural phase transition in the applied pressure range.« less

Layer Number and Stacking Order Imaging of Few-layer Graphenes by Transmission Electron Microscopy

NASA Astrophysics Data System (ADS)

Ping, Jinglei; Fuhrer, Michael

2012-02-01

A method using transmission electron microscopy (TEM) selected area electron diffraction (SAED) patterns and dark field (DF) images is developed to identify graphene layer number and stacking order by comparing intensity ratios of SAED spots with theory. Graphene samples are synthesized by ambient pressure chemical vapor depostion and then etched by hydrogen in high temperature to produce samples with crystalline stacking but varying layer number on the nanometer scale. Combined DF images from first- and second-order diffraction spots are used to produce images with layer-number and stacking-order contrast with few-nanometer resolution. This method is proved to be accurate enough for quantative stacking-order-identification of graphenes up to at least four layers. This work was partially supported by Science of Precision Multifunctional Nanostructures for Elecrical Energy Storage, an Energy Frontier Research Center funded by the U.S. DOE, Office of Science, Office of Basic Energy Sciences under Award Number DESC0001160.

In Situ Neutron Diffraction of Rare-Earth Phosphate Proton Conductors Sr/Ca-doped LaPO4 at Elevated Temperatures

NASA Astrophysics Data System (ADS)

Al-Wahish, Amal; Al-Binni, Usama; Bridges, C. A.; Huq, A.; Bi, Z.; Paranthaman, M. P.; Tang, S.; Kaiser, H.; Mandrus, D.

Acceptor-doped lanthanum orthophosphates are potential candidate electrolytes for proton ceramic fuel cells. We combined neutron powder diffraction (NPD) at elevated temperatures up to 800° C , X-ray powder diffraction (XRD) and scanning electron microscopy (SEM) to investigate the crystal structure, defect structure, thermal stability and surface topography. NPD shows an average bond length distortion in the hydrated samples. We employed Quasi-Elastic Neutron Scattering (QENS) and electrochemical impedance spectroscopy (EIS) to study the proton dynamics of the rare-earth phosphate proton conductors 4.2% Sr/Ca-doped LaPO4. We determined the bulk diffusion and the self-diffusion coefficients. Our results show that QENS and EIS are probing fundamentally different proton diffusion processes. Supported by the U.S. Department of Energy.

Terahertz Streaking of Few-Femtosecond Relativistic Electron Beams

NASA Astrophysics Data System (ADS)

Zhao, Lingrong; Wang, Zhe; Lu, Chao; Wang, Rui; Hu, Cheng; Wang, Peng; Qi, Jia; Jiang, Tao; Liu, Shengguang; Ma, Zhuoran; Qi, Fengfeng; Zhu, Pengfei; Cheng, Ya; Shi, Zhiwen; Shi, Yanchao; Song, Wei; Zhu, Xiaoxin; Shi, Jiaru; Wang, Yingxin; Yan, Lixin; Zhu, Liguo; Xiang, Dao; Zhang, Jie

2018-04-01

Streaking of photoelectrons with optical lasers has been widely used for temporal characterization of attosecond extreme ultraviolet pulses. Recently, this technique has been adapted to characterize femtosecond x-ray pulses in free-electron lasers with the streaking imprinted by far-infrared and terahertz (THz) pulses. Here, we report successful implementation of THz streaking for time stamping of an ultrashort relativistic electron beam, whose energy is several orders of magnitude higher than photoelectrons. Such an ability is especially important for MeV ultrafast electron diffraction (UED) applications, where electron beams with a few femtosecond pulse width may be obtained with longitudinal compression, while the arrival time may fluctuate at a much larger timescale. Using this laser-driven THz streaking technique, the arrival time of an ultrashort electron beam with a 6-fs (rms) pulse width has been determined with 1.5-fs (rms) accuracy. Furthermore, we have proposed and demonstrated a noninvasive method for correction of the timing jitter with femtosecond accuracy through measurement of the compressed beam energy, which may allow one to advance UED towards a sub-10-fs frontier, far beyond the approximate 100-fs (rms) jitter.

Quantitative analysis of thoria phase in Th-U alloys using diffraction studies

NASA Astrophysics Data System (ADS)

Thakur, Shital; Krishna, P. S. R.; Shinde, A. B.; Kumar, Raj; Roy, S. B.

2017-05-01

In the present study the quantitative phase analysis of Th-U alloys in bulk form namely Th-52 wt% U and Th-3wt%U has been performed over the data obtained from both X ray diffraction and neutron diffraction technique using Rietveld method of FULLPROF software. Quantifying thoria (ThO2) phase present in bulk of the sample is limited due to surface oxidation and low penetration of x rays in high Z material. Neutron diffraction study probing bulk of the samples has been presented in comparison with x-ray diffraction study.

Investigation of the phase relations in the U-Al-Ge ternary system: Influence of the Al/Ge substitution on the properties of the intermediate phases

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

Moussa, C.; El Sayah, Z.; Chajewski, G.

The phase relations within the U-Al-Ge ternary system were studied for two isothermal sections, at 673 K for the whole Gibbs triangle and at 1173 K for the concentration range 25–100 at% U. The identification of the phases, their composition ranges and stability were determined by x-ray powder diffraction, scanning electron microscopy coupled to energy dispersive spectroscopy and differential thermal analysis. The tie-lines and the solubility domains were determined for the U-Ge and U-Al binaries, the UAl{sub 3}-UGe{sub 3} solid-solution and for the unique ternary intermediate phase U{sub 3}Al{sub 2−x}Ge{sub 3+x}. The experimental isopleth section of the pseudo-binary UAl{sub 3}-UGe{submore » 3} reveals an isomorphous solid solution based on the Cu{sub 3}Au-type below the solidus. The U{sub 3}Al{sub 2−x}Ge{sub 3+x} solid solution extends for −0.1≤x≤1.35 and −0.2≤x≤1.5 at 673 K and 1173 K respectively. It crystallizes in the I-centered tetragonal symmetry. The reciprocal lattice of several compositions of the U{sub 3}Al{sub 2−x}Ge{sub 3+x} solid solution was examined by electron diffraction at room temperature, revealing the presence of a c-glide plane. Their crystal structure was refined by single crystal x-ray diffraction suggesting an isomorphous solid solution best described with the non-centrosymmetric space group I4cm in the paramagnetic domain. The magnetic measurements confirm the ferromagnetic ordering of the solid solution U{sub 3}Al{sub 2−x}Ge{sub 3+x} with an increase of Tc with the Al content. The thermal variation of the specific heat bear out the magnetic transitions with some delocalized character of the uranium 5f electrons. - Graphical abstract: The phase relations within the U-Al-Ge ternary system were experimentally assessed for two isothermal sections, at 673 K for the whole Gibbs triangle and at 1173 K for the concentration range 25–100 at% U. A complete UAl{sub 3}-UGe{sub 3} solid-solution based on the Cu{sub 3}Au-type forms below the solidus. A unique ternary phase showing a large homogeneity domain, U{sub 3}Al{sub 2−x}Ge{sub 3+x} for −0.1≤x≤1.35 and −0.2≤x≤1.5 at 673 K and 1173 K respectively has been evidenced. It is best described with the non-centrosymmetric space group I4cm above room temperature. A linear increase of the ferromagnetic ordering is observed with the Al content. - Highlights: • Isothermal sections of the U-Al-Ge system were investigated for 673 K and 1173 K. • An isomorphous solid-solution UAl{sub 3}-UGe{sub 3} forms for the whole composition range. • U{sub 3}Al{sub 2−x}Ge{sub 3+x} the unique ternary phase to form exists for a large homogeneity domain. • U{sub 3}Al{sub 2−x}Ge{sub 3+x} is best described in I4cm space group above room temperature. • The ferromagnetic transition of U{sub 3}Al{sub 2−x}Ge{sub 3+x} linearly increases with the Al content.« less

Anaerobic bioremediation of hexavalent uranium in groundwater by reductive precipitation with methanogenic granular sludge.

PubMed

Tapia-Rodriguez, Aida; Luna-Velasco, Antonia; Field, Jim A; Sierra-Alvarez, Reyes

2010-04-01

Uranium has been responsible for extensive contamination of groundwater due to releases from mill tailings and other uranium processing waste. Past evidence has confirmed that certain bacteria can enzymatically reduce soluble hexavalent uranium (U(VI)) to insoluble tetravalent uranium (U(IV)) under anaerobic conditions in the presence of appropriate electron donors. This paper focuses on the evaluation of anaerobic granular sludge as a source of inoculum for the bioremediation of uranium in water. Batch experiments were performed with several methanogenic anaerobic granular sludge samples and different electron donors. Abiotic controls consisting of heat-killed inoculum and non-inoculated treatments confirmed the biological removal process. In this study, unadapted anaerobic granular sludge immediately reduced U(VI), suggesting an intrinsic capacity of the sludge to support this process. The high biodiversity of anaerobic granular sludge most likely accounts for the presence of specific microorganisms capable of reducing U(VI). Oxidation by O(2) was shown to resolubilize the uranium. This observation combined with X-ray diffraction evidence of uraninite confirmed that the removal during anaerobic treatment was due to reductive precipitation. The anaerobic removal activity could be sustained after several respikes of U(VI). The U(VI) removal was feasible without addition of electron donors, indicating that the decay of endogenous biomass substrates was contributing electron equivalents to the process. Addition of electron donors, such as H(2) stimulated the removal of U(VI) to varying degrees. The stimulation was greater in sludge samples with lower endogenous substrate levels. The present work reveals the potential application of anaerobic granular sludge for continuous bioremediation schemes to treat uranium-contaminated water. Copyright (c) 2009 Elsevier Ltd. All rights reserved.

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.

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

Short communication on Kinetics of grain growth and particle pinning in U-10 wt.% Mo

NASA Astrophysics Data System (ADS)

Frazier, William E.; Hu, Shenyang; Overman, Nicole; Lavender, Curt; Joshi, Vineet V.

2018-01-01

The alloy U-10 wt% Mo was annealed at temperatures ranging from 700 °C to 900 °C for periods lasting up to 24 h. Annealed microstructures were examined using Electron Backscattered Diffraction (EBSD) to obtain average grain sizes and grain size distributions. From the temporal evolution of the average grain size, the activation energy of grain growth was determined to be 172.4 ± 0.961 kJ/mol. Grain growth over the annealing period stagnated after a period of 1-4 h. This stagnation is apparently caused by the pinning effect of second-phase particles in the materials. Back-scattered electron imaging (BSE) was used to confirm that these particles do not appreciably coarsen or dissolve during annealing at the aforementioned temperatures.

Electron donor concentrations in sediments and sediment properties at the agricultural chemicals team research site near New Providence, Iowa, 2006-07

USGS Publications Warehouse

Maharjan, Bijesh; Korom, Scott F.; Smith, Erik A.

2013-01-01

The concentrations of electron donors in aquifer sediments are important to the understanding of the fate and transport of redox-sensitive constituents in groundwater, such as nitrate. For a study by the U.S. Geological Survey National Water-Quality Assessment Program, 50 sediment samples were collected from below the water table from 11 boreholes at the U.S. Geological Survey Agricultural Chemicals Team research site near New Providence, Iowa, during 2006-07. All samples were analyzed for gravel, sand (coarse, medium, and fine), silt, clay, Munsell soil color, inorganic carbon content, and for the following electron donors: organic carbon, ferrous iron, and inorganic sulfide. A subset of 14 sediment samples also was analyzed for organic sulfur, but all of these samples had concentrations less than the method detection limit; therefore, the presence of this potential electron donor was not considered further. X-ray diffraction analyses provided important semi-quantitative information of well-crystallized dominant minerals within the sediments that might be contributing electron donors.

Solid-phase data from cores at the proposed Dewey Burdock uranium in-situ recovery mine, near Edgemont, South Dakota

USGS Publications Warehouse

Johnson, Raymond H.; Diehl, Sharon F.; Benzel, William M.

2013-01-01

This report releases solid-phase data from cores at the proposed Dewey Burdock uranium in-situ recovery site near Edgemont, South Dakota. These cores were collected by Powertech Uranium Corporation, and material not used for their analyses were given to the U.S. Geological Survey for additional sampling and analyses. These additional analyses included total carbon and sulfur, whole rock acid digestion for major and trace elements, 234U/238U activity ratios, X-ray diffraction, thin sections, scanning electron microscopy analyses, and cathodoluminescence. This report provides the methods and data results from these analyses along with a short summary of observations.

Energy-resolved coherent diffraction from laser-driven electronic motion in atoms

NASA Astrophysics Data System (ADS)

Shao, Hua-Chieh; Starace, Anthony F.

2017-10-01

We investigate theoretically the use of energy-resolved ultrafast electron diffraction to image laser-driven electronic motion in atoms. A chirped laser pulse is used to transfer the valence electron of the lithium atom from the ground state to the first excited state. During this process, the electronic motion is imaged by 100-fs and 1-fs electron pulses in energy-resolved diffraction measurements. Simulations show that the angle-resolved spectra reveal the time evolution of the energy content and symmetry of the electronic state. The time-dependent diffraction patterns are further interpreted in terms of the momentum transfer. For the case of incident 1-fs electron pulses, the rapid 2 s -2 p quantum beat motion of the target electron is imaged as a time-dependent asymmetric oscillation of the diffraction pattern.

Ultrafast electron diffraction with megahertz MeV electron pulses from a superconducting radio-frequency photoinjector

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

Feng, L. W.; Lin, L.; Huang, S. L.

We report ultrafast relativistic electron diffraction operating at the megahertz repetition rate where the electron beam is produced in a superconducting radio-frequency (rf) photoinjector. We show that the beam quality is sufficiently high to provide clear diffraction patterns from gold and aluminium samples. With the number of electrons, several orders of magnitude higher than that from a normal conducting photocathode rf gun, such high repetition rate ultrafast MeV electron diffraction may open up many new opportunities in ultrafast science.

A measurement of electron-wall interactions using transmission diffraction from nanofabricated gratings

NASA Astrophysics Data System (ADS)

Barwick, Brett; Gronniger, Glen; Yuan, Lu; Liou, Sy-Hwang; Batelaan, Herman

2006-10-01

Electron diffraction from metal coated freestanding nanofabricated gratings is presented, with a quantitative path integral analysis of the electron-grating interactions. Electron diffraction out to the 20th order was observed indicating the high quality of our nanofabricated gratings. The electron beam is collimated to its diffraction limit with ion-milled material slits. Our path integral analysis is first tested against single slit electron diffraction, and then further expanded with the same theoretical approach to describe grating diffraction. Rotation of the grating with respect to the incident electron beam varies the effective distance between the electron and grating bars. This allows the measurement of the image charge potential between the electron and the grating bars. Image charge potentials that were about 15% of the value for that of a pure electron-metal wall interaction were found. We varied the electron energy from 50to900eV. The interaction time is of the order of typical metal image charge response times and in principle allows the investigation of image charge formation. In addition to the image charge interaction there is a dephasing process reducing the transverse coherence length of the electron wave. The dephasing process causes broadening of the diffraction peaks and is consistent with a model that ascribes the dephasing process to microscopic contact potentials. Surface structures with length scales of about 200nm observed with a scanning tunneling microscope, and dephasing interaction strength typical of contact potentials of 0.35eV support this claim. Such a dephasing model motivated the investigation of different metallic coatings, in particular Ni, Ti, Al, and different thickness Au-Pd coatings. Improved quality of diffraction patterns was found for Ni. This coating made electron diffraction possible at energies as low as 50eV. This energy was limited by our electron gun design. These results are particularly relevant for the use of these gratings as coherent beam splitters in low energy electron interferometry.

Attomicroscopy: from femtosecond to attosecond electron microscopy

NASA Astrophysics Data System (ADS)

Hassan, Mohammed Th

2018-02-01

In the last decade, the development of ultrafast electron diffraction (UED) and microscopy (UEM) have enabled the imaging of atomic motion in real time and space. These pivotal table-top tools opened the door for a vast range of applications in different areas of science spanning chemistry, physics, materials science, and biology. We first discuss the basic principles and recent advancements, including some of the important applications, of both UED and UEM. Then, we discuss the recent advances in the field that have enhanced the spatial and temporal resolutions, where the latter, is however, still limited to a few hundreds of femtoseconds, preventing the imaging of ultrafast dynamics of matter lasting few tens of femtoseconds. Then, we present our new optical gating approach for generating an isolated 30 fs electron pulse with sufficient intensity to attain a temporal resolution on the same time scale. This achievement allows, for the first time, imaging the electron dynamics of matter. Finally, we demonstrate the feasibility of the optical gating approach to generate an isolated attosecond electron pulse, utilizing our recently demonstrated optical attosecond laser pulse, which paves the way for establishing the field of ‘Attomicroscopy’, ultimately enabling us to image the electron motion in action.

Digital electron diffraction – seeing the whole picture

PubMed Central

Beanland, Richard; Thomas, Paul J.; Woodward, David I.; Thomas, Pamela A.; Roemer, Rudolf A.

2013-01-01

The advantages of convergent-beam electron diffraction for symmetry determination at the scale of a few nm are well known. In practice, the approach is often limited due to the restriction on the angular range of the electron beam imposed by the small Bragg angle for high-energy electron diffraction, i.e. a large convergence angle of the incident beam results in overlapping information in the diffraction pattern. Techniques have been generally available since the 1980s which overcome this restriction for individual diffracted beams, by making a compromise between illuminated area and beam convergence. Here a simple technique is described which overcomes all of these problems using computer control, giving electron diffraction data over a large angular range for many diffracted beams from the volume given by a focused electron beam (typically a few nm or less). The increase in the amount of information significantly improves the ease of interpretation and widens the applicability of the technique, particularly for thin materials or those with larger lattice parameters. PMID:23778099

Identification of phases in the interaction layer between U-Mo-Zr/Al and U-Mo-Zr/Al-Si

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

Varela, C.L. Komar; Arico, S.F.; Mirandou, M.

Out-of-pile diffusion experiments were performed between U-7wt.% Mo-1wt.% Zr and Al or Al A356 (7,1wt.% Si) at 550 deg. C. In this work morphological characterization and phase identification on both interaction layer are presented. They were carried out by the use of different techniques: optical and scanning electron microscopy, X-Ray diffraction and WDS microanalysis. In the interaction layer U-7wt.% Mo-1wt.% Zr/Al, the phases UAl{sub 3}, UAl{sub 4}, Al{sub 20}Mo{sub 2}U and Al{sub 43}Mo{sub 4}U{sub 6} were identified. In the interaction layer U-7wt.% Mo-1wt.% Zr/Al A356, the phases U(Al, Si) with 25at.% Si and Si{sub 5}U{sub 3} were identified. This lastmore » phase, with a higher Si concentration, was identified with XRD Synchrotron radiation performed at the National Synchrotron Light Laboratory (LNLS), Campinas, Brasil. (author)« less

X-Ray Sum Frequency Diffraction for Direct Imaging of Ultrafast Electron Dynamics

NASA Astrophysics Data System (ADS)

Rouxel, Jérémy R.; Kowalewski, Markus; Bennett, Kochise; Mukamel, Shaul

2018-06-01

X-ray diffraction from molecules in the ground state produces an image of their charge density, and time-resolved x-ray diffraction can thus monitor the motion of the nuclei. However, the density change of excited valence electrons upon optical excitation can barely be monitored with regular diffraction techniques due to the overwhelming background contribution of the core electrons. We present a nonlinear x-ray technique made possible by novel free electron laser sources, which provides a spatial electron density image of valence electron excitations. The technique, sum frequency generation carried out with a visible pump and a broadband x-ray diffraction pulse, yields snapshots of the transition charge densities, which represent the electron density variations upon optical excitation. The technique is illustrated by ab initio simulations of transition charge density imaging for the optically induced electronic dynamics in a donor or acceptor substituted stilbene.

Electron Emission in Highly Charged Ion-Atom Collisions

NASA Astrophysics Data System (ADS)

Liao, Chunlei

1995-01-01

This dissertation addresses the problem of electron emission in highly charged ion-atom collisions. The study is carried out by measuring doubly differential cross sections (DDCS) of emitted electrons for projectiles ranging from fluorine up to gold at ejection angles (theta _{L}) from 0^circ to 70^circ with respect to the beam direction. Prominent features are a very strong forward peaked angular distribution of emitted electrons and the appearance of strong diffraction structures in the binary encounter electron (BEe) region for projectiles heavier than chlorine. This is in clear contradiction to the results found with fluorine projectiles, where the BEe production increases slightly with increasing theta_{L} and no structure is observed in the BEe region. Both can be understood in the impulse approximation as elastic scattering of quasi free target electrons in the projectile potential. Our measurements also show that the violation of q ^2 scaling of the DDCS previously established for 0^circ electron spectra persists for all emission angles and almost all electron energies. In ion-atom collisions, besides electrons from target, electrons from projectile ionization are also presented in the emitted electron spectra. Using electron-projectile coincidence technique, different collision channels can be separated. In order to eliminate the speculations of contributions from projectile related capture and loss channels, coincidence studies of diffraction structures are initiated. In the 0^circ electron spectrum of 0.3 MeV/u I^{6+} impacting on H_2, strong autoionization peaks are observed on the shoulders of the cusp peak. The energies of these autoionization lines in the projectile rest frame are determined by high-resolution electron spectroscopy, and collision mechanism is probed by electron-charge state selected projectile coincidence technique.

Relativistic electron diffraction at the UCLA Pegasus photoinjector laboratory.

PubMed

Musumeci, P; Moody, J T; Scoby, C M

2008-10-01

Electron diffraction holds the promise to yield real-time resolution of atomic motion in an easily accessible environment like a university laboratory at a fraction of the cost of fourth-generation X-ray sources. Currently the limit in time-resolution for conventional electron diffraction is set by how short an electron pulse can be made. A very promising solution to maintain the highest possible beam intensity without excessive pulse broadening from space charge effects is to increase the electron energy to the MeV level where relativistic effects significantly reduce the space charge forces. Rf photoinjectors can in principle deliver up to 10(7)-10(8) electrons packed in bunches of approximately 100-fs length, allowing an unprecedented time resolution and enabling the study of irreversible phenomena by single-shot diffraction patterns. The use of rf photoinjectors as sources for ultrafast electron diffraction has been recently at the center of various theoretical and experimental studies. The UCLA Pegasus laboratory, commissioned in early 2007 as an advanced photoinjector facility, is the only operating system in the country, which has recently demonstrated electron diffraction using a relativistic beam from an rf photoinjector. Due to the use of a state-of-the-art ultrashort photoinjector driver laser system, the beam has been measured to be sub-100-fs long, at least a factor of 5 better than what measured in previous relativistic electron diffraction setups. Moreover, diffraction patterns from various metal targets (titanium and aluminum) have been obtained using the Pegasus beam. One of the main laboratory goals in the near future is to fully develop the rf photoinjector-based ultrafast electron diffraction technique with particular attention to the optimization of the working point of the photoinjector in a low-charge ultrashort pulse regime, and to the development of suitable beam diagnostics.

Nanomodulated electron beams via electron diffraction and emittance exchange for coherent x-ray generation

NASA Astrophysics Data System (ADS)

Nanni, E. A.; Graves, W. S.; Moncton, D. E.

2018-01-01

We present a new method for generation of relativistic electron beams with current modulation on the nanometer scale and below. The current modulation is produced by diffracting relativistic electrons in single crystal Si, accelerating the diffracted beam and imaging the crystal structure, then transferring the image into the temporal dimension via emittance exchange. The modulation period can be tuned by adjusting electron optics after diffraction. This tunable longitudinal modulation can have a period as short as a few angstroms, enabling production of coherent hard x-rays from a source based on inverse Compton scattering with total accelerator length of approximately ten meters. Electron beam simulations from cathode emission through diffraction, acceleration, and image formation with variable magnification are presented along with estimates of the coherent x-ray output properties.

Energy-weighted dynamical scattering simulations of electron diffraction modalities in the scanning electron microscope.

PubMed

Pascal, Elena; Singh, Saransh; Callahan, Patrick G; Hourahine, Ben; Trager-Cowan, Carol; Graef, Marc De

2018-04-01

Transmission Kikuchi diffraction (TKD) has been gaining momentum as a high resolution alternative to electron back-scattered diffraction (EBSD), adding to the existing electron diffraction modalities in the scanning electron microscope (SEM). The image simulation of any of these measurement techniques requires an energy dependent diffraction model for which, in turn, knowledge of electron energies and diffraction distances distributions is required. We identify the sample-detector geometry and the effect of inelastic events on the diffracting electron beam as the important factors to be considered when predicting these distributions. However, tractable models taking into account inelastic scattering explicitly are lacking. In this study, we expand the Monte Carlo (MC) energy-weighting dynamical simulations models used for EBSD [1] and ECP [2] to the TKD case. We show that the foil thickness in TKD can be used as a means of energy filtering and compare band sharpness in the different modalities. The current model is shown to correctly predict TKD patterns and, through the dictionary indexing approach, to produce higher quality indexed TKD maps than conventional Hough transform approach, especially close to grain boundaries. Copyright © 2018 The Authors. Published by Elsevier B.V. All rights reserved.

Upgrade possibilities for continuous wave rf electron guns based on room-temperature very high frequency technology

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

Sannibale, F.; Filippetto, D.; Johnson, M.

The past decade was characterized by an increasing scientific demand for extending towards higher repetition rates (MHz class and beyond) the performance of already operating lower repetition rate accelerator-based instruments such as x-ray free electron lasers (FELs) and ultrafast electron diffraction (UED) and microscopy (UEM) instruments. Such a need stimulated a worldwide spread of a vibrant R & D activity targeting the development of high-brightness electron sources capable of operating at these challenging rates. Among the different technologies pursued, rf guns based on room-temperature structures resonating in the very high frequency (VHF) range (30-300 MHz) and operating in continuous wavemore » successfully demonstrated in the past few years the targeted brightness and reliability. Nonetheless, recently proposed upgrades for x-ray FELs and the always brightness-frontier applications such as UED and UEM are now requiring a further step forward in terms of beam brightness in electron sources. Here, we present a few possible upgrade paths that would allow one to extend, in a relatively simple and cost-effective way, the performance of the present VHF technology to the required new goals.« less

Upgrade possibilities for continuous wave rf electron guns based on room-temperature very high frequency technology

DOE PAGES

Sannibale, F.; Filippetto, D.; Johnson, M.; ...

2017-11-27

The past decade was characterized by an increasing scientific demand for extending towards higher repetition rates (MHz class and beyond) the performance of already operating lower repetition rate accelerator-based instruments such as x-ray free electron lasers (FELs) and ultrafast electron diffraction (UED) and microscopy (UEM) instruments. Such a need stimulated a worldwide spread of a vibrant R & D activity targeting the development of high-brightness electron sources capable of operating at these challenging rates. Among the different technologies pursued, rf guns based on room-temperature structures resonating in the very high frequency (VHF) range (30-300 MHz) and operating in continuous wavemore » successfully demonstrated in the past few years the targeted brightness and reliability. Nonetheless, recently proposed upgrades for x-ray FELs and the always brightness-frontier applications such as UED and UEM are now requiring a further step forward in terms of beam brightness in electron sources. Here, we present a few possible upgrade paths that would allow one to extend, in a relatively simple and cost-effective way, the performance of the present VHF technology to the required new goals.« less

Swift heavy ion track formation in Gd2Zr2-xTixO7 pyrochlore: Effect of electronic energy loss

NASA Astrophysics Data System (ADS)

Lang, Maik; Toulemonde, Marcel; Zhang, Jiaming; Zhang, Fuxiang; Tracy, Cameron L.; Lian, Jie; Wang, Zhongwu; Weber, William J.; Severin, Daniel; Bender, Markus; Trautmann, Christina; Ewing, Rodney C.

2014-10-01

The morphology of swift heavy ion tracks in the Gd2Zr2-xTixO7 pyrochlore system has been investigated as a function of the variation in chemical composition and electronic energy loss, dE/dx, over a range of energetic ions: 58Ni, 101Ru, 129Xe, 181Ta, 197Au, 208Pb, and 238U of 11.1 MeV/u specific energy. Bright-field transmission electron microscopy, synchrotron X-ray diffraction, and Raman spectroscopy reveal an increasing degree of amorphization with increasing Ti-content and dE/dx. The size and morphology of individual ion tracks in Gd2Ti2O7 were characterized by high-resolution transmission electron microscopy revealing a core-shell structure with an outer defect-fluorite dominated shell at low dE/dx to predominantly amorphous tracks at high dE/dx. Inelastic thermal-spike calculations have been used together with atomic-scale characterization of ion tracks in Gd2Ti2O7 by high resolution transmission electron microscopy to deduce critical energy densities for the complex core-shell morphologies induced by ions of different dE/dx.

Femtosecond time-resolved MeV electron diffraction

DOE PAGES

Zhu, Pengfei; Zhu, Y.; Hidaka, Y.; ...

2015-06-02

We report the experimental demonstration of femtosecond electron diffraction using high-brightness MeV electron beams. High-quality, single-shot electron diffraction patterns for both polycrystalline aluminum and single-crystal 1T-TaS 2 are obtained utilizing a 5 fC (~3 × 10 4 electrons) pulse of electrons at 2.8 MeV. The high quality of the electron diffraction patterns confirms that electron beam has a normalized emittance of ~50 nm rad. The transverse and longitudinal coherence length is ~11 and ~2.5 nm, respectively. The timing jitter between the pump laser and probe electron beam was found to be ~100 fs (rms). The temporal resolution is demonstrated bymore » observing the evolution of Bragg and superlattice peaks of 1T-TaS 2 following an 800 nm optical pump and was found to be 130 fs. Lastly, our results demonstrate the advantages of MeV electrons, including large elastic differential scattering cross-section and access to high-order reflections, and the feasibility of ultimately realizing below 10 fs time-resolved electron diffraction.« less

Electron diffraction covering a wide angular range from Bragg diffraction to small-angle diffraction.

PubMed

Nakajima, Hiroshi; Kotani, Atsuhiro; Harada, Ken; Mori, Shigeo

2018-04-09

We construct an electron optical system to investigate Bragg diffraction (the crystal lattice plane, 10-2 to 10-3 rad) with the objective lens turned off by adjusting the current in the intermediate lenses. A crossover was located on the selected-area aperture plane. Thus, the dark-field imaging can be performed by using a selected-area aperture to select Bragg diffraction spots. The camera length can be controlled in the range of 0.8-4 m without exciting the objective lens. Furthermore, we can observe the magnetic-field dependence of electron diffraction using the objective lens under weak excitation conditions. The diffraction mode for Bragg diffraction can be easily switched to a small-angle electron diffraction mode having a camera length of more than 100 m. We propose this experimental method to acquire electron diffraction patterns that depict an extensive angular range from 10-2 to 10-7 rad. This method is applied to analyze the magnetic microstructures in three distinct magnetic materials, i.e. a uniaxial magnetic structure of BaFe10.35Sc1.6Mg0.05O19, a martensite of a Ni-Mn-Ga alloy, and a helical magnetic structure of Ba0.5Sr1.5Zn2Fe12O22.

Hybrid Modes in Long Wavelength Free Electron Lasers

DTIC Science & Technology

2010-12-01

response, including the time for reviewing instruction, searching existing data sources, gathering and maintaining the data needed, and completing and...diffraction along one axis, allowing free space diffraction along the other axis. We continue the analysis of the relativistic electron beam, co-propagating...control diffraction along one axis, allowing free space diffraction along the other axis. We continue the analysis of the relativistic electron beam, co

Structure analysis of the single-domain Si(111)4 × 1-In surface by μ-probe Auger electron diffraction and μ-probe reflection high energy electron diffraction

NASA Astrophysics Data System (ADS)

Nakamura, N.; Anno, K.; Kono, S.

1991-10-01

A single-domain Si(111)4 × 1-In surface has been studied by μ-probe reflection high-energy electron diffraction (RHEED) to elucidate the symmetry of the 4 × 1 surface. Azimuthal diffraction patterns of In MNN Auger electron have been obtained by a μ-probe Auger electron diffraction (AED) apparatus from the single-domain Si(111)4 × 1-In surface. On the basis of information from scanning tunneling microscopy [J. Microsc. 152 (1988) 727] and under the assumption that the 4 × 1 surface is composed of In-overlayers, the μ-probe AED patterns were kinematically analyzed to reach a concrete model of indium arrangement.

Photocatalytic decomposition of Rhodamine B on uranium-doped mesoporous titanium dioxide

DOE PAGES

Liu, Yi; Becker, Blake; Burdine, Brandon; ...

2017-04-13

Mesoporous uranium-doped TiO 2 anatase materials were studied to determine the influence of U-doping on the photocatalytic properties for Rhodamine B (RhB) degradation. The physico-chemical properties of the samples were characterized and the results of X-ray diffraction, transmission electron microscopy, and Raman spectroscopy demonstrate homogeneous incorporation of uranium into the anatase lattice. X-ray photoelectron spectroscopy of the doped anatase confirmed the dominance of the U 4+ species and an increasing proportion of U 6+ species as the uranium doping was increased. The absorption thresholds of the uranium-doped anatase extended into the visible light region. A synergistic effect of the bandmore » gap energy and oxidation state of the dopant contribute to an enhanced photocatalytic capability for RhB degradation by U-doped TiO 2.« less

Photocatalytic decomposition of Rhodamine B on uranium-doped mesoporous titanium dioxide

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

Liu, Yi; Becker, Blake; Burdine, Brandon

Mesoporous uranium-doped TiO 2 anatase materials were studied to determine the influence of U-doping on the photocatalytic properties for Rhodamine B (RhB) degradation. The physico-chemical properties of the samples were characterized and the results of X-ray diffraction, transmission electron microscopy, and Raman spectroscopy demonstrate homogeneous incorporation of uranium into the anatase lattice. X-ray photoelectron spectroscopy of the doped anatase confirmed the dominance of the U 4+ species and an increasing proportion of U 6+ species as the uranium doping was increased. The absorption thresholds of the uranium-doped anatase extended into the visible light region. A synergistic effect of the bandmore » gap energy and oxidation state of the dopant contribute to an enhanced photocatalytic capability for RhB degradation by U-doped TiO 2.« less

Nanomodulated electron beams via electron diffraction and emittance exchange for coherent x-ray generation

DOE PAGES

Nanni, E. A.; Graves, W. S.; Moncton, D. E.

2018-01-19

We present a new method for generation of relativistic electron beams with current modulation on the nanometer scale and below. The current modulation is produced by diffracting relativistic electrons in single crystal Si, accelerating the diffracted beam and imaging the crystal structure, then transferring the image into the temporal dimension via emittance exchange. The modulation period can be tuned by adjusting electron optics after diffraction. This tunable longitudinal modulation can have a period as short as a few angstroms, enabling production of coherent hard x-rays from a source based on inverse Compton scattering with total accelerator length of approximately tenmore » meters. Electron beam simulations from cathode emission through diffraction, acceleration, and image formation with variable magnification are presented along with estimates of the coherent x-ray output properties.« less

Nanomodulated electron beams via electron diffraction and emittance exchange for coherent x-ray generation

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

Nanni, E. A.; Graves, W. S.; Moncton, D. E.

We present a new method for generation of relativistic electron beams with current modulation on the nanometer scale and below. The current modulation is produced by diffracting relativistic electrons in single crystal Si, accelerating the diffracted beam and imaging the crystal structure, then transferring the image into the temporal dimension via emittance exchange. The modulation period can be tuned by adjusting electron optics after diffraction. This tunable longitudinal modulation can have a period as short as a few angstroms, enabling production of coherent hard x-rays from a source based on inverse Compton scattering with total accelerator length of approximately tenmore » meters. Electron beam simulations from cathode emission through diffraction, acceleration, and image formation with variable magnification are presented along with estimates of the coherent x-ray output properties.« less

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

Zhao, Haishuang; Krysiak, Yaşar; Hoffmann, Kristin

The crystal structure and disorder phenomena of Al{sub 4}B{sub 2}O{sub 9}, an aluminum borate from the mullite-type family, were studied using automated diffraction tomography (ADT), a recently established method for collection and analysis of electron diffraction data. Al{sub 4}B{sub 2}O{sub 9}, prepared by sol-gel approach, crystallizes in the monoclinic space group C2/m. The ab initio structure determination based on three-dimensional electron diffraction data from single ordered crystals reveals that edge-connected AlO{sub 6} octahedra expanding along the b axis constitute the backbone. The ordered structure (A) was confirmed by TEM and HAADF-STEM images. Furthermore, disordered crystals with diffuse scattering along themore » b axis are observed. Analysis of the modulation pattern implies a mean superstructure (AAB) with a threefold b axis, where B corresponds to an A layer shifted by ½a and ½c. Diffraction patterns simulated for the AAB sequence including additional stacking disorder are in good agreement with experimental electron diffraction patterns. - Graphical abstract: Crystal structure and disorder phenomena of B-rich Al{sub 4}B{sub 2}O{sub 9} studied by automated electron diffraction tomography (ADT) and described by diffraction simulation using DISCUS. - Highlights: • Ab-initio structure solution by electron diffraction from single nanocrystals. • Detected modulation corresponding mainly to three-fold superstructure. • Diffuse diffraction streaks caused by stacking faults in disordered crystals. • Observed streaks explained by simulated electron diffraction patterns.« less

Splitting Fermi Surfaces and Heavy Electronic States in Non-Centrosymmetric U3Ni3Sn4

NASA Astrophysics Data System (ADS)

Maurya, Arvind; Harima, Hisatomo; Nakamura, Ai; Shimizu, Yusei; Homma, Yoshiya; Li, DeXin; Honda, Fuminori; Sato, Yoshiki J.; Aoki, Dai

2018-04-01

We report the single-crystal growth of the non-centrosymmetric paramagnet U3Ni3Sn4 by the Bridgman method and the Fermi surface properties detected by de Haas-van Alphen (dHvA) experiments. We have also investigated single-crystal U3Ni3Sn4 by single-crystal X-ray diffraction, magnetization, electrical resistivity, and heat capacity measurements. The angular dependence of the dHvA frequencies reveals many closed Fermi surfaces, which are nearly spherical in topology. The experimental results are in good agreement with local density approximation (LDA) band structure calculations based on the 5f-itinerant model. The band structure calculation predicts many Fermi surfaces, mostly with spherical shape, derived from 12 bands crossing the Fermi energy. To our knowledge, the splitting of Fermi surfaces due to the non-centrosymmetric crystal in 5f-electron systems is experimentally detected for the first time. The temperature dependence of the dHvA amplitude reveals a large cyclotron effective mass of up to 35 m0, indicating the heavy electronic state of U3Ni3Sn4 due to the proximity of the quantum critical point. From the field dependence of the dHvA amplitude, a mean free path of conduction electrons of up to 1950 Å is detected, reflecting the good quality of the grown crystal. The small splitting energy related to the antisymmetric spin-orbit interaction is most likely due to the large cyclotron effective mass.

Observations on the Role of Hydrogen in Facet Formation in Near-alpha Titanium (Preprint)

DTIC Science & Technology

2011-05-01

using quantitative tilt fractography and electron backscatter diffraction while facet topography was examined using ultra high resolution scanning...quantitative tilt fractography and electron backscatter diffraction while facet topography was examined using ultra high resolution scanning electron...tilt fractography / electron backscatter diffraction (EBSD) technique in which both the crystallographic orientation of the fractured grain and the

Total-scattering pair-distribution function of organic material from powder electron diffraction data.

PubMed

Gorelik, Tatiana E; Schmidt, Martin U; Kolb, Ute; Billinge, Simon J L

2015-04-01

This paper shows that pair-distribution function (PDF) analyses can be carried out on organic and organometallic compounds from powder electron diffraction data. Different experimental setups are demonstrated, including selected area electron diffraction and nanodiffraction in transmission electron microscopy or nanodiffraction in scanning transmission electron microscopy modes. The methods were demonstrated on organometallic complexes (chlorinated and unchlorinated copper phthalocyanine) and on purely organic compounds (quinacridone). The PDF curves from powder electron diffraction data, called ePDF, are in good agreement with PDF curves determined from X-ray powder data demonstrating that the problems of obtaining kinematical scattering data and avoiding beam damage of the sample are possible to resolve.

Doped Lanthanum Hafnates as Scintillating Materials for High-Energy Photon Detection

NASA Astrophysics Data System (ADS)

Wahid, Kareem; Pokhrel, Madhab; Mao, Yuanbing

Recent years have seen the emergence of nanocrystalline complex oxide scintillators for use in X-ray and gamma-ray detection. In this study, we investigate the structural and optical properties of La2Hf2O7 nanoparticles doped with varying levels of Eu3+ or Ce3+ by use of X-ray diffraction, Raman spectroscopy, scanning electron microscopy, transmission electron microscopy, and optical photoluminescence. In addition, scintillation response under X-ray and gamma-ray exposure is reported. The authors thank the support from the Defense Threat Reduction Agency (DTRA) of the U.S. Department of Defense (Award #HDTRA1-10-1-0114).

rf streak camera based ultrafast relativistic electron diffraction.

PubMed

Musumeci, P; Moody, J T; Scoby, C M; Gutierrez, M S; Tran, T

2009-01-01

We theoretically and experimentally investigate the possibility of using a rf streak camera to time resolve in a single shot structural changes at the sub-100 fs time scale via relativistic electron diffraction. We experimentally tested this novel concept at the UCLA Pegasus rf photoinjector. Time-resolved diffraction patterns from thin Al foil are recorded. Averaging over 50 shots is required in order to get statistics sufficient to uncover a variation in time of the diffraction patterns. In the absence of an external pump laser, this is explained as due to the energy chirp on the beam out of the electron gun. With further improvements to the electron source, rf streak camera based ultrafast electron diffraction has the potential to yield truly single shot measurements of ultrafast processes.

Oxidation behavior of U-Si compounds in air from 25 to 1000 C

NASA Astrophysics Data System (ADS)

Sooby Wood, E.; White, J. T.; Nelson, A. T.

2017-02-01

The air oxidation behavior of U3Si2, USi, and U3Si5 is studied from room temperature to 1000 C. The onsets of breakaway oxidation for each compound are identified during synthetic air ramps to 1000 C using thermogravimetric analysis. Isothermal air oxidation tests are performed below and above the breakaway oxidation onset to discern the oxidation kinetic behavior of these candidate accident tolerant fuel forms. Uranium metal is tested in the same manner to provide a reference for the oxidation behavior. Thermogravimetric, x-ray diffraction, and scanning electron microscopy analysis are presented here along with a discussion of the oxidation behavior of these materials and the impact of the lack of oxidation resistance to their deployment as accident tolerant nuclear fuels.

The Heisenberg Uncertainty Principle Demonstrated with An Electron Diffraction Experiment

ERIC Educational Resources Information Center

Matteucci, Giorgio; Ferrari, Loris; Migliori, Andrea

2010-01-01

An experiment analogous to the classical diffraction of light from a circular aperture has been realized with electrons. The results are used to introduce undergraduate students to the wave behaviour of electrons. The diffraction fringes produced by the circular aperture are compared to those predicted by quantum mechanics and are exploited to…

High quality single shot ultrafast MeV electron diffraction from a photocathode radio-frequency gun

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

Fu, Feichao; Liu, Shengguang; Zhu, Pengfei

2014-08-15

A compact ultrafast electron diffractometer, consisting of an s-band 1.6 cell photocathode radio-frequency gun, a multi-function changeable sample chamber, and a sensitive relativistic electron detector, was built at Shanghai Jiao Tong University. High-quality single-shot transmission electron diffraction patterns have been recorded by scattering 2.5 MeV electrons off single crystalline gold and polycrystalline aluminum samples. The high quality diffraction pattern indicates an excellent spatial resolution, with the ratio of the diffraction ring radius over the ring rms width beyond 10. The electron pulse width is estimated to be about 300 fs. The high temporal and spatial resolution may open new opportunities inmore » various areas of sciences.« less

High quality single shot ultrafast MeV electron diffraction from a photocathode radio-frequency gun.

PubMed

Fu, Feichao; Liu, Shengguang; Zhu, Pengfei; Xiang, Dao; Zhang, Jie; Cao, Jianming

2014-08-01

A compact ultrafast electron diffractometer, consisting of an s-band 1.6 cell photocathode radio-frequency gun, a multi-function changeable sample chamber, and a sensitive relativistic electron detector, was built at Shanghai Jiao Tong University. High-quality single-shot transmission electron diffraction patterns have been recorded by scattering 2.5 MeV electrons off single crystalline gold and polycrystalline aluminum samples. The high quality diffraction pattern indicates an excellent spatial resolution, with the ratio of the diffraction ring radius over the ring rms width beyond 10. The electron pulse width is estimated to be about 300 fs. The high temporal and spatial resolution may open new opportunities in various areas of sciences.

Total-scattering pair-distribution function of organic material from powder electron diffraction data

DOE PAGES

Gorelik, Tatiana E.; Billinge, Simon J. L.; Schmidt, Martin U.; ...

2015-04-01

This paper shows for the first time that pair-distribution function analyses can be carried out on organic and organo-metallic compounds from powder electron diffraction data. Different experimental setups are demonstrated, including selected area electron diffraction (SAED) and nanodiffraction in transmission electron microscopy (TEM) or nanodiffraction in scanning transmission electron microscopy (STEM) modes. The methods were demonstrated on organo-metallic complexes (chlorinated and unchlorinated copper-phthalocyanine) and on purely organic compounds (quinacridone). The PDF curves from powder electron diffraction data, called ePDF, are in good agreement with PDF curves determined from X-ray powder data demonstrating that the problems of obtaining kinematical scattering datamore » and avoiding beam-damage of the sample are possible to resolve.« less

Ultrafast electron diffraction optimized for studying structural dynamics in thin films and monolayers

PubMed Central

Badali, D. S.; Gengler, R. Y. N.; Miller, R. J. D.

2016-01-01

A compact electron source specifically designed for time-resolved diffraction studies of free-standing thin films and monolayers is presented here. The sensitivity to thin samples is achieved by extending the established technique of ultrafast electron diffraction to the “medium” energy regime (1–10 kV). An extremely compact design, in combination with low bunch charges, allows for high quality diffraction in a lensless geometry. The measured and simulated characteristics of the experimental system reveal sub-picosecond temporal resolution, while demonstrating the ability to produce high quality diffraction patterns from atomically thin samples. PMID:27226978

Dark-field imaging based on post-processed electron backscatter diffraction patterns of bulk crystalline materials in a scanning electron microscope.

PubMed

Brodusch, Nicolas; Demers, Hendrix; Gauvin, Raynald

2015-01-01

Dark-field (DF) images were acquired in the scanning electron microscope with an offline procedure based on electron backscatter diffraction (EBSD) patterns (EBSPs). These EBSD-DF images were generated by selecting a particular reflection on the electron backscatter diffraction pattern and by reporting the intensity of one or several pixels around this point at each pixel of the EBSD-DF image. Unlike previous studies, the diffraction information of the sample is the basis of the final image contrast with a pixel scale resolution at the EBSP providing DF imaging in the scanning electron microscope. The offline facility of this technique permits the selection of any diffraction condition available in the diffraction pattern and displaying the corresponding image. The high number of diffraction-based images available allows a better monitoring of deformation structures compared to electron channeling contrast imaging (ECCI) which is generally limited to a few images of the same area. This technique was applied to steel and iron specimens and showed its high capability in describing more rigorously the deformation structures around micro-hardness indents. Due to the offline relation between the reference EBSP and the EBSD-DF images, this new technique will undoubtedly greatly improve our knowledge of deformation mechanism and help to improve our understanding of the ECCI contrast mechanisms. Copyright © 2014 Elsevier B.V. All rights reserved.

Uranium oxidation kinetics monitored by in-situ X-ray diffraction

NASA Astrophysics Data System (ADS)

Zalkind, S.; Rafailov, G.; Halevy, I.; Livneh, T.; Rubin, A.; Maimon, H.; Schweke, D.

2017-03-01

The oxidation kinetics of U-0.1 wt%Cr at oxygen pressures of 150 Torr and the temperature range of 90-150 °C was studied by means of in-situ X-ray diffraction (XRD). A "breakaway" in the oxidation kinetics is found at ∼0.25 μm, turning from a parabolic to a linear rate law. At the initial stage of oxidation the growth plane of UO2(111) is the prominent one. As the oxide thickens, the growth rate of UO2(220) plane increases and both planes grow concurrently. The activation energies obtained for the oxide growth are Qparabolic = 17.5 kcal/mol and Qlinear = 19 kcal/mol. Enhanced oxidation around uranium carbide (UC) inclusions is clearly observed by scanning electron microscopy (SEM).

Femtosecond gas phase electron diffraction with MeV electrons.

PubMed

Yang, Jie; Guehr, Markus; Vecchione, Theodore; Robinson, Matthew S; Li, Renkai; Hartmann, Nick; Shen, Xiaozhe; Coffee, Ryan; Corbett, Jeff; Fry, Alan; Gaffney, Kelly; Gorkhover, Tais; Hast, Carsten; Jobe, Keith; Makasyuk, Igor; Reid, Alexander; Robinson, Joseph; Vetter, Sharon; Wang, Fenglin; Weathersby, Stephen; Yoneda, Charles; Wang, Xijie; Centurion, Martin

2016-12-16

We present results on ultrafast gas electron diffraction (UGED) experiments with femtosecond resolution using the MeV electron gun at SLAC National Accelerator Laboratory. UGED is a promising method to investigate molecular dynamics in the gas phase because electron pulses can probe the structure with a high spatial resolution. Until recently, however, it was not possible for UGED to reach the relevant timescale for the motion of the nuclei during a molecular reaction. Using MeV electron pulses has allowed us to overcome the main challenges in reaching femtosecond resolution, namely delivering short electron pulses on a gas target, overcoming the effect of velocity mismatch between pump laser pulses and the probe electron pulses, and maintaining a low timing jitter. At electron kinetic energies above 3 MeV, the velocity mismatch between laser and electron pulses becomes negligible. The relativistic electrons are also less susceptible to temporal broadening due to the Coulomb force. One of the challenges of diffraction with relativistic electrons is that the small de Broglie wavelength results in very small diffraction angles. In this paper we describe the new setup and its characterization, including capturing static diffraction patterns of molecules in the gas phase, finding time-zero with sub-picosecond accuracy and first time-resolved diffraction experiments. The new device can achieve a temporal resolution of 100 fs root-mean-square, and sub-angstrom spatial resolution. The collimation of the beam is sufficient to measure the diffraction pattern, and the transverse coherence is on the order of 2 nm. Currently, the temporal resolution is limited both by the pulse duration of the electron pulse on target and by the timing jitter, while the spatial resolution is limited by the average electron beam current and the signal-to-noise ratio of the detection system. We also discuss plans for improving both the temporal resolution and the spatial resolution.

A Medipix quantum area detector allows rotation electron diffraction data collection from submicrometre three-dimensional protein crystals

PubMed Central

Nederlof, Igor; van Genderen, Eric; Li, Yao-Wang; Abrahams, Jan Pieter

2013-01-01

When protein crystals are submicrometre-sized, X-ray radiation damage precludes conventional diffraction data collection. For crystals that are of the order of 100 nm in size, at best only single-shot diffraction patterns can be collected and rotation data collection has not been possible, irrespective of the diffraction technique used. Here, it is shown that at a very low electron dose (at most 0.1 e− Å−2), a Medipix2 quantum area detector is sufficiently sensitive to allow the collection of a 30-frame rotation series of 200 keV electron-diffraction data from a single ∼100 nm thick protein crystal. A highly parallel 200 keV electron beam (λ = 0.025 Å) allowed observation of the curvature of the Ewald sphere at low resolution, indicating a combined mosaic spread/beam divergence of at most 0.4°. This result shows that volumes of crystal with low mosaicity can be pinpointed in electron diffraction. It is also shown that strategies and data-analysis software (MOSFLM and SCALA) from X-ray protein crystallography can be used in principle for analysing electron-diffraction data from three-dimensional nanocrystals of proteins. PMID:23793148

Conceptual Design for Time-Resolved X-ray Diffraction in a Single Laser-Driven Compression Experiment

NASA Astrophysics Data System (ADS)

Benedetti, Laura Robin; Eggert, J. H.; Kilkenny, J. D.; Bradley, D. K.; Bell, P. M.; Palmer, N. E.; Rygg, J. R.; Boehly, T. R.; Collins, G. W.; Sorce, C.

2017-06-01

Since X-ray diffraction is the most definitive method for identifying crystalline phases of a material, it is an important technique for probing high-energy-density materials during laser-driven compression experiments. We are developing a design for collecting several x-ray diffraction datasets during a single laser-driven experiment, with a goal of achieving temporal resolution better than 1ns. The design combines x-ray streak cameras, for a continuous temporal record of diffraction, with fast x-ray imagers, to collect several diffraction patterns with sufficient solid angle range and resolution to identify crystalline texture. Preliminary experiments will be conducted at the Omega laser and then implemented at the National Ignition Facility. We will describe the status of the conceptual design, highlighting tradeoffs in the design process. We will also discuss the technical issues that must be addressed in order to develop a successful experimental platform. These include: Facility-specific geometric constraints such as unconverted laser light and target alignment; EMP issues when electronic diagnostics are close to the target; X-ray source requirements; and detector capabilities. This work was performed under the auspices of the U.S. Department of Energy by Lawrence Livermore National Laboratory under Contract DE-AC52-07NA27344, LLNL-ABS-725146.

Three-dimensional electron diffraction of plant light-harvesting complex

PubMed Central

Wang, Da Neng; Kühlbrandt, Werner

1992-01-01

Electron diffraction patterns of two-dimensional crystals of light-harvesting chlorophyll a/b-protein complex (LHC-II) from photosynthetic membranes of pea chloroplasts, tilted at different angles up to 60°, were collected to 3.2 Å resolution at -125°C. The reflection intensities were merged into a three-dimensional data set. The Friedel R-factor and the merging R-factor were 21.8 and 27.6%, respectively. Specimen flatness and crystal size were critical for recording electron diffraction patterns from crystals at high tilts. The principal sources of experimental error were attributed to limitations of the number of unit cells contributing to an electron diffraction pattern, and to the critical electron dose. The distribution of strong diffraction spots indicated that the three-dimensional structure of LHC-II is less regular than that of other known membrane proteins and is not dominated by a particular feature of secondary structure. ImagesFIGURE 1FIGURE 2 PMID:19431817

Structural, Electronic and Vibrational Properties of Nax Si 136(0 < x < 24) Clathrates

NASA Astrophysics Data System (ADS)

Higgins, Craig; Nenghabi, Emmanuel; Myles, Charles; Biswas, Koushik; Beekman, Matt; Nolas, George

2011-03-01

CRAIG HIGGINS, EMMANUEL NENGHA BI† , CHARLES W. MYLES, Texas Tech U.; KOUSHIK BISWAS, Oak Ridge National Lab; MATT BEEKMAN, U. of Oregon; GEORGE S. NOLAS, U. of South Florida - Na x Si 136 is a Type II clathrate with important thermoelectric properties. It's face-centered cubic lattice contains polyhedral ``cages'' of silicon atoms with Na atom ``guests'' in the cages. This material is very interesting because powder X-ray diffraction experiments 1 for differing Na content x have shown that, for increasing x in the range 0

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.

Incident-beam effects in electron-stimulated Auger-electron diffraction

NASA Astrophysics Data System (ADS)

Gao, Y.; Cao, Jianming

1991-04-01

We have examined incident-beam effects in electron-stimulated Auger-electron diffraction (AED) on a cleaved GaAs(110) surface. The results indicate that incident-beam diffraction is significant in an AED experiment, and that the dissipative nature of the incident beam in contributing to the Auger process must be accounted for. We have developed a qualitative model that describes the trend of the polar-angle dependence of the Auger intensity for both the incident and exit beams. In calculating the diffraction features, we used a zeroth-order approximation to simulate the dissipation of the incident beam, which is found to adequately describe the experimental data.

Exploring coherent electron excitation and migration dynamics by electron diffraction with ultrashort X-ray pulses.

PubMed

Yuan, Kai-Jun; Bandrauk, André D

2017-10-04

Exploring ultrafast charge migration is of great importance in biological and chemical reactions. We present a scheme to monitor attosecond charge migration in molecules by electron diffraction with spatial and temporal resolutions from ab initio numerical simulations. An ultraviolet pulse creates a coherent superposition of electronic states, after which a time-delayed attosecond X-ray pulse is used to ionize the molecule. It is found that diffraction patterns in the X-ray photoelectron spectra show an asymmetric structure, which is dependent on the time delay between the pump-probe pulses, encoding the information of molecular orbital symmetry and chemical bonding. We describe these phenomena by developing an electronic time-dependent ultrafast molecular photoionization model of a coherent superposition state. The periodical distortion of electron diffraction patterns illustrates the evolution of the electronic coherence, providing a tool for attosecond imaging of ultrafast molecular reaction processes.

A series of uranium (IV, V, VI) tritylimido complexes, their molecular and electronic structures and reactivity with CO2.

PubMed

Schmidt, Anna-Corina; Heinemann, Frank W; Maron, Laurent; Meyer, Karsten

2014-12-15

A series of uranium tritylimido complexes with structural continuity across complexes in different oxidation states, namely U(IV), U(V), and U(VI), is reported. This series was successfully synthesized by employing the trivalent uranium precursor, [(((nP,Me)ArO)3tacn)U(III)] (1) (where ((nP,Me)ArO)3tacn(3-) = trianion of 1,4,7-tris(2-hydroxy-5-methyl-3-neopentylbenzyl)-1,4,7-triazacyclononane), with the organic azides Me3SiN3, Me3SnN3, and Ph3CN3 (tritylazide). While the reaction with Me3SiN3 yields an inseparable mixture of both the azido and imido uranium complexes, applying the heavier Sn homologue yields the bis-μ-azido complex [{(((nP,Me)ArO)3tacn)U(IV)}2(μ-N3)2] (2) exclusively. In contrast to this one-electron redox chemistry, the reaction of precursor 1 with tritylazide solely leads to the two-electron oxidized U(V) imido [(((nP,Me)ArO)3tacn)U(V)(N-CPh3)] (3). Oxidation and reduction of 3 yield the corresponding U(VI) and U(IV) complexes [(((nP,Me)ArO)3tacn)U(VI)(N-CPh3)][B(C6F5)4] (4) and K[(((nP,Me)ArO)3tacn)U(IV)(N-CPh3)] (5), respectively. In addition, the U(V) imido 3 engages in a H atom abstraction reaction with toluene to yield the closely related amido complex [(((nP,Me)ArO)3tacn)U(IV)(N(H)-CPh3)] (6). Complex 6 and the three tritylimido complexes 3, 4, and 5, with oxidation states ranging from +IV to +VI and homologous core structures, were investigated by X-ray diffraction analyses and magnetochemical and spectroscopic studies as well as density functional theory (DFT) computational analysis. The series of structurally very similar imido complexes provides a unique opportunity to study electronic properties and to probe the uranium imido reactivity solely as a function of electron count of the metal-imido entity. Evidence for the U-N bond covalency and f-orbital participation in complexes 3-6 was drawn from the in-depth and comparative DFT study. The reactivity of the imido and amido complexes with CO2 was probed, and conclusions about the influence of the formal oxidation state are reported.

Nonlocal Electron Coherence in MoS2 Flakes Correlated through Spatial Self Phase Modulation

NASA Astrophysics Data System (ADS)

Wu, Yanling; Wu, Qiong; Sun, Fei; Tian, Yichao; Zuo, Xu; Meng, Sheng; Zhao, Jimin

2015-03-01

Electron coherence among different flake domains of MoS2 has been generated using ultrafast or continuous wave laser beams. Such electron coherence generates characteristic far-field diffraction patterns through a purely coherent nonlinear optical effect--spatial self-phase modulation (SSPM). A wind-chime model is developed to describe the establishment of the electron coherence through correlating the photo-excited electrons among different flakes using coherent light. Owing to its finite gap band structure, we find different mechanisms, including two-photon processes, might be responsible for the SSPM in MoS2 [with a large nonlinear dielectric susceptibility χ (3) = 1.6 × 10-9 e.s.u. (SI: 2.23 × 10-17 m2/V2) per layer]. Finally, we realized all optical switching based on SSPM, demonstrating that the electron coherence generation we report here is a ubiquitous property of layered quantum materials, by which novel optical applications are accessible. National Natural Science Foundation of China (11274372).

Effect of High Si Content on U3Si2 Fuel Microstructure

NASA Astrophysics Data System (ADS)

Rosales, Jhonathan; van Rooyen, Isabella J.; Meher, Subhashish; Hoggan, Rita; Parga, Clemente; Harp, Jason

2018-02-01

The development of U3Si2 as an accident-tolerant nuclear fuel has gained research interest because of its promising high uranium density and improved thermal properties. In the present study, three samples of U3Si2 fuel with varying silicon content have been fabricated by a conventional powder metallurgical route. Microstructural characterization via scanning and transmission electron microscopy reveals the presence of other stoichiometry of uranium silicide such as USi and UO2 in both samples. The detailed phase analysis by x-ray diffraction shows the presence of secondary phases, such as USi, U3Si, and UO2. The samples with higher concentrations of silicon content of 7.5 wt.% display additional elemental Si. These samples also possess an increased amount of the USi phase as compared to that in the conventional sample with 7.3 wt.% silicon. The optimization of U3Si2 fuel performance through the understanding of the role of Si content on its microstructure has been discussed.

Electron coherent diffraction tomography of a nanocrystal

NASA Astrophysics Data System (ADS)

Dronyak, Roman; Liang, Keng S.; Tsai, Jin-Sheng; Stetsko, Yuri P.; Lee, Ting-Kuo; Chen, Fu-Rong

2010-05-01

Coherent diffractive imaging (CDI) with electron or x-ray sources is a promising technique for investigating the structure of nanoparticles down to the atomic scale. In electron CDI, a two-dimensional reconstruction is demonstrated using highly coherent illumination from a field-emission gun as a source of electrons. In a three-dimensional (3D) electron CDI, we experimentally determine the morphology of a single MgO nanocrystal using the Bragg diffraction geometry. An iterative algorithm is applied to invert the 3D diffraction pattern about a (200) reflection of the nanoparticle measured at an angular range of 1.8°. The results reveal a 3D image of the sample at ˜8 nm resolution, and agree with a simulation. Our work demonstrates an alternative approach to obtain the 3D structure of nanocrystals with an electron microscope.

Oxidation behavior of U-Si compounds in air from 25 to 1000 C

DOE PAGES

Wood, E. Sooby; White, J. T.; Nelson, A. T.

2016-12-18

The air oxidation behavior of U 3Si 2, USi, and U 3Si 5 is studied from room temperature to 1000 C. Moreover, the onsets of breakaway oxidation for each compound are identified during synthetic air ramps to 1000 C using thermogravimetric analysis. Isothermal air oxidation tests are performed below and above the breakaway oxidation onset to discern the oxidation kinetic behavior of these candidate accident tolerant fuel forms. Uranium metal is tested in the same manner to provide a reference for the oxidation behavior. We present thermogravimetric, x-ray diffraction, and scanning electron microscopy analysis here along with a discussion ofmore » the oxidation behavior of these materials and the impact of the lack of oxidation resistance to their deployment as accident tolerant nuclear fuels.« less

Suppressing Ghost Diffraction in E-Beam-Written Gratings

NASA Technical Reports Server (NTRS)

Wilson, Daniel; Backlund, Johan

2009-01-01

A modified scheme for electron-beam (E-beam) writing used in the fabrication of convex or concave diffraction gratings makes it possible to suppress the ghost diffraction heretofore exhibited by such gratings. Ghost diffraction is a spurious component of diffraction caused by a spurious component of grating periodicity as described below. The ghost diffraction orders appear between the main diffraction orders and are typically more intense than is the diffuse scattering from the grating. At such high intensity, ghost diffraction is the dominant source of degradation of grating performance. The pattern of a convex or concave grating is established by electron-beam writing in a resist material coating a substrate that has the desired convex or concave shape. Unfortunately, as a result of the characteristics of electrostatic deflectors used to control the electron beam, it is possible to expose only a small field - typically between 0.5 and 1.0 mm wide - at a given fixed position of the electron gun relative to the substrate. To make a grating larger than the field size, it is necessary to move the substrate to make it possible to write fields centered at different positions, so that the larger area is synthesized by "stitching" the exposed fields.

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

Hayashida, Misa; Malac, Marek; Egerton, Ray F.

Electron tomography is a method whereby a three-dimensional reconstruction of a nanoscale object is obtained from a series of projected images measured in a transmission electron microscope. We developed an electron-diffraction method to measure the tilt and azimuth angles, with Kikuchi lines used to align a series of diffraction patterns obtained with each image of the tilt series. Since it is based on electron diffraction, the method is not affected by sample drift and is not sensitive to sample thickness, whereas tilt angle measurement and alignment using fiducial-marker methods are affected by both sample drift and thickness. The accuracy ofmore » the diffraction method benefits reconstructions with a large number of voxels, where both high spatial resolution and a large field of view are desired. The diffraction method allows both the tilt and azimuth angle to be measured, while fiducial marker methods typically treat the tilt and azimuth angle as an unknown parameter. The diffraction method can be also used to estimate the accuracy of the fiducial marker method, and the sample-stage accuracy. A nano-dot fiducial marker measurement differs from a diffraction measurement by no more than ±1°.« less

Dynamic diffraction effects and coherent breathing oscillations in ultrafast electron diffraction in layered 1T-TaSeTe

PubMed Central

Wei, Linlin; Sun, Shuaishuai; Guo, Cong; Li, Zhongwen; Sun, Kai; Liu, Yu; Lu, Wenjian; Sun, Yuping; Tian, Huanfang; Yang, Huaixin; Li, Jianqi

2017-01-01

Anisotropic lattice movements due to the difference between intralayer and interlayer bonding are observed in the layered transition-metal dichalcogenide 1T-TaSeTe following femtosecond laser pulse excitation. Our ultrafast electron diffraction investigations using 4D-transmission electron microscopy (4D-TEM) clearly reveal that the intensity of Bragg reflection spots often changes remarkably due to the dynamic diffraction effects and anisotropic lattice movement. Importantly, the temporal diffracted intensity from a specific crystallographic plane depends on the deviation parameter s, which is commonly used in the theoretical study of diffraction intensity. Herein, we report on lattice thermalization and structural oscillations in layered 1T-TaSeTe, analyzed by dynamic diffraction theory. Ultrafast alterations of satellite spots arising from the charge density wave in the present system are also briefly discussed. PMID:28470025

Coherent diffraction imaging analysis of shape-controlled nanoparticles with focused hard X-ray free-electron laser pulses.

PubMed

Takahashi, Yukio; Suzuki, Akihiro; Zettsu, Nobuyuki; Oroguchi, Tomotaka; Takayama, Yuki; Sekiguchi, Yuki; Kobayashi, Amane; Yamamoto, Masaki; Nakasako, Masayoshi

2013-01-01

We report the first demonstration of the coherent diffraction imaging analysis of nanoparticles using focused hard X-ray free-electron laser pulses, allowing us to analyze the size distribution of particles as well as the electron density projection of individual particles. We measured 1000 single-shot coherent X-ray diffraction patterns of shape-controlled Ag nanocubes and Au/Ag nanoboxes and estimated the edge length from the speckle size of the coherent diffraction patterns. We then reconstructed the two-dimensional electron density projection with sub-10 nm resolution from selected coherent diffraction patterns. This method enables the simultaneous analysis of the size distribution of synthesized nanoparticles and the structures of particles at nanoscale resolution to address correlations between individual structures of components and the statistical properties in heterogeneous systems such as nanoparticles and cells.

Electron Backscatter Diffraction (EBSD) Analysis and U-Pb Geochronology of the Oldest Lunar Zircon: Constraining Early Lunar Differentiation and Dating Impact-Related Deformation

NASA Technical Reports Server (NTRS)

Timms, Nick; Nemchin, Alexander; Grange, Marion; Reddy, Steve; Pidgeon, Bob; Geisler, Thorsten; Meyer, Chuck

2009-01-01

The evolution of the early moon was dominated by two processes (i) crystallization of the Lunar Magma Ocean (LMO) and differentiation of potassium-rare earth element-phosphorous-rich residual magma reservoir referred to as KREEP, and (ii) an intense meteorite bombardment referred to as lunar cataclysm . The exact timing of these processes is disputed, and resolution relies on collection and interpretation of precise age data. This study examines the microstructure and geochronology of zircon from lunar impact breccias collected during the Apollo 17 mission. A large zircon clast within lunar breccia 72215,195 shows sector zoning in optical microscopy, cathodoluminescence (CL) imaging and Raman mapping, and indicates that it was a relict fragment of a much larger magmatic grain. Sensitive high resolution ion microprobe (SHRIMP) U-Pb analysis of the zircon shows that U and Th concentration correlate with sector zoning, with darkest CL domains corresponding with high-U and Th (approx.150 and approx.100 ppm respectively), and the brightest-CL sectors containing approx.30-50 ppm U and approx.10-20 ppm Th. This indicates that variations in optical CL and Raman properties correspond to differential accumulation of alpha-radiation damage in each sector. Electron backscatter diffraction (EBSD) mapping shows that the quality of electron backscatter patterns (band contrast) varies with sector zoning, with the poorest quality patterns obtained from high-U and Th, dark-CL zones. EBSD mapping also reveals a deformation microstructure that is cryptic in optical, CL and Raman imaging. Two orthogonal sets of straight discrete and gradational low-angle boundaries accommodate approx.12 misorientation across the grain. The deformation bands are parallel to the crystallographic {a}-planes of the zircon, have misorientation axes parallel to the c-axis, and are geometrically consistent with formation by dislocation creep associated with <100>{010} slip. The deformation bands are unlike curved morphology of crystal-plastic microstructures in tectonically deformed terrestrial zircon, and geometrically similar to dislocation microstructures reported in experimentally shocked zircon. We interpret these crystal-plastic deformation microstructures to have resulted from a significant impact, either directly from impact shock, or during ductile flow directly following the impact. The deformation bands appear to continue undeflected through the non-indexed, radiation-damaged areas of the grain, which suggests that the orientation variation predates any significant mechanical weakening from radiation damage in the grain, and therefore occurred early in its history.

Improvement of Strength-Toughness-Hardness Balance in Large Cross-Section 718H Pre-Hardened Mold Steel

PubMed Central

Liu, Hanghang; Fu, Paixian; Liu, Hongwei; Li, Dianzhong

2018-01-01

The strength-toughness combination and hardness uniformity in large cross-section 718H pre-hardened mold steel from a 20 ton ingot were investigated with three different heat treatments for industrial applications. The different microstructures, including tempered martensite, lower bainite, and retained austenite, were obtained at equivalent hardness. The microstructures were characterized by using metallographic observations, scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), and electron back-scattered diffraction (EBSD). The mechanical properties were compared by tensile, Charpy U-notch impact and hardness uniformity tests at room temperature. The results showed that the test steels after normalizing-quenching-tempering (N-QT) possessed the best strength-toughness combination and hardness uniformity compared with the conventional quenched-tempered (QT) steel. In addition, the test steel after austempering-tempering (A-T) demonstrated the worse hardness uniformity and lower yield strength while possessing relatively higher elongation (17%) compared with the samples after N-QT (14.5%) treatments. The better ductility of A-T steel mainly depended on the amount and morphology of retained austenite and thermal/deformation-induced twined martensite. This work elucidates the mechanisms of microstructure evolution during heat treatments and will highly improve the strength-toughness-hardness trade-off in large cross-section steels. PMID:29642642

High quality single shot diffraction patterns using ultrashort megaelectron volt electron beams from a radio frequency photoinjector.

PubMed

Musumeci, P; Moody, J T; Scoby, C M; Gutierrez, M S; Bender, H A; Wilcox, N S

2010-01-01

Single shot diffraction patterns using a 250-fs-long electron beam have been obtained at the UCLA Pegasus laboratory. High quality images with spatial resolution sufficient to distinguish closely spaced peaks in the Debye-Scherrer ring pattern have been recorded by scattering the 1.6 pC 3.5 MeV electron beam generated in the rf photoinjector off a 100-nm-thick Au foil. Dark current and high emittance particles are removed from the beam before sending it onto the diffraction target using a 1 mm diameter collimating hole. These results open the door to the study of irreversible phase transformations by single shot MeV electron diffraction.

High-resolution scanning precession electron diffraction: Alignment and spatial resolution.

PubMed

Barnard, Jonathan S; Johnstone, Duncan N; Midgley, Paul A

2017-03-01

Methods are presented for aligning the pivot point of a precessing electron probe in the scanning transmission electron microscope (STEM) and for assessing the spatial resolution in scanning precession electron diffraction (SPED) experiments. The alignment procedure is performed entirely in diffraction mode, minimising probe wander within the bright-field (BF) convergent beam electron diffraction (CBED) disk and is used to obtain high spatial resolution SPED maps. Through analysis of the power spectra of virtual bright-field images extracted from the SPED data, the precession-induced blur was measured as a function of precession angle. At low precession angles, SPED spatial resolution was limited by electronic noise in the scan coils; whereas at high precession angles SPED spatial resolution was limited by tilt-induced two-fold astigmatism caused by the positive spherical aberration of the probe-forming lens. Copyright © 2016 Elsevier B.V. All rights reserved.

Specimen-thickness effects on transmission Kikuchi patterns in the scanning electron microscope.

PubMed

Rice, K P; Keller, R R; Stoykovich, M P

2014-06-01

We report the effects of varying specimen thickness on the generation of transmission Kikuchi patterns in the scanning electron microscope. Diffraction patterns sufficient for automated indexing were observed from films spanning nearly three orders of magnitude in thickness in several materials, from 5 nm of hafnium dioxide to 3 μm of aluminum, corresponding to a mass-thickness range of ~5 to 810 μg cm(-2) . The scattering events that are most likely to be detected in transmission are shown to be very near the exit surface of the films. The energies, spatial distribution and trajectories of the electrons that are transmitted through the film and are collected by the detector are predicted using Monte Carlo simulations. Published 2014. This article is a U.S. Government work and is in the public domain in the USA.

Evidence for the suppression of incident beam effects in Auger electron diffraction

NASA Astrophysics Data System (ADS)

Davoli, I.; Gunnella, R.; Bernardini, R.; De Crescenzi, M.

1998-01-01

Auger electron diffraction (AED) of the Cu(100) surface has been studied through the anisotropy of the elastic backdiffused beam electrons, the L 2,3M 4,5M 4,5 (LVV) and the M 2,3M 4,5M 4,5 (MVV) transitions in polar scan along the two main directions [001], [011] and in azimuth scan at normal emission. The intensity anisotropies of the low and high kinetic energy Auger lines are in antiphase to each other as in experiments in which these transitions are excited by X-ray photons. This behaviour has been exploited to single out the origin of the physical mechanisms accompanying the diffraction of the emitted electrons. Incident beam effects appear to be sizeable only when the collection of the AED spectra are made with an angle integrating electron analyser (cylindrical mirror analyser or low electron energy diffraction apparatus), but they appear negligible when electron collection is performed through a small solid-angle detector. The conclusions reached by our measurements are supported by good agreement with experimental and theoretical X-ray photoelectron diffraction data and demonstrate that, when the incident beam energy is sufficiently higher than the kinetic energy of the Auger electron detected, the influence of the incident beam on AED is negligible.

Crystallography and Morphology of Niobium Carbide in As-Cast HP-Niobium Reformer Tubes

NASA Astrophysics Data System (ADS)

Buchanan, Karl G.; Kral, Milo V.

2012-06-01

The microstructures of two as-cast heats of niobium-modified HP stainless steels were characterized. Particular attention was paid to the interdendritic niobium-rich carbides formed during solidification of these alloys. At low magnifications, these precipitates are grouped in colonies of similar lamellae. Higher magnifications revealed that the lamellae actually obtain two distinct morphologies. The type I morphology exhibits broad planar interfaces with a smooth platelike shape. Type II lamellae have undulating interfaces and an overall reticulated shape. To provide further insight into the origin of these two different morphologies, the microstructure and crystallography of each have been studied in detail using high resolution scanning electron microscopy, transmission electron microscopy, various electron diffraction methods (electron backscatter diffraction (EBSD), selected area diffraction (SAD), and convergent beam electron diffraction (CBED)), and energy dispersive X-ray spectroscopy.

Excitation of phonons in medium-energy electron diffraction

NASA Astrophysics Data System (ADS)

Alvarez, M. A. Vicente; Ascolani, H.; Zampieri, G.

1996-03-01

The ``elastic'' backscattering of electrons from crystalline surfaces presents two regimes: a low-energy regime, in which the characteristic low-energy electron diffraction (LEED) pattern is observed, and a medium-energy regime, in which the diffraction pattern is similar to those observed in x-ray photoemission diffraction (XPD) and Auger electron diffraction (AED) experiments. We present a model for the electron scattering which, including the vibrational degrees of freedom of the crystal, contains both regimes and explains the passage from one regime to the other. Our model is based on a separation of the electron and atomic motions (adiabatic approximation) and on a cluster-type formulation of the multiple scattering of the electron. The inelastic scattering events (excitation and/or absorption of phonons) are treated as coherent processes and no break of the phase relation between the incident and the exit paths of the electron is assumed. The LEED and the medium-energy electron diffraction regimes appear naturally in this model as the limit cases of completely elastic scattering and of inelastic scattering with excitation and/or absorption of multiple phonons. Intensity patterns calculated with this model are in very good agreement with recent experiments of electron scattering on Cu(001) at low and medium energies. We show that there is a correspondence between the type of intensity pattern and the mean number of phonons excited and/or absorbed during the scattering: a LEED-like pattern is observed when this mean number is less than 2, LEED-like and XPD/AED-like features coexist when this number is 3-4, and a XPD/AED-like pattern is observed when this number is greater than 5-6.

Diffraction effects and inelastic electron transport in angle-resolved microscopic imaging applications.

PubMed

Winkelmann, A; Nolze, G; Vespucci, S; Naresh-Kumar, G; Trager-Cowan, C; Vilalta-Clemente, A; Wilkinson, A J; Vos, M

2017-09-01

We analyse the signal formation process for scanning electron microscopic imaging applications on crystalline specimens. In accordance with previous investigations, we find nontrivial effects of incident beam diffraction on the backscattered electron distribution in energy and momentum. Specifically, incident beam diffraction causes angular changes of the backscattered electron distribution which we identify as the dominant mechanism underlying pseudocolour orientation imaging using multiple, angle-resolving detectors. Consequently, diffraction effects of the incident beam and their impact on the subsequent coherent and incoherent electron transport need to be taken into account for an in-depth theoretical modelling of the energy- and momentum distribution of electrons backscattered from crystalline sample regions. Our findings have implications for the level of theoretical detail that can be necessary for the interpretation of complex imaging modalities such as electron channelling contrast imaging (ECCI) of defects in crystals. If the solid angle of detection is limited to specific regions of the backscattered electron momentum distribution, the image contrast that is observed in ECCI and similar applications can be strongly affected by incident beam diffraction and topographic effects from the sample surface. As an application, we demonstrate characteristic changes in the resulting images if different properties of the backscattered electron distribution are used for the analysis of a GaN thin film sample containing dislocations. © 2017 The Authors. Journal of Microscopy published by JohnWiley & Sons Ltd on behalf of Royal Microscopical Society.

Data processing software suite SITENNO for coherent X-ray diffraction imaging using the X-ray free-electron laser SACLA.

PubMed

Sekiguchi, Yuki; Oroguchi, Tomotaka; Takayama, Yuki; Nakasako, Masayoshi

2014-05-01

Coherent X-ray diffraction imaging is a promising technique for visualizing the structures of non-crystalline particles with dimensions of micrometers to sub-micrometers. Recently, X-ray free-electron laser sources have enabled efficient experiments in the `diffraction before destruction' scheme. Diffraction experiments have been conducted at SPring-8 Angstrom Compact free-electron LAser (SACLA) using the custom-made diffraction apparatus KOTOBUKI-1 and two multiport CCD detectors. In the experiments, ten thousands of single-shot diffraction patterns can be collected within several hours. Then, diffraction patterns with significant levels of intensity suitable for structural analysis must be found, direct-beam positions in diffraction patterns determined, diffraction patterns from the two CCD detectors merged, and phase-retrieval calculations for structural analyses performed. A software suite named SITENNO has been developed to semi-automatically apply the four-step processing to a huge number of diffraction data. Here, details of the algorithm used in the suite are described and the performance for approximately 9000 diffraction patterns collected from cuboid-shaped copper oxide particles reported. Using the SITENNO suite, it is possible to conduct experiments with data processing immediately after the data collection, and to characterize the size distribution and internal structures of the non-crystalline particles.

Data processing software suite SITENNO for coherent X-ray diffraction imaging using the X-ray free-electron laser SACLA

PubMed Central

Sekiguchi, Yuki; Oroguchi, Tomotaka; Takayama, Yuki; Nakasako, Masayoshi

2014-01-01

Coherent X-ray diffraction imaging is a promising technique for visualizing the structures of non-crystalline particles with dimensions of micrometers to sub-micrometers. Recently, X-ray free-electron laser sources have enabled efficient experiments in the ‘diffraction before destruction’ scheme. Diffraction experiments have been conducted at SPring-8 Angstrom Compact free-electron LAser (SACLA) using the custom-made diffraction apparatus KOTOBUKI-1 and two multiport CCD detectors. In the experiments, ten thousands of single-shot diffraction patterns can be collected within several hours. Then, diffraction patterns with significant levels of intensity suitable for structural analysis must be found, direct-beam positions in diffraction patterns determined, diffraction patterns from the two CCD detectors merged, and phase-retrieval calculations for structural analyses performed. A software suite named SITENNO has been developed to semi-automatically apply the four-step processing to a huge number of diffraction data. Here, details of the algorithm used in the suite are described and the performance for approximately 9000 diffraction patterns collected from cuboid-shaped copper oxide particles reported. Using the SITENNO suite, it is possible to conduct experiments with data processing immediately after the data collection, and to characterize the size distribution and internal structures of the non-crystalline particles. PMID:24763651

A compact electron gun for time-resolved electron diffraction

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

Robinson, Matthew S.; Lane, Paul D.; Wann, Derek A., E-mail: derek.wann@york.ac.uk

A novel compact time-resolved electron diffractometer has been built with the primary goal of studying the ultrafast molecular dynamics of photoexcited gas-phase molecules. Here, we discuss the design of the electron gun, which is triggered by a Ti:Sapphire laser, before detailing a series of calibration experiments relating to the electron-beam properties. As a further test of the apparatus, initial diffraction patterns have been collected for thin, polycrystalline platinum samples, which have been shown to match theoretical patterns. The data collected demonstrate the focusing effects of the magnetic lens on the electron beam, and how this relates to the spatial resolutionmore » of the diffraction pattern.« less

Electron diffraction using ultrafast electron bunches from a laser-wakefield accelerator at kHz repetition rate

NASA Astrophysics Data System (ADS)

He, Z.-H.; Thomas, A. G. R.; Beaurepaire, B.; Nees, J. A.; Hou, B.; Malka, V.; Krushelnick, K.; Faure, J.

2013-02-01

We show that electron bunches in the 50-100 keV range can be produced from a laser wakefield accelerator using 10 mJ, 35 fs laser pulses operating at 0.5 kHz. It is shown that using a solenoid magnetic lens, the electron bunch distribution can be shaped. The resulting transverse and longitudinal coherence is suitable for producing diffraction images from a polycrystalline 10 nm aluminum foil. The high repetition rate, the stability of the electron source, and the fact that its uncorrelated bunch duration is below 100 fs make this approach promising for the development of sub-100 fs ultrafast electron diffraction experiments.

10-fs-level synchronization of photocathode laser with RF-oscillator for ultrafast electron and X-ray sources

PubMed Central

Yang, Heewon; Han, Byungheon; Shin, Junho; Hou, Dong; Chung, Hayun; Baek, In Hyung; Jeong, Young Uk; Kim, Jungwon

2017-01-01

Ultrafast electron-based coherent radiation sources, such as free-electron lasers (FELs), ultrafast electron diffraction (UED) and Thomson-scattering sources, are becoming more important sources in today’s ultrafast science. Photocathode laser is an indispensable common subsystem in these sources that generates ultrafast electron pulses. To fully exploit the potentials of these sources, especially for pump-probe experiments, it is important to achieve high-precision synchronization between the photocathode laser and radio-frequency (RF) sources that manipulate electron pulses. So far, most of precision laser-RF synchronization has been achieved by using specially designed low-noise Er-fibre lasers at telecommunication wavelength. Here we show a modular method that achieves long-term (>1 day) stable 10-fs-level synchronization between a commercial 79.33-MHz Ti:sapphire laser oscillator and an S-band (2.856-GHz) RF oscillator. This is an important first step toward a photocathode laser-based femtosecond RF timing and synchronization system that is suitable for various small- to mid-scale ultrafast X-ray and electron sources. PMID:28067288

10-fs-level synchronization of photocathode laser with RF-oscillator for ultrafast electron and X-ray sources

NASA Astrophysics Data System (ADS)

Yang, Heewon; Han, Byungheon; Shin, Junho; Hou, Dong; Chung, Hayun; Baek, In Hyung; Jeong, Young Uk; Kim, Jungwon

2017-01-01

Ultrafast electron-based coherent radiation sources, such as free-electron lasers (FELs), ultrafast electron diffraction (UED) and Thomson-scattering sources, are becoming more important sources in today’s ultrafast science. Photocathode laser is an indispensable common subsystem in these sources that generates ultrafast electron pulses. To fully exploit the potentials of these sources, especially for pump-probe experiments, it is important to achieve high-precision synchronization between the photocathode laser and radio-frequency (RF) sources that manipulate electron pulses. So far, most of precision laser-RF synchronization has been achieved by using specially designed low-noise Er-fibre lasers at telecommunication wavelength. Here we show a modular method that achieves long-term (>1 day) stable 10-fs-level synchronization between a commercial 79.33-MHz Ti:sapphire laser oscillator and an S-band (2.856-GHz) RF oscillator. This is an important first step toward a photocathode laser-based femtosecond RF timing and synchronization system that is suitable for various small- to mid-scale ultrafast X-ray and electron sources.

10-fs-level synchronization of photocathode laser with RF-oscillator for ultrafast electron and X-ray sources.

PubMed

Yang, Heewon; Han, Byungheon; Shin, Junho; Hou, Dong; Chung, Hayun; Baek, In Hyung; Jeong, Young Uk; Kim, Jungwon

2017-01-09

Ultrafast electron-based coherent radiation sources, such as free-electron lasers (FELs), ultrafast electron diffraction (UED) and Thomson-scattering sources, are becoming more important sources in today's ultrafast science. Photocathode laser is an indispensable common subsystem in these sources that generates ultrafast electron pulses. To fully exploit the potentials of these sources, especially for pump-probe experiments, it is important to achieve high-precision synchronization between the photocathode laser and radio-frequency (RF) sources that manipulate electron pulses. So far, most of precision laser-RF synchronization has been achieved by using specially designed low-noise Er-fibre lasers at telecommunication wavelength. Here we show a modular method that achieves long-term (>1 day) stable 10-fs-level synchronization between a commercial 79.33-MHz Ti:sapphire laser oscillator and an S-band (2.856-GHz) RF oscillator. This is an important first step toward a photocathode laser-based femtosecond RF timing and synchronization system that is suitable for various small- to mid-scale ultrafast X-ray and electron sources.

Diffraction and microscopy with attosecond electron pulse trains

NASA Astrophysics Data System (ADS)

Morimoto, Yuya; Baum, Peter

2018-03-01

Attosecond spectroscopy1-7 can resolve electronic processes directly in time, but a movie-like space-time recording is impeded by the too long wavelength ( 100 times larger than atomic distances) or the source-sample entanglement in re-collision techniques8-11. Here we advance attosecond metrology to picometre wavelength and sub-atomic resolution by using free-space electrons instead of higher-harmonic photons1-7 or re-colliding wavepackets8-11. A beam of 70-keV electrons at 4.5-pm de Broglie wavelength is modulated by the electric field of laser cycles into a sequence of electron pulses with sub-optical-cycle duration. Time-resolved diffraction from crystalline silicon reveals a < 10-as delay of Bragg emission and demonstrates the possibility of analytic attosecond-ångström diffraction. Real-space electron microscopy visualizes with sub-light-cycle resolution how an optical wave propagates in space and time. This unification of attosecond science with electron microscopy and diffraction enables space-time imaging of light-driven processes in the entire range of sample morphologies that electron microscopy can access.

Ab initio structure determination of nanocrystals of organic pharmaceutical compounds by electron diffraction at room temperature using a Timepix quantum area direct electron detector

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

Genderen, E. van; Clabbers, M. T. B.; Center for Cellular Imaging and NanoAnalytics

A specialized quantum area detector for electron diffraction studies makes it possible to solve the structure of small organic compound nanocrystals in non-cryo conditions by direct methods. Until recently, structure determination by transmission electron microscopy of beam-sensitive three-dimensional nanocrystals required electron diffraction tomography data collection at liquid-nitrogen temperature, in order to reduce radiation damage. Here it is shown that the novel Timepix detector combines a high dynamic range with a very high signal-to-noise ratio and single-electron sensitivity, enabling ab initio phasing of beam-sensitive organic compounds. Low-dose electron diffraction data (∼0.013 e{sup −} Å{sup −2} s{sup −1}) were collected at roommore » temperature with the rotation method. It was ascertained that the data were of sufficient quality for structure solution using direct methods using software developed for X-ray crystallography (XDS, SHELX) and for electron crystallography (ADT3D/PETS, SIR2014)« less

Polyaniline (PANI) modified bentonite by plasma technique for U(VI) removal from aqueous solution

NASA Astrophysics Data System (ADS)

Liu, Xinghao; Cheng, Cheng; Xiao, Chengjian; Shao, Dadong; Xu, Zimu; Wang, Jiaquan; Hu, Shuheng; Li, Xiaolong; Wang, Weijuan

2017-07-01

Polyaniline (PANI) modified bentonite (PANI/bentonie) was synthesized by plasma induced polymerization of aniline on bentonite surface, and applied to uptake of uranium(VI) ions from aqueous solution. The as-synthesized PANI/bentonie was characterized by scanning electron microscopy (SEM), powder X-ray diffraction (XRD), thermal gravimetric analysis (TGA), and X-ray photoelectron spectroscopy (XPS). Batch adsorption technique was utilized to investigate the adsorption of U(VI) on bentonite and PANI/bentonite. The adsorption of U(VI) (10 mg/L) on PANI/bentonite surface is fairly depend on solution pH, ionic strength, and temperature in solution. The modified PANI on PANI/bentonite surface significantly enhances its adsorption capability for U(VI). The presence of humic acid (HA) can sound enhance U(VI) adsorption on PANI/bentonite at pH < 6.5 because of the strong complexation, and inhibits U(VI) adsorption at pH > 6.5. According to the thermodynamic parameters, the adsorption of U(VI) on PANI/bentonite surface is a spontaneous and endothermic process. The results highlight the application of PANI/bentonite composites as candidate material for the uptake of trace U(VI) from aqueous solution.

Two-dimensional mapping of polarizations of rhombohedral nanostructures in the orthorhombic phase of KNbO3 by the combined use of scanning transmission electron microscopy and convergent-beam electron diffraction

NASA Astrophysics Data System (ADS)

Tsuda, Kenji; Tanaka, Michiyoshi

2015-08-01

Rhombohedral nanostructures previously found in the orthorhombic phase of KNbO3, by convergent-beam electron diffraction [Tsuda et al., Appl. Phys. Lett. 102, 051913 (2013)], have been investigated by the combined use of scanning transmission electron microscopy and convergent-beam electron diffraction. Two-dimensional distributions of the rhombohedral nanostructures, or nanometer-scale spatial fluctuations of polarization clusters, have been successfully visualized. The correlation length of the observed spatial fluctuations of local polarizations is related to the cpc/apc ratio and the transition entropy.

Metallurgical characterization of melt-spun ribbons of U-5.4 wt%Nb alloy

NASA Astrophysics Data System (ADS)

Ma, Rong; Ren, Zhiyong; Tang, Qingfu; Chen, Dong; Liu, Tingyi; Su, Bin; Wang, Zhenhong; Luo, Chao

2018-06-01

The microstructures and micro-mechanical properties of the melt-spun ribbons of U-5.4 wt%Nb alloy were characterized using optical microscopy, scanning electron microscopy, X-ray diffraction and nanoindentation. Observed variations in microstructures and properties are related to the changes in ribbon thicknesses and cooling rates. The microstructures of the melt-spun ribbon consist of fine-scale columnar grains (∼1 μm) adjacent to the chill surface and coarse cellular grains in the remainder of the ribbon. In addition, the formation of inclusions in the ribbon is suppressed kinetically due to the high cooling rate during melt spinning. Compared with the water-quenched specimen prepared by traditional gravity casting and solution heat treatment, the elastic modulus values of the U-5.4 wt%Nb alloy were examined to vary with grain size and exhibited diverse energy dissipation capacities.

Study on structural recovery of graphite irradiated with swift heavy ions at high temperature

NASA Astrophysics Data System (ADS)

Pellemoine, F.; Avilov, M.; Bender, M.; Ewing, R. C.; Fernandes, S.; Lang, M.; Li, W. X.; Mittig, W.; Schein, M.; Severin, D.; Tomut, M.; Trautmann, C.; Zhang, F. X.

2015-12-01

Thin graphite foils bombarded with an intense high-energy (8.6 MeV/u) gold beam reaching fluences up to 1 × 1015 ions/cm2 lead to swelling and electrical resistivity changes. As shown earlier, these effects are diminished with increasing irradiation temperature. The work reported here extends the investigation of beam induced changes of these samples by structural analysis using synchrotron X-ray diffraction and transmission electron microscope. A nearly complete recovery from swelling at irradiation temperatures above about 1500 °C is identified.

Teaching Diffraction of Light and Electrons: Classroom Analogies to Classic Experiments

ERIC Educational Resources Information Center

Velentzas, Athanasios

2014-01-01

Diffraction and interference are phenomena that demonstrate the wave nature of light and of particles. Experiments relating to the diffraction/interference of light can easily be carried out in an educational lab, but it may be impossible to perform experiments involving electrons because of the lack of specialized equipment needed for such…

Exploring transmission Kikuchi diffraction using a Timepix detector

NASA Astrophysics Data System (ADS)

Vespucci, S.; Winkelmann, A.; Mingard, K.; Maneuski, D.; O'Shea, V.; Trager-Cowan, C.

2017-02-01

Electron backscatter diffraction (EBSD) is a well-established scanning electron microscope (SEM)-based technique [1]. It allows the non-destructive mapping of the crystal structure, texture, crystal phase and strain with a spatial resolution of tens of nanometers. Conventionally this is performed by placing an electron sensitive screen, typically consisting of a phosphor screen combined with a charge coupled device (CCD) camera, in front of a specimen, usually tilted 70° to the normal of the exciting electron beam. Recently, a number of authors have shown that a significant increase in spatial resolution is achievable when Kikuchi diffraction patterns are acquired in transmission geometry; that is when diffraction patterns are generated by electrons transmitted through an electron-transparent, usually thinned, specimen. The resolution of this technique, called transmission Kikuchi diffraction (TKD), has been demonstrated to be better than 10 nm [2,3]. We have recently demonstrated the advantages of a direct electron detector, Timepix [4,5], for the acquisition of standard EBSD patterns [5]. In this article we will discuss the advantages of Timepix to perform TKD and for acquiring spot diffraction patterns and more generally for acquiring scanning transmission electron microscopy micrographs in the SEM. Particularly relevant for TKD, is its very compact size, which allows much more flexibility in the positioning of the detector in the SEM chamber. We will furthermore show recent results using Timepix as a virtual forward scatter detector, and will illustrate the information derivable on producing images through processing of data acquired from different areas of the detector. We will show results from samples ranging from gold nanoparticles to nitride semiconductor nanorods.

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

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

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

2015-06-15

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

Atomic-scale diffractive imaging of sub-cycle electron dynamics in condensed matter

PubMed Central

Yakovlev, Vladislav S.; Stockman, Mark I.; Krausz, Ferenc; Baum, Peter

2015-01-01

For interaction of light with condensed-matter systems, we show with simulations that ultrafast electron and X-ray diffraction can provide a time-dependent record of charge-density maps with sub-cycle and atomic-scale resolutions. Using graphene as an example material, we predict that diffraction can reveal localised atomic-scale origins of optical and electronic phenomena. In particular, we point out nontrivial relations between microscopic electric current and density in undoped graphene. PMID:26412407

Atomic-scale diffractive imaging of sub-cycle electron dynamics in condensed matter

DOE PAGES

Yakovlev, Vladislav S.; Stockman, Mark I.; Krausz, Ferenc; ...

2015-09-28

For interaction of light with condensed-matter systems, we show with simulations that ultrafast electron and X-ray diffraction can provide a time-dependent record of charge-density maps with sub-cycle and atomic-scale resolutions. Using graphene as an example material, we predict that diffraction can reveal localised atomic-scale origins of optical and electronic phenomena. Here, we point out nontrivial relations between microscopic electric current and density in undoped graphene.

Low-kilovolt coherent electron diffractive imaging instrument based on a single-atom electron source

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

Lin, Chun-Yueh; Chang, Wei-Tse; Chen, Yi-Sheng

2016-03-15

In this work, a transmission-type, low-kilovolt coherent electron diffractive imaging instrument was constructed. It comprised a single-atom field emitter, a triple-element electrostatic lens, a sample holder, and a retractable delay line detector to record the diffraction patterns at different positions behind the sample. It was designed to image materials thinner than 3 nm. The authors analyzed the asymmetric triple-element electrostatic lens for focusing the electron beams and achieved a focused beam spot of 87 nm on the sample plane at the electron energy of 2 kV. High-angle coherent diffraction patterns of a suspended graphene sample corresponding to (0.62 Å){sup −1} were recorded. This workmore » demonstrated the potential of coherent diffractive imaging of thin two-dimensional materials, biological molecules, and nano-objects at a voltage between 1 and 10 kV. The ultimate goal of this instrument is to achieve atomic resolution of these materials with high contrast and little radiation damage.« less

Neutron diffraction study of the in situ oxidation of UO(2).

PubMed

Desgranges, Lionel; Baldinozzi, Gianguido; Rousseau, Gurvan; Nièpce, Jean-Claude; Calvarin, Gilbert

2009-08-17

This paper discusses uranium oxide crystal structure modifications that are observed during the low-temperature oxidation which transforms UO(2) into U(3)O(8). The symmetries and the structural parameters of UO(2), beta-U(4)O(9), beta-U(3)O(7), and U(3)O(8) were determined by refining neutron diffraction patterns on pure single-phase samples. Neutron diffraction patterns were also collected during the in situ oxidation of powder samples at 483 K. The lattice parameters and relative ratios of the four pure phases were measured during the progression of the isothermal oxidation. The transformation of UO(2) into U(3)O(8) involves a complex modification of the oxygen sublattice and the onset of complex superstructures for U(4)O(9) and U(3)O(7), associated with regular stacks of complex defects known as cuboctahedra, which consist of 13 oxygen atoms. The kinetics of the oxidation process are discussed on the basis of the results of the structural analysis.

Capturing Structural Dynamics in Crystalline Silicon Using Chirped Electrons from a Laser Wakefield Accelerator

PubMed Central

He, Z.-H.; Beaurepaire, B.; Nees, J. A.; Gallé, G.; Scott, S. A.; Pérez, J. R. Sánchez; Lagally, M. G.; Krushelnick, K.; Thomas, A. G. R.; Faure, J.

2016-01-01

Recent progress in laser wakefield acceleration has led to the emergence of a new generation of electron and X-ray sources that may have enormous benefits for ultrafast science. These novel sources promise to become indispensable tools for the investigation of structural dynamics on the femtosecond time scale, with spatial resolution on the atomic scale. Here, we demonstrate the use of laser-wakefield-accelerated electron bunches for time-resolved electron diffraction measurements of the structural dynamics of single-crystal silicon nano-membranes pumped by an ultrafast laser pulse. In our proof-of-concept study, we resolve the silicon lattice dynamics on a picosecond time scale by deflecting the momentum-time correlated electrons in the diffraction peaks with a static magnetic field to obtain the time-dependent diffraction efficiency. Further improvements may lead to femtosecond temporal resolution, with negligible pump-probe jitter being possible with future laser-wakefield-accelerator ultrafast-electron-diffraction schemes. PMID:27824086

Capturing Structural Dynamics in Crystalline Silicon Using Chirped Electrons from a Laser Wakefield Accelerator

DOE PAGES

He, Z. -H.; Beaurepaire, B.; Nees, J. A.; ...

2016-11-08

Recent progress in laser wakefield acceleration has led to the emergence of a new generation of electron and X-ray sources that may have enormous benefits for ultrafast science. These novel sources promise to become indispensable tools for the investigation of structural dynamics on the femtosecond time scale, with spatial resolution on the atomic scale. Here in this paper, we demonstrate the use of laser-wakefield-accelerated electron bunches for time-resolved electron diffraction measurements of the structural dynamics of single-crystal silicon nano-membranes pumped by an ultrafast laser pulse. In our proof-of-concept study, we resolve the silicon lattice dynamics on a picosecond time scalemore » by deflecting the momentum-time correlated electrons in the diffraction peaks with a static magnetic field to obtain the time-dependent diffraction efficiency. Further improvements may lead to femtosecond temporal resolution, with negligible pump-probe jitter being possible with future laser-wakefield-accelerator ultrafast-electron-diffraction schemes.« less

The significance of Bragg's law in electron diffraction and microscopy, and Bragg's second law.

PubMed

Humphreys, C J

2013-01-01

Bragg's second law, which deserves to be more widely known, is recounted. The significance of Bragg's law in electron diffraction and microscopy is then discussed, with particular emphasis on differences between X-ray and electron diffraction. As an example of such differences, the critical voltage effect in electron diffraction is described. It is then shown that the lattice imaging of crystals in high-resolution electron microscopy directly reveals the Bragg planes used for the imaging process, exactly as visualized by Bragg in his real-space law. Finally, it is shown how in 2012, for the first time, on the centennial anniversary of Bragg's law, single atoms have been identified in an electron microscope using X-rays emitted from the specimen. Hence atomic resolution X-ray maps of a crystal in real space can be formed which give the positions and identities of the different atoms in the crystal, or of a single impurity atom in the crystal.

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

PubMed

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

2018-06-06

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

Physical properties of monolithic U8 wt.%-Mo

NASA Astrophysics Data System (ADS)

Hengstler, R. M.; Beck, L.; Breitkreutz, H.; Jarousse, C.; Jungwirth, R.; Petry, W.; Schmid, W.; Schneider, J.; Wieschalla, N.

2010-07-01

As a possible high density fuel for research reactors, monolithic U8 wt.%-Mo ("U8Mo") was examined with regard to its structural, thermal and electric properties. X-ray diffraction by the Bragg-Brentano method was used to reveal the tetragonal lattice structure of rolled U8Mo. The specific heat capacity of cast U8Mo was determined by differential scanning calorimetry, its thermal diffusivity was measured by the laser flash method and its mass density by Archimedes' principle. From these results, the thermal conductivity of U8Mo in the temperature range from 40 °C to 250 °C was calculated; in the measured temperature range, it is in good accordance with literature data for UMo with 8 and 9 wt.% Mo, is higher than for 10 wt.% Mo and lower than for 5 wt.% Mo. The electric conductivity of rolled and cast U8Mo was measured by a four-wire method and the electron based part of the thermal conductivity calculated by the Wiedemann-Frantz law. Rolled and cast U8Mo was irradiated at about 150 °C with 80 MeV 127I ions to receive the same iodine ion density in the damage peak region as the fission product density in the fuel of a typical high flux reactor after the targeted nuclear burn-up. XRD analysis of irradiated U8Mo showed a change of the lattice parameters as well as the creation of UO 2 in the superficial sample regions; however, a phase change by irradiation was not observed. The determination of the electron based part of the thermal conductivity of the irradiated samples failed due to high measurement errors which are caused by the low thickness of the damage region in the ion irradiated samples.

Comments on the paper "Bragg's law diffraction simulations for electron backscatter diffraction analysis" by Josh Kacher, Colin Landon, Brent L. Adams & David Fullwood.

PubMed

Maurice, Claire; Fortunier, Roland; Driver, Julian; Day, Austin; Mingard, Ken; Meaden, Graham

2010-06-01

This comment on the paper "Bragg's Law diffraction simulations for electron backscatter diffraction analysis" by Kacher et al. explains the limitations in determining elastic strains using synthetic EBSD patterns. Of particular importance are those due to the accuracy of determination of the EBSD geometry projection parameters. Additional references and supporting information are provided. Copyright 2010 Elsevier B.V. All rights reserved.

Anomalous Diffraction in Crystallographic Phase Evaluation

PubMed Central

Hendrickson, Wayne A.

2014-01-01

X-ray diffraction patterns from crystals of biological macromolecules contain sufficient information to define atomic structures, but atomic positions are inextricable without having electron-density images. Diffraction measurements provide amplitudes, but the computation of electron density also requires phases for the diffracted waves. The resonance phenomenon known as anomalous scattering offers a powerful solution to this phase problem. Exploiting scattering resonances from diverse elements, the methods of multiwavelength anomalous diffraction (MAD) and single-wavelength anomalous diffraction (SAD) now predominate for de novo determinations of atomic-level biological structures. This review describes the physical underpinnings of anomalous diffraction methods, the evolution of these methods to their current maturity, the elements, procedures and instrumentation used for effective implementation, and the realm of applications. PMID:24726017

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.

Serial single molecule electron diffraction imaging: diffraction background of superfluid helium droplets

NASA Astrophysics Data System (ADS)

Zhang, Jie; He, Yunteng; Lei, Lei; Alghamdi, Maha; Oswalt, Andrew; Kong, Wei

2017-08-01

In an effort to solve the crystallization problem in crystallography, we have been engaged in developing a method termed "serial single molecule electron diffraction imaging" (SS-EDI). The unique features of SS-EDI are superfluid helium droplet cooling and field-induced orientation: together the two features constitute a molecular goniometer. Unfortunately, the helium atoms surrounding the sample molecule also contribute to a diffraction background. In this report, we analyze the properties of a superfluid helium droplet beam and its doping statistics, and demonstrate the feasibility of overcoming the background issue by using the velocity slip phenomenon of a pulsed droplet beam. Electron diffraction profiles and pair correlation functions of ferrocene-monomer-doped droplets and iodine-nanocluster-doped droplets are presented. The timing of the pulsed electron gun and the effective doping efficiency under different dopant pressures can both be controlled for size selection. This work clears any doubt of the effectiveness of superfluid helium droplets in SS-EDI, thereby advancing the effort in demonstrating the "proof-of-concept" one step further.

Molecular structures and intramolecular dynamics of pentahalides

NASA Astrophysics Data System (ADS)

Ischenko, A. A.

2017-03-01

This paper reviews advances of modern gas electron diffraction (GED) method combined with high-resolution spectroscopy and quantum chemical calculations in studies of the impact of intramolecular dynamics in free molecules of pentahalides. Some recently developed approaches to the electron diffraction data interpretation, based on direct incorporation of the adiabatic potential energy surface parameters to the diffraction intensity are described. In this way, complementary data of different experimental and computational methods can be directly combined for solving problems of the molecular structure and its dynamics. The possibility to evaluate some important parameters of the adiabatic potential energy surface - barriers to pseudorotation and saddle point of intermediate configuration from diffraction intensities in solving the inverse GED problem is demonstrated on several examples. With increasing accuracy of the electron diffraction intensities and the development of the theoretical background of electron scattering and data interpretation, it has become possible to investigate complex nuclear dynamics in fluxional systems by the GED method. Results of other research groups are also included in the discussion.

Tuning the physical properties in strontium iridate heterostructures

NASA Astrophysics Data System (ADS)

Nichols, John; Meyer, Tricia; Lee, Ho Nyung

2015-03-01

Strontium iridate (Srn+1IrnO3n+1) has received lots of attention recently for its potential to reveal novel physical phenomena due to strong spin-orbital coupling with an interaction energy comparable to that of the on-site Coulomb interaction and crystal field splitting. The coexistence of fundamental interactions has created an exotic Jeff = 1/2 antiferromagnetic insulating ground state in Sr2IrO4. In particular, it is known that this system can be driven into a metallic state with the simultaneous increase in dimensionality (n) and strain. We have investigated the effects of electron confinement by interfacing strontium iridates with other perovskite oxides. We have synthesized thin film heterostructures, SrIrO3/AMO3 (A = Sr, La; B = Ti, Mn, Rh), layer-by-layer with pulsed laser deposition equipped with reflection high-energy electron diffraction. Based on investigations with x-ray diffraction, dc transport, SQUID magnetometry, and various spectroscopic measurements, we will present that the physical properties of the heterostructures are strongly dependent on spatial confinement and epitaxial strain. *This work was supported by the U. S. Department of Energy, Office of Science, Basic Energy Sciences, Materials Science and Engineering Division.

Behavior of magnesium at high pressures and high temperatures

NASA Astrophysics Data System (ADS)

Cynn, H.; Evans, W.; Yoo, C. S.; Ohishi, Y.; Sata, N.; Shimomura, O.

2004-03-01

Structural stability relationship manifested by 3-, 4-, 5d-electron transition metals also appears in so-called nearly free electron metal, magnesium as exampled by HCP to BCC structure change at high pressures. This transition has been examined by theory and confirmed by experiment. Recently, HCP to DHCP crystal structure change has been reported at high temperatures below 20 GPa. However, this type of structure change is rather common in 4f-electron lanthanides. In this study, we used synchrotron x-ray diffraction to find out the relationship between BCC and DHCP employing a diamond anvil cell technique coupled with external and laser heating methods. We also examined pressure gradient effects in relation with the existence of DHCP. This work has been supported by PDRP program at the Lawrence Livermore National Laboratory, University of California under the auspices of the U.S. Department of Energy under Contract No. W-7405-ENG-48

Device and method for creating Gaussian aberration-corrected electron beams

DOEpatents

McMorran, Benjamin; Linck, Martin

2016-01-19

Electron beam phase gratings have phase profiles that produce a diffracted beam having a Gaussian or other selected intensity profile. Phase profiles can also be selected to correct or compensate electron lens aberrations. Typically, a low diffraction order produces a suitable phase profile, and other orders are discarded.

Breaking resolution limits in ultrafast electron diffraction and microscopy.

PubMed

Baum, Peter; Zewail, Ahmed H

2006-10-31

Ultrafast electron microscopy and diffraction are powerful techniques for the study of the time-resolved structures of molecules, materials, and biological systems. Central to these approaches is the use of ultrafast coherent electron packets. The electron pulses typically have an energy of 30 keV for diffraction and 100-200 keV for microscopy, corresponding to speeds of 33-70% of the speed of light. Although the spatial resolution can reach the atomic scale, the temporal resolution is limited by the pulse width and by the difference in group velocities of electrons and the light used to initiate the dynamical change. In this contribution, we introduce the concept of tilted optical pulses into diffraction and imaging techniques and demonstrate the methodology experimentally. These advances allow us to reach limits of time resolution down to regimes of a few femtoseconds and, possibly, attoseconds. With tilted pulses, every part of the sample is excited at precisely the same time as when the electrons arrive at the specimen. Here, this approach is demonstrated for the most unfavorable case of ultrafast crystallography. We also present a method for measuring the duration of electron packets by autocorrelating electron pulses in free space and without streaking, and we discuss the potential of tilting the electron pulses themselves for applications in domains involving nuclear and electron motions.

Preparation of atomically flat TiO2(001) surfaces

NASA Astrophysics Data System (ADS)

Wang, Yang; Weitering, Hanno H.; Snijders, Paul C.

2015-03-01

Transition metal oxides with the rutile structure (MO2, M = e.g. Ti, V, or Nb) have highly directional partially occupied t2g orbitals. Some of these orbitals form quasi-1D electronic bands along the rutile c-axis, and Peierls-like ordering phenomena have been observed in VO2 and NbO2. Tailoring the electronic properties of these materials via quantum confinement requires epitaxial growth on suitable substrates such as low index TiO2 surfaces. Because of the high surface energy of rutile TiO2(001), the standard approach of sputtering and annealing usually introduces faceting. Here we demonstrate a facile method to create atomically flat, non-faceted TiO2(001) surfaces. Using scanning tunneling microscopy we observe terraces with a width of approximately 150 nm. Step heights of approximately 0.3 nm are observed, consistent with the c lattice parameter of rutile TiO2. Low energy electron diffraction patterns reveal sharp diffraction spots with an in-plane lattice constant of 0.358 nm which is consistent with a (1x1) ordering of the (001) plane. These TiO2(001) single crystal surfaces can serve as an ideal substrate for further growth of rutile heterostructures. Research sponsored by the U.S. Department of Energy, Office of Science, Basic Energy Sciences, Materials Sciences and Engineering Division.

Enhancement of diffraction efficiency and storage life of poly(vinyl chloride)-based optical recording medium with incorporation of an electron donor

NASA Astrophysics Data System (ADS)

John, Beena Mary; Ushamani, M.; Sreekumar, K.; Joseph, Rani; Sudha Kartha, C.

2007-01-01

The diffraction efficiency, sensitivity, and storage life of methylene blue-sensitized poly(vinyl chloride) film was improved by the addition of an electron donor in the matrix. The addition of pyridine enhanced the diffraction efficiency by two times, and storage life of the gratings was increased to 2-3 days.

Ab initio structure determination of nanocrystals of organic pharmaceutical compounds by electron diffraction at room temperature using a Timepix quantum area direct electron detector.

PubMed

van Genderen, E; Clabbers, M T B; Das, P P; Stewart, A; Nederlof, I; Barentsen, K C; Portillo, Q; Pannu, N S; Nicolopoulos, S; Gruene, T; Abrahams, J P

2016-03-01

Until recently, structure determination by transmission electron microscopy of beam-sensitive three-dimensional nanocrystals required electron diffraction tomography data collection at liquid-nitrogen temperature, in order to reduce radiation damage. Here it is shown that the novel Timepix detector combines a high dynamic range with a very high signal-to-noise ratio and single-electron sensitivity, enabling ab initio phasing of beam-sensitive organic compounds. Low-dose electron diffraction data (∼ 0.013 e(-) Å(-2) s(-1)) were collected at room temperature with the rotation method. It was ascertained that the data were of sufficient quality for structure solution using direct methods using software developed for X-ray crystallography (XDS, SHELX) and for electron crystallography (ADT3D/PETS, SIR2014).

Single-shot coherent diffraction imaging of microbunched relativistic electron beams for free-electron laser applications.

PubMed

Marinelli, A; Dunning, M; Weathersby, S; Hemsing, E; Xiang, D; Andonian, G; O'Shea, F; Miao, Jianwei; Hast, C; Rosenzweig, J B

2013-03-01

With the advent of coherent x rays provided by the x-ray free-electron laser (FEL), strong interest has been kindled in sophisticated diffraction imaging techniques. In this Letter, we exploit such techniques for the diagnosis of the density distribution of the intense electron beams typically utilized in an x-ray FEL itself. We have implemented this method by analyzing the far-field coherent transition radiation emitted by an inverse-FEL microbunched electron beam. This analysis utilizes an oversampling phase retrieval method on the transition radiation angular spectrum to reconstruct the transverse spatial distribution of the electron beam. This application of diffraction imaging represents a significant advance in electron beam physics, having critical applications to the diagnosis of high-brightness beams, as well as the collective microbunching instabilities afflicting these systems.

Solving the jitter problem in microwave compressed ultrafast electron diffraction instruments: Robust sub-50 fs cavity-laser phase stabilization

PubMed Central

Otto, M. R.; René de Cotret, L. P.; Stern, M. J.; Siwick, B. J.

2017-01-01

We demonstrate the compression of electron pulses in a high-brightness ultrafast electron diffraction instrument using phase-locked microwave signals directly generated from a mode-locked femtosecond oscillator. Additionally, a continuous-wave phase stabilization system that accurately corrects for phase fluctuations arising in the compression cavity from both power amplification and thermal drift induced detuning was designed and implemented. An improvement in the microwave timing stability from 100 fs to 5 fs RMS is measured electronically, and the long-term arrival time stability (>10 h) of the electron pulses improves to below our measurement resolution of 50 fs. These results demonstrate sub-relativistic ultrafast electron diffraction with compressed pulses that is no longer limited by laser-microwave synchronization. PMID:28852686

Quantum diffraction and shielding effects on the low-energy electron-ion bremsstrahlung in two-component semiclassical plasmas

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

Lee, Myoung-Jae; Jung, Young-Dae, E-mail: ydjung@hanyang.ac.kr; Department of Physics, Applied Physics, and Astronomy, Rensselaer Polytechnic Institute, 110 8th Street, Troy, New York 12180-3590

2015-10-15

The quantum diffraction and shielding effects on the low-energy bremsstrahlung process are investigated in two-component semiclassical plasmas. The impact-parameter analysis with the micropotential taking into account the quantum diffraction and shielding effects is employed to obtain the electron-ion bremsstrahlung radiation cross section as a function of the de Broglie wavelength, density parameter, impact parameter, photon energy, and projectile energy. The result shows that the influence of quantum diffraction and shielding strongly suppresses the bremsstrahlung radiation spectrum in semiclassical plasmas. It is found that the quantum diffraction and shielding effects have broaden the photon emission domain. It is also found thatmore » the photon emission domain is almost independent of the radiation photon energy. In addition, it is found that the influence of quantum diffraction and shielding on the bremsstrahlung spectrum decreases with an increase of the projectile energy. The density effect on the electron-ion bremsstrahlung cross section is also discussed.« less

Holographic Reconstruction of Photoelectron Diffraction and Its Circular Dichroism for Local Structure Probing

NASA Astrophysics Data System (ADS)

Matsui, Fumihiko; Matsushita, Tomohiro; Daimon, Hiroshi

2018-06-01

The local atomic structure around a specific element atom can be recorded as a photoelectron diffraction pattern. Forward focusing peaks and diffraction rings around them indicate the directions and distances from the photoelectron emitting atom to the surrounding atoms. The state-of-the-art holography reconstruction algorithm enables us to image the local atomic arrangement around the excited atom in a real space. By using circularly polarized light as an excitation source, the angular momentum transfer from the light to the photoelectron induces parallax shifts in these diffraction patterns. As a result, stereographic images of atomic arrangements are obtained. These diffraction patterns can be used as atomic-site-resolved probes for local electronic structure investigation in combination with spectroscopy techniques. Direct three-dimensional atomic structure visualization and site-specific electronic property analysis methods are reviewed. Furthermore, circular dichroism was also found in valence photoelectron and Auger electron diffraction patterns. The investigation of these new phenomena provides hints for the development of new techniques for local structure probing.

Radiation damage free ghost diffraction with atomic resolution

DOE PAGES

Li, Zheng; Medvedev, Nikita; Chapman, Henry N.; ...

2017-12-21

The x-ray free electron lasers can enable diffractive structural determination of protein nanocrystals and single molecules that are too small and radiation-sensitive for conventional x-ray diffraction. However the electronic form factor may be modified during the ultrashort x-ray pulse due to photoionization and electron cascade caused by the intense x-ray pulse. For general x-ray imaging techniques, the minimization of the effects of radiation damage is of major concern to ensure reliable reconstruction of molecular structure. Here in this paper, we show that radiation damage free diffraction can be achieved with atomic spatial resolution by using x-ray parametric down-conversion and ghostmore » diffraction with entangled photons of x-ray and optical frequencies. We show that the formation of the diffraction patterns satisfies a condition analogous to the Bragg equation, with a resolution that can be as fine as the crystal lattice length scale of several Ångstrom. Since the samples are illuminated by low energy optical photons, they can be free of radiation damage.« less

Radiation damage free ghost diffraction with atomic resolution

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

Li, Zheng; Medvedev, Nikita; Chapman, Henry N.

The x-ray free electron lasers can enable diffractive structural determination of protein nanocrystals and single molecules that are too small and radiation-sensitive for conventional x-ray diffraction. However the electronic form factor may be modified during the ultrashort x-ray pulse due to photoionization and electron cascade caused by the intense x-ray pulse. For general x-ray imaging techniques, the minimization of the effects of radiation damage is of major concern to ensure reliable reconstruction of molecular structure. Here in this paper, we show that radiation damage free diffraction can be achieved with atomic spatial resolution by using x-ray parametric down-conversion and ghostmore » diffraction with entangled photons of x-ray and optical frequencies. We show that the formation of the diffraction patterns satisfies a condition analogous to the Bragg equation, with a resolution that can be as fine as the crystal lattice length scale of several Ångstrom. Since the samples are illuminated by low energy optical photons, they can be free of radiation damage.« less

The use of analytical surface tools in the fundamental study of wear. [atomic nature of wear

NASA Technical Reports Server (NTRS)

Buckley, D. H.

1977-01-01

Various techniques and surface tools available for the study of the atomic nature of the wear of materials are reviewed These include chemical etching, x-ray diffraction, electron diffraction, scanning electron microscopy, low-energy electron diffraction, Auger emission spectroscopy analysis, electron spectroscopy for chemical analysis, field ion microscopy, and the atom probe. Properties of the surface and wear surface regions which affect wear, such as surface energy, crystal structure, crystallographic orientation, mode of dislocation behavior, and cohesive binding, are discussed. A number of mechanisms involved in the generation of wear particles are identified with the aid of the aforementioned tools.

Local nanoscale strain mapping of a metallic glass during in situ testing

NASA Astrophysics Data System (ADS)

Gammer, Christoph; Ophus, Colin; Pekin, Thomas C.; Eckert, Jürgen; Minor, Andrew M.

2018-04-01

The local elastic strains during tensile deformation in a CuZrAlAg metallic glass are obtained by fitting an elliptic shape function to the characteristic amorphous ring in electron diffraction patterns. Scanning nanobeam electron diffraction enables strain mapping with a resolution of a few nanometers. Here, a fast direct electron detector is used to acquire the diffraction patterns at a sufficient speed to map the local transient strain during continuous tensile loading in situ in the transmission electron microscope. The elastic strain in tensile direction was found to increase during loading. After catastrophic fracture, a residual elastic strain that relaxes over time was observed.

Low-energy transmission electron diffraction and imaging of large-area graphene

PubMed Central

Zhao, Wei; Xia, Bingyu; Lin, Li; Xiao, Xiaoyang; Liu, Peng; Lin, Xiaoyang; Peng, Hailin; Zhu, Yuanmin; Yu, Rong; Lei, Peng; Wang, Jiangtao; Zhang, Lina; Xu, Yong; Zhao, Mingwen; Peng, Lianmao; Li, Qunqing; Duan, Wenhui; Liu, Zhongfan; Fan, Shoushan; Jiang, Kaili

2017-01-01

Two-dimensional (2D) materials have attracted interest because of their excellent properties and potential applications. A key step in realizing industrial applications is to synthesize wafer-scale single-crystal samples. Until now, single-crystal samples, such as graphene domains up to the centimeter scale, have been synthesized. However, a new challenge is to efficiently characterize large-area samples. Currently, the crystalline characterization of these samples still relies on selected-area electron diffraction (SAED) or low-energy electron diffraction (LEED), which is more suitable for characterizing very small local regions. This paper presents a highly efficient characterization technique that adopts a low-energy electrostatically focused electron gun and a super-aligned carbon nanotube (SACNT) film sample support. It allows rapid crystalline characterization of large-area graphene through a single photograph of a transmission-diffracted image at a large beam size. Additionally, the low-energy electron beam enables the observation of a unique diffraction pattern of adsorbates on the suspended graphene at room temperature. This work presents a simple and convenient method for characterizing the macroscopic structures of 2D materials, and the instrument we constructed allows the study of the weak interaction with 2D materials. PMID:28879233

Low-energy transmission electron diffraction and imaging of large-area graphene.

PubMed

Zhao, Wei; Xia, Bingyu; Lin, Li; Xiao, Xiaoyang; Liu, Peng; Lin, Xiaoyang; Peng, Hailin; Zhu, Yuanmin; Yu, Rong; Lei, Peng; Wang, Jiangtao; Zhang, Lina; Xu, Yong; Zhao, Mingwen; Peng, Lianmao; Li, Qunqing; Duan, Wenhui; Liu, Zhongfan; Fan, Shoushan; Jiang, Kaili

2017-09-01

Two-dimensional (2D) materials have attracted interest because of their excellent properties and potential applications. A key step in realizing industrial applications is to synthesize wafer-scale single-crystal samples. Until now, single-crystal samples, such as graphene domains up to the centimeter scale, have been synthesized. However, a new challenge is to efficiently characterize large-area samples. Currently, the crystalline characterization of these samples still relies on selected-area electron diffraction (SAED) or low-energy electron diffraction (LEED), which is more suitable for characterizing very small local regions. This paper presents a highly efficient characterization technique that adopts a low-energy electrostatically focused electron gun and a super-aligned carbon nanotube (SACNT) film sample support. It allows rapid crystalline characterization of large-area graphene through a single photograph of a transmission-diffracted image at a large beam size. Additionally, the low-energy electron beam enables the observation of a unique diffraction pattern of adsorbates on the suspended graphene at room temperature. This work presents a simple and convenient method for characterizing the macroscopic structures of 2D materials, and the instrument we constructed allows the study of the weak interaction with 2D materials.

Protein structure determination by electron diffraction using a single three-dimensional nanocrystal.

PubMed

Clabbers, M T B; van Genderen, E; Wan, W; Wiegers, E L; Gruene, T; Abrahams, J P

2017-09-01

Three-dimensional nanometre-sized crystals of macromolecules currently resist structure elucidation by single-crystal X-ray crystallography. Here, a single nanocrystal with a diffracting volume of only 0.14 µm 3 , i.e. no more than 6 × 10 5 unit cells, provided sufficient information to determine the structure of a rare dimeric polymorph of hen egg-white lysozyme by electron crystallography. This is at least an order of magnitude smaller than was previously possible. The molecular-replacement solution, based on a monomeric polyalanine model, provided sufficient phasing power to show side-chain density, and automated model building was used to reconstruct the side chains. Diffraction data were acquired using the rotation method with parallel beam diffraction on a Titan Krios transmission electron microscope equipped with a novel in-house-designed 1024 × 1024 pixel Timepix hybrid pixel detector for low-dose diffraction data collection. Favourable detector characteristics include the ability to accurately discriminate single high-energy electrons from X-rays and count them, fast readout to finely sample reciprocal space and a high dynamic range. This work, together with other recent milestones, suggests that electron crystallography can provide an attractive alternative in determining biological structures.

Protein structure determination by electron diffraction using a single three-dimensional nanocrystal

PubMed Central

Clabbers, M. T. B.; van Genderen, E.; Wiegers, E. L.; Gruene, T.; Abrahams, J. P.

2017-01-01

Three-dimensional nanometre-sized crystals of macromolecules currently resist structure elucidation by single-crystal X-ray crystallography. Here, a single nanocrystal with a diffracting volume of only 0.14 µm3, i.e. no more than 6 × 105 unit cells, provided sufficient information to determine the structure of a rare dimeric polymorph of hen egg-white lysozyme by electron crystallography. This is at least an order of magnitude smaller than was previously possible. The molecular-replacement solution, based on a monomeric polyalanine model, provided sufficient phasing power to show side-chain density, and automated model building was used to reconstruct the side chains. Diffraction data were acquired using the rotation method with parallel beam diffraction on a Titan Krios transmission electron microscope equipped with a novel in-house-designed 1024 × 1024 pixel Timepix hybrid pixel detector for low-dose diffraction data collection. Favourable detector characteristics include the ability to accurately discriminate single high-energy electrons from X-rays and count them, fast readout to finely sample reciprocal space and a high dynamic range. This work, together with other recent milestones, suggests that electron crystallography can provide an attractive alternative in determining biological structures. PMID:28876237

The Application of Vector Diffraction to the Scalar Anomalous Diffraction Approximation of van de Hulst.

DTIC Science & Technology

1987-05-01

plvdl ’ , systems, Applied Optics, 16( 12), 1181 - iAQ. Champion, 7. ’., G . H . Meeten and ". enir, ’ " . , ’ particles in the colloidal state, ourna: ,f...he her, 4a London, Faraday Transactions * - Champion, J. V. , G . H . Meeten , 1. 4. U 0 1n and -arp. Optical extinction of randomly ,oriented in, T...distance into the (poly) dispersion. We can find T -from f du fdy fda G (u,y,$) Qi(u,y,S) n(u) g (y) h (B) (15) where u is some parameter specifying

Single-electron pulses for ultrafast diffraction

PubMed Central

Aidelsburger, M.; Kirchner, F. O.; Krausz, F.; Baum, P.

2010-01-01

Visualization of atomic-scale structural motion by ultrafast electron diffraction and microscopy requires electron packets of shortest duration and highest coherence. We report on the generation and application of single-electron pulses for this purpose. Photoelectric emission from metal surfaces is studied with tunable ultraviolet pulses in the femtosecond regime. The bandwidth, efficiency, coherence, and electron pulse duration are investigated in dependence on excitation wavelength, intensity, and laser bandwidth. At photon energies close to the cathode’s work function, the electron pulse duration shortens significantly and approaches a threshold that is determined by interplay of the optical pulse width and the acceleration field. An optimized choice of laser wavelength and bandwidth results in sub-100-fs electron pulses. We demonstrate single-electron diffraction from polycrystalline diamond films and reveal the favorable influences of matched photon energies on the coherence volume of single-electron wave packets. We discuss the consequences of our findings for the physics of the photoelectric effect and for applications of single-electron pulses in ultrafast 4D imaging of structural dynamics. PMID:21041681

Uranium mobility and accumulation along the Rio Paguate, Jackpile Mine in Laguna Pueblo, NM.

PubMed

Blake, Johanna M; De Vore, Cherie L; Avasarala, Sumant; Ali, Abdul-Mehdi; Roldan, Claudia; Bowers, Fenton; Spilde, Michael N; Artyushkova, Kateryna; Kirk, Matthew F; Peterson, Eric; Rodriguez-Freire, Lucia; Cerrato, José M

2017-04-19

The mobility and accumulation of uranium (U) along the Rio Paguate, adjacent to the Jackpile Mine, in Laguna Pueblo, New Mexico was investigated using aqueous chemistry, electron microprobe, X-ray diffraction and spectroscopy analyses. Given that it is not common to identify elevated concentrations of U in surface water sources, the Rio Paguate is a unique site that concerns the Laguna Pueblo community. This study aims to better understand the solid chemistry of abandoned mine waste sediments from the Jackpile Mine and identify key hydrogeological and geochemical processes that affect the fate of U along the Rio Paguate. Solid analyses using X-ray fluorescence determined that sediments located in the Jackpile Mine contain ranges of 320 to 9200 mg kg -1 U. The presence of coffinite, a U(iv)-bearing mineral, was identified by X-ray diffraction analyses in abandoned mine waste solids exposed to several decades of weathering and oxidation. The dissolution of these U-bearing minerals from abandoned mine wastes could contribute to U mobility during rain events. The U concentration in surface waters sampled closest to mine wastes are highest during the southwestern monsoon season. Samples collected from September 2014 to August 2016 showed higher U concentrations in surface water adjacent to the Jackpile Mine (35.3 to 772 μg L -1 ) compared with those at a wetland 4.5 kilometers downstream of the mine (5.77 to 110 μg L -1 ). Sediments co-located in the stream bed and bank along the reach between the mine and wetland had low U concentrations (range 1-5 mg kg -1 ) compared to concentrations in wetland sediments with higher organic matter (14-15%) and U concentrations (2-21 mg kg -1 ). Approximately 10% of the total U in wetland sediments was amenable to complexation with 1 mM sodium bicarbonate in batch experiments; a decrease of U concentration in solution was observed over time in these experiments likely due to re-association with sediments in the reactor. The findings from this study provide new insights about how hydrologic events may affect the reactivity of U present in mine waste solids exposed to surface oxidizing conditions, and the influence of organic-rich sediments on U accumulation in the Rio Paguate.

Comparing results of X-ray diffraction, µ-Raman spectroscopy and neutron diffraction when identifying chemical phases in seized nuclear material, during a comparative nuclear forensics exercise.

PubMed

Rondahl, Stina Holmgren; Pointurier, Fabien; Ahlinder, Linnea; Ramebäck, Henrik; Marie, Olivier; Ravat, Brice; Delaunay, François; Young, Emma; Blagojevic, Ned; Hester, James R; Thorogood, Gordon; Nelwamondo, Aubrey N; Ntsoane, Tshepo P; Roberts, Sarah K; Holliday, Kiel S

2018-01-01

This work presents the results for identification of chemical phases obtained by several laboratories as a part of an international nuclear forensic round-robin exercise. In this work powder X-ray diffraction (p-XRD) is regarded as the reference technique. Neutron diffraction produced a superior high-angle diffraction pattern relative to p-XRD. Requiring only small amounts of sample, µ-Raman spectroscopy was used for the first time in this context as a potentially complementary technique to p-XRD. The chemical phases were identified as pure UO 2 in two materials, and as a mixture of UO 2 , U 3 O 8 and an intermediate species U 3 O 7 in the third material.

Publications - GMC 58 | Alaska Division of Geological & Geophysical Surveys

Science.gov Websites

DGGS GMC 58 Publication Details Title: X-ray diffraction and scanning electron microscopy mineral , Michael, and Core Laboratories, 1985, X-ray diffraction and scanning electron microscopy mineral analyses

Non-spectroscopic composition measurements of SrTiO 3-La 0.7Sr 0.3MnO 3 multilayers using scanning convergent beam electron diffraction

DOE PAGES

Ophus, Colin; Ercius, Peter; Huijben, Mark; ...

2017-02-08

The local atomic structure of a crystalline sample aligned along a zone axis can be probed with a focused electron probe, which produces a convergent beam electron diffraction pattern. The introduction of high speed direct electron detectors has allowed for experiments that can record a full diffraction pattern image at thousands of probe positions on a sample. By incoherently summing these patterns over crystalline unit cells, we demonstrate in this paper that in addition to crystal structure and thickness, we can also estimate the local composition of a perovskite superlattice sample. This is achieved by matching the summed patterns tomore » a library of simulated diffraction patterns. Finally, this technique allows for atomic-scale chemical measurements without requiring a spectrometer or hardware aberration correction.« less

Ab initio structure determination of nanocrystals of organic pharmaceutical compounds by electron diffraction at room temperature using a Timepix quantum area direct electron detector

PubMed Central

van Genderen, E.; Clabbers, M. T. B.; Das, P. P.; Stewart, A.; Nederlof, I.; Barentsen, K. C.; Portillo, Q.; Pannu, N. S.; Nicolopoulos, S.; Gruene, T.; Abrahams, J. P.

2016-01-01

Until recently, structure determination by transmission electron microscopy of beam-sensitive three-dimensional nanocrystals required electron diffraction tomography data collection at liquid-nitrogen temperature, in order to reduce radiation damage. Here it is shown that the novel Timepix detector combines a high dynamic range with a very high signal-to-noise ratio and single-electron sensitivity, enabling ab initio phasing of beam-sensitive organic compounds. Low-dose electron diffraction data (∼0.013 e− Å−2 s−1) were collected at room temperature with the rotation method. It was ascertained that the data were of sufficient quality for structure solution using direct methods using software developed for X-ray crystallography (XDS, SHELX) and for electron crystallography (ADT3D/PETS, SIR2014). PMID:26919375

Application of Brazilian kaolinite clay as adsorbent to removal of U(VI) from aqueous solution: Kinetic and thermodynamic of cation-basic interactions

NASA Astrophysics Data System (ADS)

Guerra, Denis L.; Leidens, Victor L.; Viana, Rúbia R.; Airoldi, Claudio

2010-05-01

The compound N 1-[3-(trimethoxysilyl)propyl]diethylenetriamine was anchored onto Amazon kaolinite surface by heterogeneous route. The modified and natural kaolinite samples were characterized by transmission electron microscopy, scanning electron microscopic, X-ray diffraction, and nuclear magnetic nuclei of 29Si and 13C. The well-defined peaks obtained in the 13C NMR spectrum in the 5.0-62.1 ppm region confirmed the attachment of organic functional groups as pendant chains bonded into the porous clay. The ability of these materials to remove U(VI) from aqueous solution was followed by a series of adsorption isotherms adjusted to a Sips equation at room temperature and pH 4.0. The kinetic parameters analyzed by the Lagergren and Elovich models gave a good fit for a pseudo-second order reaction with k2 values 16.0 and 25.1 mmol g -1 min -1 ranges for natural and modified kaolinite clays, respectively. The energetic effects caused by metal ion adsorption were determined through calorimetric titrations.

Structure resolution by electron diffraction tomography of the complex layered iron-rich Fe-2234-type Sr{sub 5}Fe{sub 6}O{sub 15.4}

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

Lepoittevin, Christophe, E-mail: christophe.lepoittevin@neel.cnrs.fr

2016-10-15

The crystal structure of the strontium ferrite Sr{sub 5}Fe{sub 6}O{sub 15.4}, was solved by direct methods on electron diffraction tomography data acquired on a transmission electron microscope. The refined cell parameters are a=27.4047(3) Å, b=5.48590(7) Å and c=42.7442(4) Å in Fm2m symmetry. Its structure is built up from the intergrowth sequence between a quadruple perovskite-type layer with a complex rock-salt (RS)-type block. In the latter iron atoms are found in two different environments : tetragonal pyramid and tetrahedron. The structural model was refined by Rietveld method based on the powder X-ray diffraction pattern. - Highlights: • Complex structure of Sr{submore » 5}Fe{sub 6}O{sub 15.4} solved by electron diffraction tomography. • Observed Fourier maps allow determining missing oxygen atoms in the structure. • Structural model refined from powder X-ray diffraction data. • Intergrowth between quadruple perovskite layer with double rock-salt-type layer.« less

Breaking resolution limits in ultrafast electron diffraction and microscopy

PubMed Central

Baum, Peter; Zewail, Ahmed H.

2006-01-01

Ultrafast electron microscopy and diffraction are powerful techniques for the study of the time-resolved structures of molecules, materials, and biological systems. Central to these approaches is the use of ultrafast coherent electron packets. The electron pulses typically have an energy of 30 keV for diffraction and 100–200 keV for microscopy, corresponding to speeds of 33–70% of the speed of light. Although the spatial resolution can reach the atomic scale, the temporal resolution is limited by the pulse width and by the difference in group velocities of electrons and the light used to initiate the dynamical change. In this contribution, we introduce the concept of tilted optical pulses into diffraction and imaging techniques and demonstrate the methodology experimentally. These advances allow us to reach limits of time resolution down to regimes of a few femtoseconds and, possibly, attoseconds. With tilted pulses, every part of the sample is excited at precisely the same time as when the electrons arrive at the specimen. Here, this approach is demonstrated for the most unfavorable case of ultrafast crystallography. We also present a method for measuring the duration of electron packets by autocorrelating electron pulses in free space and without streaking, and we discuss the potential of tilting the electron pulses themselves for applications in domains involving nuclear and electron motions. PMID:17056711

Magnetic ground state and electronic structure of CeRu(2)Al(10).

PubMed

Goraus, Jerzy; Ślebarski, Andrzej

2012-03-07

We present a combined theoretical and experimental study of the electronic structure for CeRu(2)Al(10) based on ab initio band structure calculations and x-ray photoemission spectroscopy (XPS) data. Our calculations were performed for the base unit cell and for the hypothetical unit cell which enables antiferromagnetic ordering. The stability of the magnetic phase was investigated within fixed spin moment calculations. When additional 4f correlations are not included in the LSDA C U approach, CeRu(2)Al(10) exhibits an unstable magnetic configuration with the difference in total energy per unit cell between the weakly magnetic state and the non-magnetic one of the order ~0.3 meV. We found that Coulomb correlations among 4f electrons, when they are included in the LSDA C U approach, stabilize the magnetic structure. In the weakly correlated system (small U) an antiferromagnetic (AFM) ground state with the lowest total energy is preferred. The situation is, however, the opposite when the 4f correlations are strong. In this case the ferromagnetic (FM) ground state is preferred. By comparing our calculations with the experimental data we conclude that the 4f correlations in CeRu(2)Al(10) are weak. We also carried out a structural relaxation of atomic positions within the Cmcm unit cell and we found that the Al atoms exhibit noticeable displacement from their positions known from x-ray diffraction (XRD) analysis.

Disentangling atomic-layer-specific x-ray absorption spectra by Auger electron diffraction spectroscopy

NASA Astrophysics Data System (ADS)

Matsui, Fumihiko; Matsushita, Tomohiro; Kato, Yukako; Hashimoto, Mie; Daimon, Hiroshi

2009-11-01

In order to investigate the electronic and magnetic structures of each atomic layer at subsurface, we have proposed a new method, Auger electron diffraction spectroscopy, which is the combination of x-ray absorption spectroscopy (XAS) and Auger electron diffraction (AED) techniques. We have measured a series of Ni LMM AED patterns of the Ni film grown on Cu(001) surface for various thicknesses. Then we deduced a set of atomic-layer-specific AED patterns in a numerical way. Furthermore, we developed an algorithm to disentangle XANES spectra from different atomic layers using these atomic-layer-specific AED patterns. Surface and subsurface core level shift were determined for each atomic layer.

Low-energy electron point projection microscopy/diffraction study of suspended graphene

NASA Astrophysics Data System (ADS)

Hsu, Wei-Hao; Chang, Wei-Tse; Lin, Chun-Yueh; Chang, Mu-Tung; Hsieh, Chia-Tso; Wang, Chang-Ran; Lee, Wei-Li; Hwang, Ing-Shouh

2017-11-01

In this work, we present our study of suspended graphene with low-energy electrons based on a point projection microscopic/diffractive imaging technique. Both exfoliated and chemical vapor deposition (CVD) graphene samples were studied in an ultra-high vacuum chamber. This method allows imaging of individual adsorbates at the nanometer scale and characterizing graphene layers, graphene lattice orientations, ripples on graphene membranes, etc. We found that long-duration exposure to low-energy electron beams induced aggregation of adsorbates on graphene when the electron dose rate was above a certain level. We also discuss the potential of this technique to conduct coherent diffractive imaging for determining the atomic structures of biological molecules adsorbed on suspended graphene.

Feynman Path Integral Approach to Electron Diffraction for One and Two Slits: Analytical Results

ERIC Educational Resources Information Center

Beau, Mathieu

2012-01-01

In this paper we present an analytic solution of the famous problem of diffraction and interference of electrons through one and two slits (for simplicity, only the one-dimensional case is considered). In addition to exact formulae, various approximations of the electron distribution are shown which facilitate the interpretation of the results.…

Dark-field phase retrieval under the constraint of the Friedel symmetry in coherent X-ray diffraction imaging.

PubMed

Kobayashi, Amane; Sekiguchi, Yuki; Takayama, Yuki; Oroguchi, Tomotaka; Nakasako, Masayoshi

2014-11-17

Coherent X-ray diffraction imaging (CXDI) is a lensless imaging technique that is suitable for visualizing the structures of non-crystalline particles with micrometer to sub-micrometer dimensions from material science and biology. One of the difficulties inherent to CXDI structural analyses is the reconstruction of electron density maps of specimen particles from diffraction patterns because saturated detector pixels and a beam stopper result in missing data in small-angle regions. To overcome this difficulty, the dark-field phase-retrieval (DFPR) method has been proposed. The DFPR method reconstructs electron density maps from diffraction data, which are modified by multiplying Gaussian masks with an observed diffraction pattern in the high-angle regions. In this paper, we incorporated Friedel centrosymmetry for diffraction patterns into the DFPR method to provide a constraint for the phase-retrieval calculation. A set of model simulations demonstrated that this constraint dramatically improved the probability of reconstructing correct electron density maps from diffraction patterns that were missing data in the small-angle region. In addition, the DFPR method with the constraint was applied successfully to experimentally obtained diffraction patterns with significant quantities of missing data. We also discuss this method's limitations with respect to the level of Poisson noise in X-ray detection.

Fine Structure of Diffuse Scattering Rings in Al-Li-Cu Quasicrystal: A Comparative X-ray and Electron Diffraction Study

NASA Astrophysics Data System (ADS)

Donnadieu, P.; Dénoyer, F.

1996-11-01

A comparative X-ray and electron diffraction study has been performed on Al-Li-Cu icosahedral quasicrystal in order to investigate the diffuse scattering rings revealed by a previous work. Electron diffraction confirms the existence of rings but shows that the rings have a fine structure. The diffuse aspect on the X-ray diffraction patterns is then due to an averaging effect. Recent simulations based on the model of canonical cells related to the icosahedral packing give diffractions patterns in agreement with this fine structure effect. Nous comparons les diagrammes de diffraction des rayon-X et des électrons obtenus sur les mêmes échantillons du quasicristal icosaèdrique Al-Li-Cu. Notre but est d'étudier les anneaux de diffusion diffuse mis en évidence par un travail précédent. Les diagrammes de diffraction électronique confirment la présence des anneaux mais ils montrent aussi que ces anneaux possèdent une structure fine. L'aspect diffus des anneaux révélés par la diffraction des rayons X est dû à un effet de moyenne. Des simulations récentes basées sur la décomposition en cellules canoniques de l'empilement icosaédrique produisent des diagrammes de diffraction en accord avec ces effects de structure fine.

Study of gold nanoparticle synthesis by synchrotron x-ray diffraction and fluorescence

NASA Astrophysics Data System (ADS)

Yan, Zhongying; Wang, Xiao; Yu, Le; Moeendarbari, Sina; Hao, Yaowu; Cai, Zhonghou; Cheng, Xuemei

Gold nanoparticles have a wide range of potential applications, including therapeutic agent delivery, catalysis, and electronics. Recently a new process of hollow nanoparticle synthesis was reported, the mechanism of which was hypothesized to involve electroless deposition around electrochemically evolved hydrogen bubbles. However, the growth mechanism still needs experimental evidence. We report investigation of this synthesis process using synchrotron x-ray diffraction and fluorescence measurements performed at beamline 2-ID-D of the Advanced Photon Source (APS). A series of gold nanoparticle samples with different synthesis time (50-1200 seconds) were deposited using a mixture electrolyte solution of Na3Au(SO3)2 and H4N2NiO6S2 on anodic aluminum oxide (AAO) membranes. The 2D mapping of fluorescence intensity and comparison of x-ray diffraction peaks of the samples have provided valuable information on the growth mechanism. Work at Bryn Mawr College and University of Texas at Arlington is supported by NSF Grants (1207085 and 1207377) and use of the APS at Argonne National Laboratory is supported by the U. S. Department of Energy under Contract No. DE-AC02-06CH11357.

Application of δ recycling to electron automated diffraction tomography data from inorganic crystalline nanovolumes.

PubMed

Rius, Jordi; Mugnaioli, Enrico; Vallcorba, Oriol; Kolb, Ute

2013-07-01

δ Recycling is a simple procedure for directly extracting phase information from Patterson-type functions [Rius (2012). Acta Cryst. A68, 399-400]. This new phasing method has a clear theoretical basis and was developed with ideal single-crystal X-ray diffraction data. On the other hand, introduction of the automated diffraction tomography (ADT) technique has represented a significant advance in electron diffraction data collection [Kolb et al. (2007). Ultramicroscopy, 107, 507-513]. When combined with precession electron diffraction, it delivers quasi-kinematical intensity data even for complex inorganic compounds, so that single-crystal diffraction data of nanometric volumes are now available for structure determination by direct methods. To check the tolerance of δ recycling to missing data-collection corrections and to deviations from kinematical behaviour of ADT intensities, δ recycling has been applied to differently shaped nanocrystals of various inorganic materials. The results confirm that it can phase ADT data very efficiently. In some cases even more complete structure models than those derived from conventional direct methods and least-squares refinement have been found. During this study it has been demonstrated that the Wilson-plot scaling procedure is largely insensitive to sample thickness variations and missing absorption corrections affecting electron ADT intensities.

Structural and electron diffraction scaling of twisted graphene bilayers

NASA Astrophysics Data System (ADS)

Zhang, Kuan; Tadmor, Ellad B.

2018-03-01

Multiscale simulations are used to study the structural relaxation in twisted graphene bilayers and the associated electron diffraction patterns. The initial twist forms an incommensurate moiré pattern that relaxes to a commensurate microstructure comprised of a repeating pattern of alternating low-energy AB and BA domains surrounding a high-energy AA domain. The simulations show that the relaxation mechanism involves a localized rotation and shrinking of the AA domains that scales in two regimes with the imposed twist. For small twisting angles, the localized rotation tends to a constant; for large twist, the rotation scales linearly with it. This behavior is tied to the inverse scaling of the moiré pattern size with twist angle and is explained theoretically using a linear elasticity model. The results are validated experimentally through a simulated electron diffraction analysis of the relaxed structures. A complex electron diffraction pattern involving the appearance of weak satellite peaks is predicted for the small twist regime. This new diffraction pattern is explained using an analytical model in which the relaxation kinematics are described as an exponentially-decaying (Gaussian) rotation field centered on the AA domains. Both the angle-dependent scaling and diffraction patterns are in quantitative agreement with experimental observations. A Matlab program for extracting the Gaussian model parameters accompanies this paper.

Specimen preparation for cryogenic coherent X-ray diffraction imaging of biological cells and cellular organelles by using the X-ray free-electron laser at SACLA

PubMed Central

Kobayashi, Amane; Sekiguchi, Yuki; Oroguchi, Tomotaka; Okajima, Koji; Fukuda, Asahi; Oide, Mao; Yamamoto, Masaki; Nakasako, Masayoshi

2016-01-01

Coherent X-ray diffraction imaging (CXDI) allows internal structures of biological cells and cellular organelles to be analyzed. CXDI experiments have been conducted at 66 K for frozen-hydrated biological specimens at the SPring-8 Angstrom Compact Free-Electron Laser facility (SACLA). In these cryogenic CXDI experiments using X-ray free-electron laser (XFEL) pulses, specimen particles dispersed on thin membranes of specimen disks are transferred into the vacuum chamber of a diffraction apparatus. Because focused single XFEL pulses destroy specimen particles at the atomic level, diffraction patterns are collected through raster scanning the specimen disks to provide fresh specimen particles in the irradiation area. The efficiency of diffraction data collection in cryogenic experiments depends on the quality of the prepared specimens. Here, detailed procedures for preparing frozen-hydrated biological specimens, particularly thin membranes and devices developed in our laboratory, are reported. In addition, the quality of the frozen-hydrated specimens are evaluated by analyzing the characteristics of the collected diffraction patterns. Based on the experimental results, the internal structures of the frozen-hydrated specimens and the future development for efficient diffraction data collection are discussed. PMID:27359147

Specimen preparation for cryogenic coherent X-ray diffraction imaging of biological cells and cellular organelles by using the X-ray free-electron laser at SACLA.

PubMed

Kobayashi, Amane; Sekiguchi, Yuki; Oroguchi, Tomotaka; Okajima, Koji; Fukuda, Asahi; Oide, Mao; Yamamoto, Masaki; Nakasako, Masayoshi

2016-07-01

Coherent X-ray diffraction imaging (CXDI) allows internal structures of biological cells and cellular organelles to be analyzed. CXDI experiments have been conducted at 66 K for frozen-hydrated biological specimens at the SPring-8 Angstrom Compact Free-Electron Laser facility (SACLA). In these cryogenic CXDI experiments using X-ray free-electron laser (XFEL) pulses, specimen particles dispersed on thin membranes of specimen disks are transferred into the vacuum chamber of a diffraction apparatus. Because focused single XFEL pulses destroy specimen particles at the atomic level, diffraction patterns are collected through raster scanning the specimen disks to provide fresh specimen particles in the irradiation area. The efficiency of diffraction data collection in cryogenic experiments depends on the quality of the prepared specimens. Here, detailed procedures for preparing frozen-hydrated biological specimens, particularly thin membranes and devices developed in our laboratory, are reported. In addition, the quality of the frozen-hydrated specimens are evaluated by analyzing the characteristics of the collected diffraction patterns. Based on the experimental results, the internal structures of the frozen-hydrated specimens and the future development for efficient diffraction data collection are discussed.

Single-slit electron diffraction with Aharonov-Bohm phase: Feynman's thought experiment with quantum point contacts.

PubMed

Khatua, Pradip; Bansal, Bhavtosh; Shahar, Dan

2014-01-10

In a "thought experiment," now a classic in physics pedagogy, Feynman visualizes Young's double-slit interference experiment with electrons in magnetic field. He shows that the addition of an Aharonov-Bohm phase is equivalent to shifting the zero-field wave interference pattern by an angle expected from the Lorentz force calculation for classical particles. We have performed this experiment with one slit, instead of two, where ballistic electrons within two-dimensional electron gas diffract through a small orifice formed by a quantum point contact (QPC). As the QPC width is comparable to the electron wavelength, the observed intensity profile is further modulated by the transverse waveguide modes present at the injector QPC. Our experiments open the way to realizing diffraction-based ideas in mesoscopic physics.

Large-scale purification and crystallization of the endoribonuclease XendoU: troubleshooting with His-tagged proteins

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

Renzi, Fabiana; Panetta, Gianna; Vallone, Beatrice

Recombinant His-tagged XendoU, a eukaryotic endoribonuclease, appeared to aggregate in the presence of divalent cations. Monodisperse protein which yielded crystals diffracting to 2.2 Å was obtained by addition of EDTA. XendoU is the first endoribonuclease described in higher eukaryotes as being involved in the endonucleolytic processing of intron-encoded small nucleolar RNAs. It is conserved among eukaryotes and its viral homologue is essential in SARS replication and transcription. The large-scale purification and crystallization of recombinant XendoU are reported. The tendency of the recombinant enzyme to aggregate could be reversed upon the addition of chelating agents (EDTA, imidazole): aggregation is a potentialmore » drawback when purifying and crystallizing His-tagged proteins, which are widely used, especially in high-throughput structural studies. Purified monodisperse XendoU crystallized in two different space groups: trigonal P3{sub 1}21, diffracting to low resolution, and monoclinic C2, diffracting to higher resolution.« less

Compression of subrelativistic space-charge-dominated electron bunches for single-shot femtosecond electron diffraction.

PubMed

van Oudheusden, T; Pasmans, P L E M; van der Geer, S B; de Loos, M J; van der Wiel, M J; Luiten, O J

2010-12-31

We demonstrate the compression of 95 keV, space-charge-dominated electron bunches to sub-100 fs durations. These bunches have sufficient charge (200 fC) and are of sufficient quality to capture a diffraction pattern with a single shot, which we demonstrate by a diffraction experiment on a polycrystalline gold foil. Compression is realized by means of velocity bunching by inverting the positive space-charge-induced velocity chirp. This inversion is induced by the oscillatory longitudinal electric field of a 3 GHz radio-frequency cavity. The arrival time jitter is measured to be 80 fs.

Digital direct electron imaging of energy-filtered electron backscatter diffraction patterns

NASA Astrophysics Data System (ADS)

Vespucci, S.; Winkelmann, A.; Naresh-Kumar, G.; Mingard, K. P.; Maneuski, D.; Edwards, P. R.; Day, A. P.; O'Shea, V.; Trager-Cowan, C.

2015-11-01

Electron backscatter diffraction is a scanning electron microscopy technique used to obtain crystallographic information on materials. It allows the nondestructive mapping of crystal structure, texture, and strain with a lateral and depth resolution on the order of tens of nanometers. Electron backscatter diffraction patterns (EBSPs) are presently acquired using a detector comprising a scintillator coupled to a digital camera, and the crystallographic information obtainable is limited by the conversion of electrons to photons and then back to electrons again. In this article we will report the direct acquisition of energy-filtered EBSPs using a digital complementary metal-oxide-semiconductor hybrid pixel detector, Timepix. We show results from a range of samples with different mass and density, namely diamond, silicon, and GaN. Direct electron detection allows the acquisition of EBSPs at lower (≤5 keV) electron beam energies. This results in a reduction in the depth and lateral extension of the volume of the specimen contributing to the pattern and will lead to a significant improvement in lateral and depth resolution. Direct electron detection together with energy filtering (electrons having energy below a specific value are excluded) also leads to an improvement in spatial resolution but in addition provides an unprecedented increase in the detail in the acquired EBSPs. An increase in contrast and higher-order diffraction features are observed. In addition, excess-deficiency effects appear to be suppressed on energy filtering. This allows the fundamental physics of pattern formation to be interrogated and will enable a step change in the use of electron backscatter diffraction (EBSD) for crystal phase identification and the mapping of strain. The enhancement in the contrast in high-pass energy-filtered EBSD patterns is found to be stronger for lighter, less dense materials. The improved contrast for such materials will enable the application of the EBSD technique to be expanded to materials for which conventional EBSD analysis is not presently practicable.

Plutonium-uranium mixed oxide characterization by coupling micro-X-ray diffraction and absorption investigations

NASA Astrophysics Data System (ADS)

Degueldre, C.; Martin, M.; Kuri, G.; Grolimund, D.; Borca, C.

2011-09-01

Plutonium-uranium mixed oxide (MOX) fuels are currently used in nuclear reactors. The potential differences of metal redox state and microstructural developments of the matrix before and after irradiation are commonly analysed by electron probe microanalysis. In this work the structure and next-neighbor atomic environments of Pu and U oxide features within unirradiated homogeneous MOX and irradiated (60 MW d kg -1) MOX samples was analysed by micro-X-ray fluorescence (μ-XRF), micro-X-ray diffraction (μ-XRD) and micro-X-ray absorption fine structure (μ-XAFS) spectroscopy. The grain properties, chemical bonding, valences and stoichiometry of Pu and U are determined from the experimental data gained for the unirradiated as well as for irradiated fuel material examined in the center of the fuel as well as in its peripheral zone (rim). The formation of sub-grains is observed as well as their development from the center to the rim (polygonization). In the irradiated sample Pu remains tetravalent (>95%) and no (<5%) Pu(V) or Pu(VI) can be detected while the fuel could undergo slight oxidation in the rim zone. Any slight potential plutonium oxidation is buffered by the uranium dioxide matrix while locally fuel cladding interaction could also affect the redox of the fuel.

Comparing results of X-ray diffraction, µ-Raman spectroscopy and neutron diffraction when identifying chemical phases in seized nuclear material, during a comparative nuclear forensics exercise

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

Rondahl, Stina Holmgren; Pointurier, Fabien; Ahlinder, Linnea

This work presents the results for identification of chemical phases obtained by several laboratories as a part of an international nuclear forensic round-robin exercise. In this work powder X-ray diffraction (p-XRD) is regarded as the reference technique. Neutron diffraction produced a superior high-angle diffraction pattern relative to p-XRD. Requiring only small amounts of sample, µ-Raman spectroscopy was used for the first time in this context as a potentially complementary technique to p-XRD. The chemical phases were identified as pure UO 2 in two materials, and as a mixture of UO 2, U 3O 8 and an intermediate species U 3Omore » 7 in the third material.« less

Comparing results of X-ray diffraction, µ-Raman spectroscopy and neutron diffraction when identifying chemical phases in seized nuclear material, during a comparative nuclear forensics exercise

DOE PAGES

Rondahl, Stina Holmgren; Pointurier, Fabien; Ahlinder, Linnea; ...

2018-01-24

This work presents the results for identification of chemical phases obtained by several laboratories as a part of an international nuclear forensic round-robin exercise. In this work powder X-ray diffraction (p-XRD) is regarded as the reference technique. Neutron diffraction produced a superior high-angle diffraction pattern relative to p-XRD. Requiring only small amounts of sample, µ-Raman spectroscopy was used for the first time in this context as a potentially complementary technique to p-XRD. The chemical phases were identified as pure UO 2 in two materials, and as a mixture of UO 2, U 3O 8 and an intermediate species U 3Omore » 7 in the third material.« less

Observation of coherent optical phonons excited by femtosecond laser radiation in Sb films by ultrafast electron diffraction method

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

Mironov, B. N.; Kompanets, V. O.; Aseev, S. A., E-mail: isanfemto@yandex.ru

2017-03-15

The generation of coherent optical phonons in a polycrystalline antimony film sample has been investigated using femtosecond electron diffraction method. Phonon vibrations have been induced in the Sb sample by the main harmonic of a femtosecond Ti:Sa laser (λ = 800 nm) and probed by a pulsed ultrashort photoelectron beam synchronized with the pump laser. The diffraction patterns recorded at different times relative to the pump laser pulse display oscillations of electron diffraction intensity corresponding to the frequencies of vibrations of optical phonons: totally symmetric (A{sub 1g}) and twofold degenerate (E{sub g}) phonon modes. The frequencies that correspond to combinationsmore » of these phonon modes in the Sb sample have also been experimentally observed.« less

Transmission electron microscope studies of extraterrestrial materials

NASA Technical Reports Server (NTRS)

Keller, Lindsay P.

1995-01-01

Transmission Electron Microscopy, X-Ray spectrometry and electron-energy-loss spectroscopy are used to analyse carbon in interplanetary dust particles. Optical micrographs are shown depicting cross sections of the dust particles embedded in sulphur. Selected-area electron diffraction patterns are shown. Transmission Electron Microscope specimens of lunar soil were prepared using two methods: ion-milling and ultramicrotomy. A combination of high resolution TEM imaging and electron diffraction is used to characterize the opaque assemblages. The opaque assemblages analyzed in this study are dominated by ilmenite with lesser rutile and spinel exsolutions, and traces of Fe metal.

Study of the Decomposition and Phase Transition of Uranium Nitride under UHV Conditions via TDS, XRD, SEM, and XPS.

PubMed

Wang, Xiaofang; Long, Zhong; Bin, Ren; Yang, Ruilong; Pan, Qifa; Li, Fangfang; Luo, Lizhu; Hu, Yin; Liu, Kezhao

2016-11-07

Uranium nitrides are among the most promising fuels for Generation IV nuclear reactors, but until now, very little has been known about their thermal stability properties under nonequilibrium conditions. In this work, thermal decomposition of nitrogen-rich uranium nitride (denoted as UN 2-x ) under ultrahigh-vacuum (UHV) conditions was investigated by thermal desorption spectroscopy (TDS). It has been shown that the nitrogen TDS spectrum consists of two peaks at about 723 and 1038 K. The X-ray diffraction, scanning electron microscopy, and X-ray photoelectron microscopy results indicate that UN 2-x (UN 2 phase) decomposed into the α-U 2 N 3 phase in the first step and the α-U 2 N 3 phase decomposed into the UN phase in the second step.

Plasma-induced grafting of acrylic acid on bentonite for the removal of U(VI) from aqueous solution

NASA Astrophysics Data System (ADS)

Hongshan, ZHU; Shengxia, DUAN; Lei, CHEN; Ahmed, ALSAEDI; Tasawar, HAYAT; Jiaxing, LI

2017-11-01

Fabrication of reusable adsorbents with satisfactory adsorption capacity and using environment-friendly preparation processes is required for the environment-related applications. In this study, acrylic acid (AA) was grafted onto bentonite (BT) to generate an AA-graft-BT (AA-g-BT) composite using a plasma-induced grafting technique considered to be an environment-friendly method. The as-prepared composite was characterized by scanning electron microscopy, x-ray powder diffraction, thermal gravity analysis, Fourier transform infrared spectroscopy and Barrett-Emmett-Teller analysis, demonstrating the successful grafting of AA onto BT. In addition, the removal of uranium(VI) (U(VI)) from contaminated aqueous solutions was examined using the as-prepared composite. The influencing factors, including contact time, pH value, ionic strength, temperature, and initial concentration, for the removal of U(VI) were investigated by batch experiments. The experimental process fitted best with the pseudo-second-order kinetic and the Langmuir models. Moreover, thermodynamic investigation revealed a spontaneous and endothermic process. Compared with previous adsorbents, AA-g-BT has potential practical applications in treating U(VI)-contaminated solutions.

Crystal grain growth at the α -uranium phase transformation in praseodymium

NASA Astrophysics Data System (ADS)

Cunningham, Nicholas C.; Velisavljevic, Nenad; Vohra, Yogesh K.

2005-01-01

Structural phase transformations under pressure are examined in praseodymium metal for the range 0-40GPa at ambient temperature. Pressure was generated with a diamond-anvil cell, and data were collected using high-resolution synchrotron x-ray diffraction and the image plate technique. The structural sequence double hexagonal close packed (dhcp)→face centered cubic (fcc)→distorted-fcc (d-fcc)→ α -uranium (α-U) is observed with increasing pressure. Rietveld refinement of all crystallographic phases provided confirmation of the hR24 structure for the d-fcc phase while the previously reported monoclinic phase between the d-fcc and the α-U phase was not confirmed. We observe dramatic crystal grain growth during the volume collapse concurrent with the symmetry-lowering transition to the α-U structure. No preferred orientation axis is observed, and the formation process for these large grains is expected to be via a nucleation and growth mechanism. An analogous effect in rare earth metal cerium suggests that the grain growth during transformation to the α-U structure is a common occurrence in f -electron metals at high pressures.

Low-energy Auger electron diffraction: influence of multiple scattering and angular momentum

NASA Astrophysics Data System (ADS)

Chassé, A.; Niebergall, L.; Kucherenko, Yu.

2002-04-01

The angular dependence of Auger electrons excited from single-crystal surfaces is treated theoretically within a multiple-scattering cluster model taking into account the full Auger transition matrix elements. In particular the model has been used to discuss the influence of multiple scattering and angular momentum of the Auger electron wave on Auger electron diffraction (AED) patterns in the region of low kinetic energies. Theoretical results of AED patterns are shown and discussed in detail for Cu(0 0 1) and Ni(0 0 1) surfaces, respectively. Even though Cu and Ni are very similar in their electronic and scattering properties recently strong differences have been found in AED patterns measured in the low-energy region. It is shown that the differences may be caused to superposition of different electron diffraction effects in an energy-integrated experiment. A good agreement between available experimental and theoretical results has been achieved.

Magnetic and crystal structures of the honeycomb lattice Na2IrO3 and single layer Sr2IrO4

NASA Astrophysics Data System (ADS)

Ye, Feng

2013-03-01

5 d based iridates have recently attracted great attention due to the large spin-orbit coupling (SOC). It is now recognized that the SOC that competes with other relevant energies, particularly the on-site Coulomb interaction U, and have driven novel electronic and magnetic phases. Combining single crystal neutron and x-ray diffractions, we have investigated the magnetic and crystal structures of the honeycomb lattice Na2IrO3. The system orders magnetically below 18.1 K with Ir4+ ions forming zigzag spin chains within the layered honeycomb network with ordered moment of 0.22 μB /Ir site. Such a configuration sharply contrasts the Neel or stripe states proposed in the Kitaev-Heisenberg model. The structure refinement reveals that the Ir atoms form nearly ideal 2D honeycomb lattice while the IrO6 octahedra experience a trigonal distortion that is critical to the ground state. The results of this study provide much-needed experimental insights into the magnetic and crystal structure crucial to the understanding of the exotic magnetic order and possible topological characteristics in the 5 d-electron based honeycomb lattice. Neutron diffraction experiments are also performed to investigate the magnetic and crystal structure of the single layer iridate Sr2IrO4, where new structural information and spin order are obtained that is not available from previous neutron powder diffraction measurement. This work was sponsored in part by the Scientific User Facilities Division, Office of Basic Energy Sciences, US Department of Energy.

Symposium N: Materials and Devices for Thermal-to-Electric Energy Conversion

DTIC Science & Technology

2010-08-24

X - ray diffraction, transmission electron microscopy, scanning electron microscopy, and dynamic light scattering. Thermal conductivity measurements...SEM), X - ray diffraction (XRD) measurements as well as Raman spectroscopy. The results from these techniques indicate a clear modification...was examined by using scanning electron microscope (SEM; HITACHI S-4500 model) attached with an energy dispersive x - ray spectroscopy. The electrical

Atomic structure solution of the complex quasicrystal approximant Al77Rh15Ru8 from electron diffraction data.

PubMed

Samuha, Shmuel; Mugnaioli, Enrico; Grushko, Benjamin; Kolb, Ute; Meshi, Louisa

2014-12-01

The crystal structure of the novel Al77Rh15Ru8 phase (which is an approximant of decagonal quasicrystals) was determined using modern direct methods (MDM) applied to automated electron diffraction tomography (ADT) data. The Al77Rh15Ru8 E-phase is orthorhombic [Pbma, a = 23.40 (5), b = 16.20 (4) and c = 20.00 (5) Å] and has one of the most complicated intermetallic structures solved solely by electron diffraction methods. Its structural model consists of 78 unique atomic positions in the unit cell (19 Rh/Ru and 59 Al). Precession electron diffraction (PED) patterns and high-resolution electron microscopy (HRTEM) images were used for the validation of the proposed atomic model. The structure of the E-phase is described using hierarchical packing of polyhedra and a single type of tiling in the form of a parallelogram. Based on this description, the structure of the E-phase is compared with that of the ε6-phase formed in Al-Rh-Ru at close compositions.

Auger electron diffraction study of Fe 1- xNi x alloys epitaxially grown on Cu(100)

NASA Astrophysics Data System (ADS)

Martin, M. G.; Foy, E.; Chevrier, F.; Krill, G.; Asensio, M. C.

1999-08-01

We have combined Auger electron diffraction (AED), low-energy electron diffraction (LEED) and high-energy electron diffraction (RHEED) to examine the structure of Fe xNi 1- x alloys when the Fe content approaches 65%. At this concentration, the 'invar effect' takes place, so the magnetization falls to zero, and the thermal expansion coefficient is very small. The Fe xNi 1- x alloys, grown as metastable thin films by molecular-beam epitaxy on Cu(100) substrates, were studied as a function of the x stoichiometry. In contrast to the related bulk alloy compounds, we observe the collapse of the fcc-to-bcc structural transition in the Fe-rich films. Furthermore, the local atomic structure around Fe and Ni in the alloy has been simultaneously determined by the angular intensity distributions of Fe L 3VV (703 eV) and Ni L 3VV (848 eV) Auger electrons measured as a function of polar and azimuthal angles. For the films deposited at room temperature, we have confirmed the pseudomorphic growth morphology and the uniformity of the alloys.

ELECTRON MICROSCOPE AND X-RAY DIFFRACTION STUDIES ON A HOMOLOGOUS SERIES OF SATURATED PHOSPHATIDYLCHOLINES.

PubMed

ELBERS, P F; VERVERGAERT, P H

1965-05-01

Three homologous saturated phosphatidylcholines were studied by electron microscopy after tricomplex fixation. The results are compared with those obtained by x-ray diffraction analysis of the same and some other homologous compounds, in the dry crystalline state and after tricomplex fixation. By electron microscopy alternating dark and light bands are observed which are likely to correspond to phosphatide double layers. X-Ray diffraction reveals the presence of lamellar structures of regular spacing. The layer spacings obtained by both methods are in good agreement. From the electron micrographs the width of the polar parts of the double layers can be derived directly. The width of the carboxylglycerylphosphorylcholine moiety of the layers is found by extrapolating the x-ray diffraction data to zero chain length of the fatty acids. When from this width the contribution of the carboxylglyceryl part of the molecules is subtracted, again we find good agreement with the electron microscope measurements. An attempt has been made to account for the different layer spacings measured in terms of orientation of the molecules within the double layers.

Investigation of the effect of phase nonuniformities and the microwave field distribution on the electronic efficiency of a diffraction-radiation generator

NASA Astrophysics Data System (ADS)

Maksimov, P. P.; Tsvyk, A. I.; Shestopalov, V. P.

1985-10-01

The effect of local phase nonuniformities of the diffraction gratings and the field distribution of the open cavity on the electronic efficiency of a diffraction-radiation generator (DRG) is analyzed numerically on the basis of a self-consistent system of nonlinear stationary equations for the DRG. It is shown that the interaction power and efficiency of a DRG can be increased by the use of an open cavity with a nonuniform diffraction grating and a complex form of microwave field distribution over the interaction space.

Modulated Electron Emission by Scattering-Interference of Primary Electrons

NASA Astrophysics Data System (ADS)

Valeri, Sergio; di Bona, Alessandro

We review the effects of scattering-interference of the primary, exciting beam on the electron emission from ordered atomic arrays. The yield of elastically and inelastically backscattered electrons, Auger electrons and secondary electrons shows a marked dependence on the incidence angle of primary electrons. Both the similarity and the relative importance of processes experienced by incident and excident electrons are discussed. We also present recent studies of electron focusing and defocusing along atomic chains. The interplay between these two processes determines the in-depth profile of the primary electron intensity anisotropy. Finally, the potential for surface-structural studies and limits for quantitative analysis are discussed, in comparison with the Auger electron diffraction (AED) and photoelectron diffraction (PD) techniques.

Imaging ultrafast dynamics of molecules with laser-induced electron diffraction.

PubMed

Lin, C D; Xu, Junliang

2012-10-14

We introduce a laser-induced electron diffraction method (LIED) for imaging ultrafast dynamics of small molecules with femtosecond mid-infrared lasers. When molecules are placed in an intense laser field, both low- and high-energy photoelectrons are generated. According to quantitative rescattering (QRS) theory, high-energy electrons are produced by a rescattering process where electrons born at the early phase of the laser pulse are driven back to rescatter with the parent ion. From the high-energy electron momentum spectra, field-free elastic electron-ion scattering differential cross sections (DCS), or diffraction images, can be extracted. With mid-infrared lasers as the driving pulses, it is further shown that the DCS can be used to extract atomic positions in a molecule with sub-angstrom spatial resolution, in close analogy to the standard electron diffraction method. Since infrared lasers with pulse duration of a few to several tens of femtoseconds are already available, LIED can be used for imaging dynamics of molecules with sub-angstrom spatial and a few-femtosecond temporal resolution. The first experiment with LIED has shown that the bond length of oxygen molecules shortens by 0.1 Å in five femtoseconds after single ionization. The principle behind LIED and its future outlook as a tool for dynamic imaging of molecules are presented.

Influence of quantum diffraction and shielding on electron-ion collision in two-component semiclassical plasmas

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

Hong, Woo-Pyo; Jung, Young-Dae, E-mail: ydjung@hanyang.ac.kr; Department of Applied Physics and Department of Bionanotechnology, Hanyang University, Ansan, Kyunggi-Do 426-791

2015-01-15

The influence of quantum diffraction and shielding on the electron-ion collision process is investigated in two-component semiclassical plasmas. The eikonal method and micropotential taking into account the quantum diffraction and shielding are used to obtain the eikonal scattering phase shift and the eikonal collision cross section as functions of the collision energy, density parameter, Debye length, electron de Broglie wavelength, and the impact parameter. The result shows that the quantum diffraction and shielding effects suppress the eikonal scattering phase shift as well as the differential eikonal collision cross section, especially, in small-impact parameter regions. It is also shown that themore » quantum shielding effect on the eikonal collision cross section is more important in low-collision energies. In addition, it is found that the eikonal collision cross section increases with an increase in the density parameter. The variations of the eikonal cross section due to the quantum diffraction and shielding effects are also discussed.« less

Folding and stacking defects of graphene flakes probed by electron nanobeam

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

Persichetti, L.; Fanfoni, M.; Sgarlata, A.

2011-07-25

Combining nanoscale imaging with local electron spectroscopy and diffraction has provided direct information on folding and stacking defects of graphene flakes produced by unrolled multi-walled carbon nanotubes. Structural data obtained by nanoarea electron diffraction complemented with systematic electron energy loss spectroscopy measurements of the surface plasmon losses of single flakes show the presence of flat bilayer regions coexisting with folded areas where the topology of buckled graphene resembles that of warped carbon nanostructures.

Structural changes induced by lattice-electron interactions: SiO2 stishovite and FeTiO3 ilmenite.

PubMed

Yamanaka, Takamitsu

2005-09-01

The bright source and highly collimated beam of synchrotron radiation offers many advantages for single-crystal structure analysis under non-ambient conditions. The structure changes induced by the lattice-electron interaction under high pressure have been investigated using a diamond anvil pressure cell. The pressure dependence of electron density distributions around atoms is elucidated by a single-crystal diffraction study using deformation electron density analysis and the maximum entropy method. In order to understand the bonding electrons under pressure, diffraction intensity measurements of FeTiO3 ilmenite and gamma-SiO2 stishovite single crystals at high pressures were made using synchrotron radiation. Both diffraction studies describe the electron density distribution including bonding electrons and provide the effective charge of the cations. In both cases the valence electrons are more localized around the cations with increasing pressure. This is consistent with molecular orbital calculations, proving that the bonding electron density becomes smaller with pressure. The thermal displacement parameters of both samples are reduced with increasing pressure.

Femtosecond Electron Wave Packet Propagation and Diffraction: Towards Making the ``Molecular Movie"

NASA Astrophysics Data System (ADS)

Miller, R. J. Dwayne

2003-03-01

Time-resolved electron diffraction harbors great promise for achieving atomic resolution of the fastest chemical processes. The generation of sufficiently short electron pulses to achieve this real time view of a chemical reaction has been limited by problems in maintaining short electron pulses with realistic electron densities to the sample. The propagation dynamics of femtosecond electron packets in the drift region of a photoelectron gun are investigated with an N-body numerical simulation and mean-field model. This analyis shows that the redistribution of electrons inside the packet, arising from space-charge and dispersion contributions, changes the pulse envelope and leads to the development of a spatially linear axial velocity distribution. These results have been used in the design of femtosecond photoelectron guns with higher time resolution and novel electron-optical methods of pulse characterization that are approaching 100 fs timescales. Time-resolved diffraction studies with electron pulses of approximately 500 femtoseconds have focused on solid-liquid phase transitions under far from equilibrium conditions. This work gives a microscopic description of the melting process and illustrates the promise of atomically resolving transition state processes.

Classification and assessment of retrieved electron density maps in coherent X-ray diffraction imaging using multivariate analysis.

PubMed

Sekiguchi, Yuki; Oroguchi, Tomotaka; Nakasako, Masayoshi

2016-01-01

Coherent X-ray diffraction imaging (CXDI) is one of the techniques used to visualize structures of non-crystalline particles of micrometer to submicrometer size from materials and biological science. In the structural analysis of CXDI, the electron density map of a sample particle can theoretically be reconstructed from a diffraction pattern by using phase-retrieval (PR) algorithms. However, in practice, the reconstruction is difficult because diffraction patterns are affected by Poisson noise and miss data in small-angle regions due to the beam stop and the saturation of detector pixels. In contrast to X-ray protein crystallography, in which the phases of diffracted waves are experimentally estimated, phase retrieval in CXDI relies entirely on the computational procedure driven by the PR algorithms. Thus, objective criteria and methods to assess the accuracy of retrieved electron density maps are necessary in addition to conventional parameters monitoring the convergence of PR calculations. Here, a data analysis scheme, named ASURA, is proposed which selects the most probable electron density maps from a set of maps retrieved from 1000 different random seeds for a diffraction pattern. Each electron density map composed of J pixels is expressed as a point in a J-dimensional space. Principal component analysis is applied to describe characteristics in the distribution of the maps in the J-dimensional space. When the distribution is characterized by a small number of principal components, the distribution is classified using the k-means clustering method. The classified maps are evaluated by several parameters to assess the quality of the maps. Using the proposed scheme, structure analysis of a diffraction pattern from a non-crystalline particle is conducted in two stages: estimation of the overall shape and determination of the fine structure inside the support shape. In each stage, the most accurate and probable density maps are objectively selected. The validity of the proposed scheme is examined by application to diffraction data that were obtained from an aggregate of metal particles and a biological specimen at the XFEL facility SACLA using custom-made diffraction apparatus.

Recombinant Reflectin-Based Optical Materials

DTIC Science & Technology

2012-01-01

sili- con substrates were placed in a sealed plastic box. The RH was controlled using a Dydra electronic cigar humidifier and monitored using a Fisher...diffraction gratings to generate diffraction patterns. Nano-spheres and la- mellar microstructures of refCBA samples were observed by scanning electron ...samples were observed by scanning electron microscopy and atomic force microscopy. Despite the reduced complexity of the refCBA protein compared to natural

Effect of screw threading dislocations and inverse domain boundaries in GaN on the shape of reciprocal-space maps.

PubMed

Barchuk, Mykhailo; Motylenko, Mykhaylo; Lukin, Gleb; Pätzold, Olf; Rafaja, David

2017-04-01

The microstructure of polar GaN layers, grown by upgraded high-temperature vapour phase epitaxy on [001]-oriented sapphire substrates, was studied by means of high-resolution X-ray diffraction and transmission electron microscopy. Systematic differences between reciprocal-space maps measured by X-ray diffraction and those which were simulated for different densities of threading dislocations revealed that threading dislocations are not the only microstructure defect in these GaN layers. Conventional dark-field transmission electron microscopy and convergent-beam electron diffraction detected vertical inversion domains as an additional microstructure feature. On a series of polar GaN layers with different proportions of threading dislocations and inversion domain boundaries, this contribution illustrates the capability and limitations of coplanar reciprocal-space mapping by X-ray diffraction to distinguish between these microstructure features.

Coherent Diffractive Imaging: From Nanometric Down to Picometric Resolution

NASA Astrophysics Data System (ADS)

De Caro, Liberato; Carlino, Elvio; Siliqi, Dritan; Giannini, Cinzia

Coherent diffractive imaging (CDI) is a novel technique for inspecting (crystalline and non-crystalline) matter from nanometric down to picometric resolution. It was used originally with X-rays and, more recently, with electrons (so-called electron diffractive imaging, or EDI). This chapter introduces basic concepts concerning CDI and addresses the different types of X-ray CDI experiments that have been conducted, namely plane wave CDI from isolated objects in forward scattering, focused-beam Fresnel CDI from isolated objects in forward scattering, Bragg CDI from nanocrystals, and keyhole CDI and ptychography from extended objects. A CDI experiment with a transmission electron microscope, alternatively named an EDI experiment, is also introduced.

TAKASAGO-6 apparatus for cryogenic coherent X-ray diffraction imaging of biological non-crystalline particles using X-ray free electron laser at SACLA.

PubMed

Kobayashi, Amane; Sekiguchi, Yuki; Takayama, Yuki; Oroguchi, Tomotaka; Shirahama, Keiya; Torizuka, Yasufumi; Manoda, Masahiro; Nakasako, Masayoshi; Yamamoto, Masaki

2016-05-01

Coherent X-ray diffraction imaging (CXDI) is a technique for structure analyses of non-crystalline particles with dimensions ranging from micrometer to sub-micrometer. We have developed a diffraction apparatus named TAKASAGO-6 for use in single-shot CXDI experiments of frozen-hydrated non-crystalline biological particles at cryogenic temperature with X-ray free electron laser pulses provided at a repetition rate of 30 Hz from the SPring-8 Angstrom Compact free-electron LAser. Specimen particles are flash-cooled after being dispersed on thin membranes supported by specially designed disks. The apparatus is equipped with a high-speed translation stage with a cryogenic pot for raster-scanning of the disks at a speed higher than 25 μm/33 ms. In addition, we use devices assisting the easy transfer of cooled specimens from liquid-nitrogen storages to the cryogenic pot. In the current experimental procedure, more than 20 000 diffraction patterns can be collected within 1 h. Here we report the key components and performance of the diffraction apparatus. Based on the efficiency of the diffraction data collection and the structure analyses of metal particles, biological cells, and cellular organelles, we discuss the future application of this diffraction apparatus for structure analyses of biological specimens.

Filming nuclear dynamics of iodine using x-ray diffraction at the LCLS

NASA Astrophysics Data System (ADS)

Ware, Matthew; Natan, Adi; Glownia, James; Cryan, James; Bucksbaum, Phil

2017-04-01

We will provide an overview of our analysis of the nuclear dynamics of iodine. At the LCLS, we pumped a gas cell of iodine with a weak 520nm, 50 fs pulse, and the nuclear dynamics are then probed with 9 keV, 40 fs x-rays with variable time delay. This allows us to simultaneously image nuclear wavepackets on the dissociating A state, on the bound B state, and even Raman wavepackets in the ground electronic state. We will explain at length how we isolate each of these signals using a Legendre decomposition of our x-ray data and the selection rules for each of the transitions. Likewise, we will discuss how we convert the x-ray diffraction patterns into real-space movies of the nuclear dynamics. Research supported by the U.S. Department of Energy, Office of Basic Energy Sciences, Atomic, Molecular, and Optical Science Program. Use of LCLS supported under DOE Contract No. DE-AC02-76F00515.

Large-Pore 3D Cubic Mesoporous (KIT-6) Hybrid Bearing a Hard-Soft Donor Combined Ligand for Enhancing U(VI) Capture: An Experimental and Theoretical Investigation.

PubMed

Yuan, Li-Yong; Zhu, Lin; Xiao, Cheng-Liang; Wu, Qun-Yan; Zhang, Nan; Yu, Ji-Pan; Chai, Zhi-Fang; Shi, Wei-Qun

2017-02-01

A preorganized tetradentate phenanthrolineamide (DAPhen) ligand with hard and soft donors combined in the same molecule has been found to possess high extraction ability toward actinides over lanthanides from acidic aqueous solution in our previous work. Herein we grafted phenanthrolineamide groups onto a large-pore three-dimensional cubic silica support by the reaction of DAPhen siloxane with KIT-6 substrate to prepare a novel uranium-selective sorbent, KIT-6-DAPhen. The as-synthesized sorbent was well-characterized by scanning electron microscopy, high-resolution transmission electron microscopy, N 2 adsorption/desorption, X-ray diffraction, FT-IR, 13 C cross-polarization magic-angle spinning NMR, and TGA techniques, which confirmed the consummation of the functionalization. Subsequently, the effects of contact time, solution pH, initial U(VI) concentration, and the presence of competing metal ions on the U(VI) sorption onto KIT-6-DAPhen sorbent were investigated in detail. It was found that KIT-6-DAPhen showed largely enhanced sorption capacity and excellent selectivity toward U(VI). The maximum sorption capacity of KIT-6-DAPhen at pH 5.0 reaches 328 mg of U/g of sorbent, which is superior to most of functionalized mesoporous silica materials. Density functional theory coupled with quasi-relativistic small-core pseudopotentials was used to explore the sorption interaction between U(VI) and KIT-6-DAPhen, which gives a sorption reaction of KIT-6-DAPhen + [UO 2 (H 2 O) 5 ] 2+ + NO 3 - ⇄ [UO 2 (KIT-6-DAPhen)(NO 3 )] + + 5H 2 O. The findings of the present work provide new clues for developing new actinide sorbents by combining new ligands with various mesoporous matrixes.

The collection of MicroED data for macromolecular crystallography.

PubMed

Shi, Dan; Nannenga, Brent L; de la Cruz, M Jason; Liu, Jinyang; Sawtelle, Steven; Calero, Guillermo; Reyes, Francis E; Hattne, Johan; Gonen, Tamir

2016-05-01

The formation of large, well-ordered crystals for crystallographic experiments remains a crucial bottleneck to the structural understanding of many important biological systems. To help alleviate this problem in crystallography, we have developed the MicroED method for the collection of electron diffraction data from 3D microcrystals and nanocrystals of radiation-sensitive biological material. In this approach, liquid solutions containing protein microcrystals are deposited on carbon-coated electron microscopy grids and are vitrified by plunging them into liquid ethane. MicroED data are collected for each selected crystal using cryo-electron microscopy, in which the crystal is diffracted using very few electrons as the stage is continuously rotated. This protocol gives advice on how to identify microcrystals by light microscopy or by negative-stain electron microscopy in samples obtained from standard protein crystallization experiments. The protocol also includes information about custom-designed equipment for controlling crystal rotation and software for recording experimental parameters in diffraction image metadata. Identifying microcrystals, preparing samples and setting up the microscope for diffraction data collection take approximately half an hour for each step. Screening microcrystals for quality diffraction takes roughly an hour, and the collection of a single data set is ∼10 min in duration. Complete data sets and resulting high-resolution structures can be obtained from a single crystal or by merging data from multiple crystals.

A pipeline for comprehensive and automated processing of electron diffraction data in IPLT.

PubMed

Schenk, Andreas D; Philippsen, Ansgar; Engel, Andreas; Walz, Thomas

2013-05-01

Electron crystallography of two-dimensional crystals allows the structural study of membrane proteins in their native environment, the lipid bilayer. Determining the structure of a membrane protein at near-atomic resolution by electron crystallography remains, however, a very labor-intense and time-consuming task. To simplify and accelerate the data processing aspect of electron crystallography, we implemented a pipeline for the processing of electron diffraction data using the Image Processing Library and Toolbox (IPLT), which provides a modular, flexible, integrated, and extendable cross-platform, open-source framework for image processing. The diffraction data processing pipeline is organized as several independent modules implemented in Python. The modules can be accessed either from a graphical user interface or through a command line interface, thus meeting the needs of both novice and expert users. The low-level image processing algorithms are implemented in C++ to achieve optimal processing performance, and their interface is exported to Python using a wrapper. For enhanced performance, the Python processing modules are complemented with a central data managing facility that provides a caching infrastructure. The validity of our data processing algorithms was verified by processing a set of aquaporin-0 diffraction patterns with the IPLT pipeline and comparing the resulting merged data set with that obtained by processing the same diffraction patterns with the classical set of MRC programs. Copyright © 2013 Elsevier Inc. All rights reserved.

A pipeline for comprehensive and automated processing of electron diffraction data in IPLT

PubMed Central

Schenk, Andreas D.; Philippsen, Ansgar; Engel, Andreas; Walz, Thomas

2013-01-01

Electron crystallography of two-dimensional crystals allows the structural study of membrane proteins in their native environment, the lipid bilayer. Determining the structure of a membrane protein at near-atomic resolution by electron crystallography remains, however, a very labor-intense and time-consuming task. To simplify and accelerate the data processing aspect of electron crystallography, we implemented a pipeline for the processing of electron diffraction data using the Image Processing Library & Toolbox (IPLT), which provides a modular, flexible, integrated, and extendable cross-platform, open-source framework for image processing. The diffraction data processing pipeline is organized as several independent modules implemented in Python. The modules can be accessed either from a graphical user interface or through a command line interface, thus meeting the needs of both novice and expert users. The low-level image processing algorithms are implemented in C++ to achieve optimal processing performance, and their interface is exported to Python using a wrapper. For enhanced performance, the Python processing modules are complemented with a central data managing facility that provides a caching infrastructure. The validity of our data processing algorithms was verified by processing a set of aquaporin-0 diffraction patterns with the IPLT pipeline and comparing the resulting merged data set with that obtained by processing the same diffraction patterns with the classical set of MRC programs. PMID:23500887

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.

Direct Measurement of Polarization-Induced Fields in GaN/AlN by Nano-Beam Electron Diffraction

NASA Astrophysics Data System (ADS)

Carvalho, Daniel; Müller-Caspary, Knut; Schowalter, Marco; Grieb, Tim; Mehrtens, Thorsten; Rosenauer, Andreas; Ben, Teresa; García, Rafael; Redondo-Cubero, Andrés; Lorenz, Katharina; Daudin, Bruno; Morales, Francisco M.

2016-06-01

The built-in piezoelectric fields in group III-nitrides can act as road blocks on the way to maximizing the efficiency of opto-electronic devices. In order to overcome this limitation, a proper characterization of these fields is necessary. In this work nano-beam electron diffraction in scanning transmission electron microscopy mode has been used to simultaneously measure the strain state and the induced piezoelectric fields in a GaN/AlN multiple quantum well system.

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

PubMed

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

2013-10-01

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

Use of reciprocal lattice layer spacing in electron backscatter diffraction pattern analysis

PubMed

Michael; Eades

2000-03-01

In the scanning electron microscope using electron backscattered diffraction, it is possible to measure the spacing of the layers in the reciprocal lattice. These values are of great use in confirming the identification of phases. The technique derives the layer spacing from the higher-order Laue zone rings which appear in patterns from many materials. The method adapts results from convergent-beam electron diffraction in the transmission electron microscope. For many materials the measured layer spacing compares well with the calculated layer spacing. A noted exception is for higher atomic number materials. In these cases an extrapolation procedure is described that requires layer spacing measurements at a range of accelerating voltages. This procedure is shown to improve the accuracy of the technique significantly. The application of layer spacing measurements in EBSD is shown to be of use for the analysis of two polytypes of SiC.

Characterization of calcium crystals in Abelia using x-ray diffraction and electron microscopes

USDA-ARS?s Scientific Manuscript database

Localization, chemical composition, and morphology of calcium crystals in leaves and stems of Abelia mosanensis and A. ×grandiflora were analyzed with a variable pressure scanning electron microscope (VP-SEM) equipped with an X-ray diffraction system, low temperature SEM (LT-SEM) and a transmission ...

Multiple defocused coherent diffraction imaging: method for simultaneously reconstructing objects and probe using X-ray free-electron lasers.

PubMed

Hirose, Makoto; Shimomura, Kei; Suzuki, Akihiro; Burdet, Nicolas; Takahashi, Yukio

2016-05-30

The sample size must be less than the diffraction-limited focal spot size of the incident beam in single-shot coherent X-ray diffraction imaging (CXDI) based on a diffract-before-destruction scheme using X-ray free electron lasers (XFELs). This is currently a major limitation preventing its wider applications. We here propose multiple defocused CXDI, in which isolated objects are sequentially illuminated with a divergent beam larger than the objects and the coherent diffraction pattern of each object is recorded. This method can simultaneously reconstruct both objects and a probe from the coherent X-ray diffraction patterns without any a priori knowledge. We performed a computer simulation of the prposed method and then successfully demonstrated it in a proof-of-principle experiment at SPring-8. The prposed method allows us to not only observe broad samples but also characterize focused XFEL beams.

Characterization of mineral coatings associated with a Pleistocene-Holocene rock art style: The Northern Running Figures of the East Alligator River region, western Arnhem Land, Australia.

PubMed

King, Penelope L; Troitzsch, Ulrike; Jones, Tristen

2017-02-01

This data article contains mineralogic and chemical data from mineral coatings associated with rock art from the East Alligator River region. The coatings were collected adjacent to a rock art style known as the "Northern Running Figures" for the purposes of radiocarbon dating (doi:10.1016/j.jasrep.2016.11.016; (T. Jones, V. Levchenko, P.L. King, U. Troitzsch, D. Wesley, 2017) [1]). This contribution includes raw and processed powder X-ray Diffraction data, Scanning Electron Microscopy energy dispersive spectroscopy data, and Fourier Transform infrared spectral data.

Flux growth of high-quality CoFe 2O 4 single crystals and their characterization

NASA Astrophysics Data System (ADS)

Wang, W. H.; Ren, X.

2006-04-01

We report the growth of high-quality CoFe 2O 4 single crystals using a borax flux method. The crystals were characterized by powder X-ray diffraction, electron probe microanalysis and Raman spectroscopy. We found the crystals are flux-free and highly homogeneous in composition. X-ray rocking curves of the CoFe 2O 4 single crystals showed a full-width at half-maximum of 0.15°. The saturation magnetization of the CoFe 2O 4 single crystals was measured to be 90 emu/g or equivalently 3.65 μ B/f.u. at 5 K.

Reduced Uranium Phases Produced from Anaerobic Reaction with Nanoscale Zerovalent Iron.

PubMed

Tsarev, Sergey; Collins, Richard N; Fahy, Adam; Waite, T David

2016-03-01

Nanoscale zerovalent iron (nZVI) has shown potential to be an effective remediation agent for uranium-contaminated subsurface environments, however, the nature of the reaction products and their formation kinetics have not been fully elucidated over a range of environmentally relevant conditions. In this study, the oxygen-free reaction of U(VI) with varying quantities of nZVI was examined at pH 7 in the presence of both calcium and carbonate using a combination of X-ray absorption spectroscopy, X-ray diffraction and transmission electron microscopy. It was observed that the structure of the reduced U solid phases was time dependent and largely influenced by the ratio of nZVI to U in the system. At the highest U:Fe molar ratio examined (1:4), nanoscale uraninite (UO2) was predominantly formed within 1 day of reaction. At lower U:Fe molar ratios (1:21), evidence was obtained for the formation of sorbed U(IV) and U(V) surface complexes which slowly transformed to UO2 nanoparticles that were stable for up to 1 year of anaerobic incubation. After 8 days of reaction at the lowest U:Fe molar ratio examined (1:110), sorbed U(IV) was still the major form of U associated with the solid phase. Regardless of the U:Fe molar ratio, the anaerobic corrosion of nZVI resulted in the slow formation of micron-sized fibrous chukanovite (Fe2(OH)2CO3) particles.

Electron-spectroscopy and -diffraction study of the conductivity of CVD diamond ( 0 0 1 )2×1 surface

NASA Astrophysics Data System (ADS)

Kono, S.; Takano, T.; Shimomura, M.; Goto, T.; Sato, K.; Abukawa, T.; Tachiki, M.; Kawarada, H.

2003-04-01

A chemical vapor deposition as-grown diamond (0 0 1) single-domain 2 × 1 surface was studied by electron-spectroscopy and electron-diffraction in ultrahigh vacuum (UHV). In order to change the surface conductivity (SC) of the diamond in UHV, three annealing stages were used; without annealing, annealing at 300 °C and annealing at 550 °C. From low energy electron diffraction and X-ray photoelectron spectroscopic (XPS) studies, an existence of SC was suggested for the first two stages of annealing and an absence of SC was suggested for the last stage of annealing. Changes in C KVV Auger electron spectroscopic spectra, C KVV Auger electron diffraction (AED) patterns and C 1s XPS peak positions were noticed between the annealing stages at 300 and 550 °C. These changes are interpreted as such that the state of hydrogen involvement in a subsurface of diamond (0 0 1)2 × 1 changes as SC changes. In particular, the presence of local disorder in diamond configuration in SC subsurface is pointed out from C KVV AED. From C 1s XPS peak shifts, a lower bound for the Fermi-level for SC layers from the valence band top is presented to be ˜0.5 eV.

The Art of Photoelectron Spectroscopy, from Micro to Nano

NASA Astrophysics Data System (ADS)

Rotenberg, Eli

Angle-resolved photoemission spectroscopy (ARPES) was developed for the determination of the electronic bandstructure of solids. In the last 20 years, ARPES has become nearly unlimited with respect to instrumental resolution, and therefore able to illuminate more subtle electronic aspects, such as ground-state symmetry breaking and the many-body interactions (MBIs) that characterize ground states such as superconductivity. These MBIs involve exchange of momentum among electrons or with excitations such as phonons, and can therefore couple to nanoscale structures. By controlling the structure at the nanoscale, we can therefore hope to control or enhance the ground state properties of materials through nanoscale engineering. This dream has motivated the development of nanoscale ARPES (nanoARPES) machines that are now coming online worldwide. After a brief overview, I will show the latest results from the new nanoARPES endstation at the MAESTRO facility (Microscopic and Electronic Structure Observatory), a new user beamline commissioned this year at the Advanced Light Source (ALS). We achieved routine operation at spatial resolution around 120 nm, and expect improvement down to 50 nm or better. Examples will include graphene and 2D-metal-chalcogenide heterostructures. I will also discuss the prospects for dramatic improvements expected as new diffraction-limited light sources such as the ALS-U project are realized. Work performed at the Advanced Light Source is supported by the Director, Office of Science, Office of Basic Energy Sciences, of the U.S. Department of Energy under Contract No. DE-AC02-05CH11231.

Two-Dimensional Light Diffraction from an EPROM Chip

ERIC Educational Resources Information Center

Ekkens, Tom

2018-01-01

In introductory physics classes, a laser pointer and a compact disc are all the items required to illustrate diffraction of light in a single dimension. If a two-dimensional diffraction pattern is desired, double axis diffraction grating material is available or a CCD sensor can be extracted from an unused electronics device. This article presents…

Characterization of X80 and X100 Microalloyed Pipeline Steel Using Quantitative X-ray Diffraction

NASA Astrophysics Data System (ADS)

Wiskel, J. B.; Li, X.; Ivey, D. G.; Henein, H.

2018-06-01

Quantitative X-ray diffraction characterization of four (4) X80 and three (3) X100 microalloyed steels was undertaken. The effect of through-thickness position, processing parameters, and composition on the measured crystallite size, microstrain, and J index (relative magnitude of crystallographic texture) was determined. Microstructure analysis using optical microscopy, scanning electron microscopy, transmission electron microscopy, and electron-backscattered diffraction was also undertaken. The measured value of microstrain increased with increasing alloy content and decreasing cooling interrupt temperature. Microstructural features corresponding to crystallite size in the X80 steels were both above and below the detection limit for quantitative X-ray diffraction. The X100 steels consistently exhibited microstructure features below the crystallite size detection limit. The yield stress of each steel increased with increasing microstrain. The increase in microstrain from X80 to X100 is also associated with a change in microstructure from predominantly polygonal ferrite to bainitic ferrite.

Mapping of reciprocal space of La{sub 0.30}CoO{sub 2} in 3D: Analysis of superstructure diffractions and intergrowths with Co{sub 3}O{sub 4}

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

Brázda, Petr, E-mail: brazda@fzu.cz; Palatinus, Lukáš; Klementová, Mariana

2015-07-15

We have used electron diffraction tomography and powder X-ray diffraction to elucidate the structural properties of layered cobaltate γ-La{sub 0.30}CoO{sub 2}. The structure consists of hexagonal sheets of edge-sharing CoO{sub 6} octahedra interleaved by lanthanum monolayers. The La{sup 3+} cations occupy only one third of available P2 sites, forming a 2-dimensional a√3×a√3 superstructure in a–b plane. The results show that there exists no order in the mutual relative shift between the neighbouring La interlayers within the a–b plane. This is manifested in the observed monotonous decrease of the diffracted intensity of the superstructure diffractions along c{sup ⁎} in both X-raymore » and electron diffraction data. The observed lack of stacking order differentiates the La{sub x}CoO{sub 2} from its Ca and Sr analogues where at least a partial stacking order of the cationic interlayers is manifested in experimental data published in literature. - Highlights: • We use electron diffraction tomography for reciprocal space mapping of La{sub 0.30}CoO{sub 2}. • We observed a complete disorder of the stacking of Lanthanum interlayers. • Co{sub 3}O{sub 4} intergrown with La{sub 0.30}CoO{sub 2} crystals brings about fake superstructure diffractions. • Twinning of Co{sub 3}O{sub 4} enhances the problem of fake superstructure diffractions.« less

Energetics of a uranothorite (Th 1–xU xSiO 4) solid solution

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

Guo, Xiaofeng; Szenknect, Stephanie; Mesbah, Adel

High-temperature oxide melt solution calorimetric measurements were completed to determine the enthalpies of formation of the uranothorite, (USiO 4) x–(ThSiO 4) 1–x, solid solution. Phase-pure samples with x values of 0, 0.11, 0.21, 0.35, 0.71, and 0.84 were prepared, purified, and characterized by powder X-ray diffraction, electron probe microanalysis, thermogravimetric analysis and differential scanning calorimetry coupled with in situ mass spectrometry, and high-temperature oxide melt solution calorimetry. This work confirms the energetic metastability of coffinite, USiO 4, and U-rich intermediate silicate phases with respect to a mixture of binary oxides. Furthermore, variations in unit cell parameters and negative excess volumesmore » of mixing, coupled with strongly exothermic enthalpies of mixing in the solid solution, suggest short-range cation ordering that can stabilize intermediate compositions, especially near x = 0.5.« less

Energetics of a uranothorite (Th 1–xU xSiO 4) solid solution

DOE PAGES

Guo, Xiaofeng; Szenknect, Stephanie; Mesbah, Adel; ...

2016-10-11

High-temperature oxide melt solution calorimetric measurements were completed to determine the enthalpies of formation of the uranothorite, (USiO 4) x–(ThSiO 4) 1–x, solid solution. Phase-pure samples with x values of 0, 0.11, 0.21, 0.35, 0.71, and 0.84 were prepared, purified, and characterized by powder X-ray diffraction, electron probe microanalysis, thermogravimetric analysis and differential scanning calorimetry coupled with in situ mass spectrometry, and high-temperature oxide melt solution calorimetry. This work confirms the energetic metastability of coffinite, USiO 4, and U-rich intermediate silicate phases with respect to a mixture of binary oxides. Furthermore, variations in unit cell parameters and negative excess volumesmore » of mixing, coupled with strongly exothermic enthalpies of mixing in the solid solution, suggest short-range cation ordering that can stabilize intermediate compositions, especially near x = 0.5.« less

Three-dimensional rotation electron diffraction: software RED for automated data collection and data processing

PubMed Central

Wan, Wei; Sun, Junliang; Su, Jie; Hovmöller, Sven; Zou, Xiaodong

2013-01-01

Implementation of a computer program package for automated collection and processing of rotation electron diffraction (RED) data is described. The software package contains two computer programs: RED data collection and RED data processing. The RED data collection program controls the transmission electron microscope and the camera. Electron beam tilts at a fine step (0.05–0.20°) are combined with goniometer tilts at a coarse step (2.0–3.0°) around a common tilt axis, which allows a fine relative tilt to be achieved between the electron beam and the crystal in a large tilt range. An electron diffraction (ED) frame is collected at each combination of beam tilt and goniometer tilt. The RED data processing program processes three-dimensional ED data generated by the RED data collection program or by other approaches. It includes shift correction of the ED frames, peak hunting for diffraction spots in individual ED frames and identification of these diffraction spots as reflections in three dimensions. Unit-cell parameters are determined from the positions of reflections in three-dimensional reciprocal space. All reflections are indexed, and finally a list with hkl indices and intensities is output. The data processing program also includes a visualizer to view and analyse three-dimensional reciprocal lattices reconstructed from the ED frames. Details of the implementation are described. Data collection and data processing with the software RED are demonstrated using a calcined zeolite sample, silicalite-1. The structure of the calcined silicalite-1, with 72 unique atoms, could be solved from the RED data by routine direct methods. PMID:24282334

Three-dimensional rotation electron diffraction: software RED for automated data collection and data processing.

PubMed

Wan, Wei; Sun, Junliang; Su, Jie; Hovmöller, Sven; Zou, Xiaodong

2013-12-01

Implementation of a computer program package for automated collection and processing of rotation electron diffraction (RED) data is described. The software package contains two computer programs: RED data collection and RED data processing. The RED data collection program controls the transmission electron microscope and the camera. Electron beam tilts at a fine step (0.05-0.20°) are combined with goniometer tilts at a coarse step (2.0-3.0°) around a common tilt axis, which allows a fine relative tilt to be achieved between the electron beam and the crystal in a large tilt range. An electron diffraction (ED) frame is collected at each combination of beam tilt and goniometer tilt. The RED data processing program processes three-dimensional ED data generated by the RED data collection program or by other approaches. It includes shift correction of the ED frames, peak hunting for diffraction spots in individual ED frames and identification of these diffraction spots as reflections in three dimensions. Unit-cell parameters are determined from the positions of reflections in three-dimensional reciprocal space. All reflections are indexed, and finally a list with hkl indices and intensities is output. The data processing program also includes a visualizer to view and analyse three-dimensional reciprocal lattices reconstructed from the ED frames. Details of the implementation are described. Data collection and data processing with the software RED are demonstrated using a calcined zeolite sample, silicalite-1. The structure of the calcined silicalite-1, with 72 unique atoms, could be solved from the RED data by routine direct methods.

Study of residual stresses in CT test specimens welded by electron beam

NASA Astrophysics Data System (ADS)

Papushkin, I. V.; Kaisheva, D.; Bokuchava, G. D.; Angelov, V.; Petrov, P.

2018-03-01

The paper reports result of residual stress distribution studies in CT specimens reconstituted by electron beam welding (EBW). The main aim of the study is evaluation of the applicability of the welding technique for CT specimens’ reconstitution. Thus, the temperature distribution during electron beam welding of a CT specimen was calculated using Green’s functions and the residual stress distribution was determined experimentally using neutron diffraction. Time-of-flight neutron diffraction experiments were performed on a Fourier stress diffractometer at the IBR-2 fast pulsed reactor in FLNP JINR (Dubna, Russia). The neutron diffraction data estimates yielded a maximal stress level of ±180 MPa in the welded joint.

Geometry of phase-separated domains in phospholipid bilayers by diffraction-contrast electron microscopy.

PubMed Central

Hui, S W

1981-01-01

The sizes and shapes of solidus (gel) phase domains in the hydrated molecular bilayers of dilauroylphosphatidylcholine/dipalmitoylphasphatidylcholine (DLPC/DPPC) (1:1) and phosphatidylserine (PS)/DPPC (1:2) are visualized directly by low dose diffraction-contrast electron microscopy. The temperature and humidity of the bilayers are controlled by an environmental chamber set in an electron microscope. The contrast between crystalline domains is enhanced by electron optical filtering of the diffraction patterns of the bilayers. The domains are seen as a patchwork in the plane of the bilayer, with an average width of 0.2-0.5 micrometer. The percentage of solidus area measured from diffraction-contrast micrographs at various temperatures agrees in general with those depicted by known phase diagrams. The shape and size of the domains resemble those seen by freeze-fracture in multilamellar vesicles. Temperature-related changes in domain size and in phase boundary per unit area are more pronounced in the less miscible DLPC/DPPC mixture. No significant change in these geometric parameters with temperature is found in the PS/DPPC mixture. Mapping domains by their molecular diffraction signals not only verifies the existance of areas of different molecular packing during phase separation but also provides a quantitative measurement of structural boundaries and defects in lipid bilayers. Images FIGURE 1 FIGURE 3 FIGURE 6 PMID:6894707

Lattice parameter functions of (AmyU1-y)O2-x based on XRD and XANES measurements

NASA Astrophysics Data System (ADS)

Nishi, Tsuyoshi; Nakada, Masami; Hirata, Masaru

2017-12-01

The lattice parameters of (Am0.50U0.50)O2.0, (Am0.37U0.63)O2.0, and (Am0.50U0.50)O2-x were determined by powder X-ray diffraction with Cu Kα radiation. In addition, the lattice parameter functions of (AmyU1-y)O2-x (0.00

Diffraction of real and virtual photons in a pyrolytic graphite crystal as source of intensive quasimonochromatic X-ray beam

NASA Astrophysics Data System (ADS)

Bogomazova, E. A.; Kalinin, B. N.; Naumenko, G. A.; Padalko, D. V.; Potylitsyn, A. P.; Sharafutdinov, A. F.; Vnukov, I. E.

2003-01-01

A series of experiments on the parametric X-rays radiation (PXR) generation and radiation soft component diffraction of relativistic electrons in pyrolytic graphite (PG) crystals have been carried out at the Tomsk synchrotron. It is shown that the experimental results with PG crystals are explained by the kinematic PXR theory if we take into account a contribution of the real photons diffraction (transition radiation, bremsstrahlung and PXR photons as well). The measurements of the emission spectrum of channeled electrons in the photon energy range much smaller than the characteristic energy of channeling radiation have been performed with a crystal-diffraction spectrometer. For electrons incident along the <1 1 0> axis of a silicon crystal, the radiation intensity in the energy range 30⩽ ω⩽360 keV exceeds the bremsstrahlung one almost by an order of magnitude. Different possibilities to create an effective source of the monochromatic X-ray beam based on the real and virtual photons diffraction in the PG crystals have been considered.

Combining experiment and optical simulation in coherent X-ray nanobeam characterization of Si/SiGe semiconductor heterostructures

DOE PAGES

Tilka, J. A.; Park, J.; Ahn, Y.; ...

2016-07-06

Here, the highly coherent and tightly focused x-ray beams produced by hard x-ray light sources enable the nanoscale characterization of the structure of electronic materials but are accompanied by significant challenges in the interpretation of diffraction and scattering patterns. X-ray nanobeams exhibit optical coherence combined with a large angular divergence introduced by the x-ray focusing optics. The scattering of nanofocused x-ray beams from intricate semiconductor heterostructures produces a complex distribution of scattered intensity. We report here an extension of coherent xray optical simulations of convergent x-ray beam diffraction patterns to arbitrary x-ray incident angles to allow the nanobeam diffraction patternsmore » of complex heterostructures to be simulated faithfully. These methods are used to extract the misorientation of lattice planes and the strain of individual layers from synchrotron x-ray nanobeam diffraction patterns of Si/SiGe heterostructures relevant to applications in quantum electronic devices. The systematic interpretation of nanobeam diffraction patterns from semiconductor heterostructures presents a new opportunity in characterizing and ultimately designing electronic materials.« less

Coherent diffractive imaging of single helium nanodroplets with a high harmonic generation source.

PubMed

Rupp, Daniela; Monserud, Nils; Langbehn, Bruno; Sauppe, Mario; Zimmermann, Julian; Ovcharenko, Yevheniy; Möller, Thomas; Frassetto, Fabio; Poletto, Luca; Trabattoni, Andrea; Calegari, Francesca; Nisoli, Mauro; Sander, Katharina; Peltz, Christian; J Vrakking, Marc; Fennel, Thomas; Rouzée, Arnaud

2017-09-08

Coherent diffractive imaging of individual free nanoparticles has opened routes for the in situ analysis of their transient structural, optical, and electronic properties. So far, single-shot single-particle diffraction was assumed to be feasible only at extreme ultraviolet and X-ray free-electron lasers, restricting this research field to large-scale facilities. Here we demonstrate single-shot imaging of isolated helium nanodroplets using extreme ultraviolet pulses from a femtosecond-laser-driven high harmonic source. We obtain bright wide-angle scattering patterns, that allow us to uniquely identify hitherto unresolved prolate shapes of superfluid helium droplets. Our results mark the advent of single-shot gas-phase nanoscopy with lab-based short-wavelength pulses and pave the way to ultrafast coherent diffractive imaging with phase-controlled multicolor fields and attosecond pulses.Diffraction imaging studies of free individual nanoparticles have so far been restricted to XUV and X-ray free - electron laser facilities. Here the authors demonstrate the possibility of using table-top XUV laser sources to image prolate shapes of superfluid helium droplets.

Dynamical electron diffraction simulation for non-orthogonal crystal system by a revised real space method.

PubMed

Lv, C L; Liu, Q B; Cai, C Y; Huang, J; Zhou, G W; Wang, Y G

2015-01-01

In the transmission electron microscopy, a revised real space (RRS) method has been confirmed to be a more accurate dynamical electron diffraction simulation method for low-energy electron diffraction than the conventional multislice method (CMS). However, the RRS method can be only used to calculate the dynamical electron diffraction of orthogonal crystal system. In this work, the expression of the RRS method for non-orthogonal crystal system is derived. By taking Na2 Ti3 O7 and Si as examples, the correctness of the derived RRS formula for non-orthogonal crystal system is confirmed by testing the coincidence of numerical results of both sides of Schrödinger equation; moreover, the difference between the RRS method and the CMS for non-orthogonal crystal system is compared at the accelerating voltage range from 40 to 10 kV. Our results show that the CMS method is almost the same as the RRS method for the accelerating voltage above 40 kV. However, when the accelerating voltage is further lowered to 20 kV or below, the CMS method introduces significant errors, not only for the higher-order Laue zone diffractions, but also for zero-order Laue zone. These indicate that the RRS method for non-orthogonal crystal system is necessary to be used for more accurate dynamical simulation when the accelerating voltage is low. Furthermore, the reason for the increase of differences between those diffraction patterns calculated by the RRS method and the CMS method with the decrease of the accelerating voltage is discussed. © 2015 The Authors Journal of Microscopy © 2015 Royal Microscopical Society.

Attosecond electron pulses for 4D diffraction and microscopy

PubMed Central

Baum, Peter; Zewail, Ahmed H.

2007-01-01

In this contribution, we consider the advancement of ultrafast electron diffraction and microscopy to cover the attosecond time domain. The concept is centered on the compression of femtosecond electron packets to trains of 15-attosecond pulses by the use of the ponderomotive force in synthesized gratings of optical fields. Such attosecond electron pulses are significantly shorter than those achievable with extreme UV light sources near 25 nm (≈50 eV) and have the potential for applications in the visualization of ultrafast electron dynamics, especially of atomic structures, clusters of atoms, and some materials. PMID:18000040

TAKASAGO-6 apparatus for cryogenic coherent X-ray diffraction imaging of biological non-crystalline particles using X-ray free electron laser at SACLA

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

Kobayashi, Amane; Sekiguchi, Yuki; Oroguchi, Tomotaka

Coherent X-ray diffraction imaging (CXDI) is a technique for structure analyses of non-crystalline particles with dimensions ranging from micrometer to sub-micrometer. We have developed a diffraction apparatus named TAKASAGO-6 for use in single-shot CXDI experiments of frozen-hydrated non-crystalline biological particles at cryogenic temperature with X-ray free electron laser pulses provided at a repetition rate of 30 Hz from the SPring-8 Angstrom Compact free-electron LAser. Specimen particles are flash-cooled after being dispersed on thin membranes supported by specially designed disks. The apparatus is equipped with a high-speed translation stage with a cryogenic pot for raster-scanning of the disks at a speedmore » higher than 25 μm/33 ms. In addition, we use devices assisting the easy transfer of cooled specimens from liquid-nitrogen storages to the cryogenic pot. In the current experimental procedure, more than 20 000 diffraction patterns can be collected within 1 h. Here we report the key components and performance of the diffraction apparatus. Based on the efficiency of the diffraction data collection and the structure analyses of metal particles, biological cells, and cellular organelles, we discuss the future application of this diffraction apparatus for structure analyses of biological specimens.« less

Quantum-chemical calculations and electron diffraction study of the equilibrium molecular structure of vitamin K3

NASA Astrophysics Data System (ADS)

Khaikin, L. S.; Tikhonov, D. S.; Grikina, O. E.; Rykov, A. N.; Stepanov, N. F.

2014-05-01

The equilibrium molecular structure of 2-methyl-1,4-naphthoquinone (vitamin K3) having C s symmetry is experimentally characterized for the first time by means of gas-phase electron diffraction using quantum-chemical calculations and data on the vibrational spectra of related compounds.

Noble Gas Isotopic Signatures and X-Ray and Electron Diffraction Characteristics of Tagish Lake Carbonaceous Chondrite

NASA Technical Reports Server (NTRS)

Nakamura, T.; Noguchi, T.; Zolensky, M. E.; Takaoka, N.

2001-01-01

Noble gas isotopic signatures and X-ray and electron diffraction characteristics of Tagish Lake indicate that it is a unique carbonaceous chondrite rich in saponite, Fe-Mg-Ca carbonate, primordial noble gases, and presolar grains. Additional information is contained in the original extended abstract.

Electron diffraction study of the sillenites Bi{sub 12}SiO{sub 20}, Bi{sub 25}FeO{sub 39} and Bi{sub 25}InO{sub 39}: Evidence of short-range ordering of oxygen-vacancies in the trivalent sillenites

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

Scurti, Craig A.; Arenas, D. J.; Auvray, Nicolas

We present an electron diffraction study of three sillenites, Bi{sub 12}SiO{sub 20}, Bi{sub 25}FeO{sub 39}, and Bi{sub 25}InO{sub 39} synthesized using the solid-state method. We explore a hypothesis, inspired by optical studies in the literature, that suggests that trivalent sillenites have additional disorder not present in the tetravalent compounds. Electron diffraction patterns of Bi{sub 25}FeO{sub 39} and Bi{sub 25}InO{sub 39} show streaks that confirm deviations from the ideal sillenite structure. Multi-slice simulations of electron-diffraction patterns are presented for different perturbations to the sillenite structure - partial substitution of the M site by Bi{sup 3+}, random and ordered oxygen-vacancies, and amore » frozen-phonon model. Although comparison of experimental data to simulations cannot be conclusive, we consider the streaks as evidence of short-range ordered oxygen-vacancies.« less

Electron Matter Optics and the Quantum Electron Stern-Gerlach Magnet

NASA Astrophysics Data System (ADS)

McGregor, Scot; Bach, Roger; Yin, Xiaolu; Liou, Sy-Hwang; Batelaan, Herman; Gronniger, Glen

2011-05-01

We explore electron interferometry for the purpose of performing fundamental quantum mechanical experiments and sensing applications. To this end electron matter optics elements, in particular, a diffraction limited single slit, a double slit, and a nano-fabricated grating diffraction apparatus as well as a Mach-Zehnder IFM were previously developed. The double slit diffraction pattern has been recorded one electron at a time. Furthermore, the capability of closing each slit on demand has been developed, in that way realizing the thought experiment that Feynman explains in his lectures. The capability of the Mach-Zehnder interferometer to sense DC and AC electromagnetic fields for industrial applications is currently under investigation. Also, the construction of a new type of interferometer that has the potential to significantly increase the enclosed area and thus its sensitivity is in progress. Finally an idea to separate an electron beam fully into its two spin component using an electron interferometer is presented. We gratefully acknowledge funding by NSF Grant No. 0969506 and R. B. and S. M. acknowledge DOE-GAANN fellowships.

A protocol for searching the most probable phase-retrieved maps in coherent X-ray diffraction imaging by exploiting the relationship between convergence of the retrieved phase and success of calculation.

PubMed

Sekiguchi, Yuki; Hashimoto, Saki; Kobayashi, Amane; Oroguchi, Tomotaka; Nakasako, Masayoshi

2017-09-01

Coherent X-ray diffraction imaging (CXDI) is a technique for visualizing the structures of non-crystalline particles with size in the submicrometer to micrometer range in material sciences and biology. In the structural analysis of CXDI, the electron density map of a specimen particle projected along the direction of the incident X-rays can be reconstructed only from the diffraction pattern by using phase-retrieval (PR) algorithms. However, in practice, the reconstruction, relying entirely on the computational procedure, sometimes fails because diffraction patterns miss the data in small-angle regions owing to the beam stop and saturation of the detector pixels, and are modified by Poisson noise in X-ray detection. To date, X-ray free-electron lasers have allowed us to collect a large number of diffraction patterns within a short period of time. Therefore, the reconstruction of correct electron density maps is the bottleneck for efficiently conducting structure analyses of non-crystalline particles. To automatically address the correctness of retrieved electron density maps, a data analysis protocol to extract the most probable electron density maps from a set of maps retrieved from 1000 different random seeds for a single diffraction pattern is proposed. Through monitoring the variations of the phase values during PR calculations, the tendency for the PR calculations to succeed when the retrieved phase sets converged on a certain value was found. On the other hand, if the phase set was in persistent variation, the PR calculation tended to fail to yield the correct electron density map. To quantify this tendency, here a figure of merit for the variation of the phase values during PR calculation is introduced. In addition, a PR protocol to evaluate the similarity between a map of the highest figure of merit and other independently reconstructed maps is proposed. The protocol is implemented and practically examined in the structure analyses for diffraction patterns from aggregates of gold colloidal particles. Furthermore, the feasibility of the protocol in the structure analysis of organelles from biological cells is examined.

Carrier Dynamics and Application of the Phase Coherent Photorefractive Effect in ZnSe Quantum Wells

NASA Astrophysics Data System (ADS)

Dongol, Amit

The intensity dependent diffraction efficiency of a phase coherent photorefractive (PCP) ZnSe quantum well (QW) is investigated at 80 K in a two-beam four-wave mixing (FWM) configuration using 100 fs laser pulses with a repetition rate of 80 MHz. The observed diffraction efficiencies of the first and second-order diffracted beam are on the order of 10-3 and 10-5, respectively, revealing nearly no intensity dependence. The first-order diffraction is caused by the PCP effect where the probe-pulse is diffracted due to a long-living incoherent electron density grating in the QW. The second-order diffraction is created by a combination of diffraction processes. For negative probe-pulse delay, the exciton polarization is diffracted at the electron grating twice by a cascade effect. For positive delay, the diffracted signal is modified by the destructive interference with a chi(5) generated signal due to a dynamical screening effect. Model calculations of the signal traces based on the optical Bloch equations considering inhomogeneous broadening of exciton energies are in good agreement with the experimental data. To study the carrier dynamics responsible for the occurrence of the PCP effect, threebeam FWM experiments are carried out. The non-collinear wave-vectors k1 , k2 and k3 at central wavelength of 441 nm (~2.81 eV) were resonantly tuned to the heavy-hole exciton transition energy at 20 K. In the FWM experiment the time coincident strong pump pulses k1 and k2 create both an exciton density grating in the QW and an electron-hole pair grating in the GaAs while the delayed weak pulse k3 simultaneously probes the exciton lifetime as well as the electron grating capture time. The model calculations are in good agreement with the experimental results also providing information about the transfer delay of electrons arriving from the substrate to the QW. For negative probe-pulse delay we still observe a diffracted signal due to the long living electron density grating in the QW. The electron grating build-up and decay times are also studied with the modified three-beam FWM set-up. Using an optical shutter for pump pulses k1and k2, the dynamics of the electron grating formation and its decay is continuously probed by a delayed pulse k3. The obtained build-up and decay times are found to depend nearly linearly on the intensity of incident pulses k1 and k2 being on the order of several microseconds at low pump intensities. The PCP effect in ZnSe QW possesses a time-gating capability which can be used for real-time holographic imaging. In this work we demonstrate contrast enhanced real time holographic imaging (CEHI) of floating glass beads and of living unicellular animals (Paramecium and Euglena cells) in aqueous solution. We also demonstrate CEHI of a ~100 im thick wire concealed behind a layer of chicken skin. The results demonstrate the potential of PCP QWs for real-time and depth-resolved imaging of moving micrometer sized biological objects in transparent media or of obscured objects in turbid media.

Structure Evolution and Distributions of Grain-Boundary Misorientainons in Submicrocrystalline Molybdenum Irradiated with a Pulsed Electron Beam

NASA Astrophysics Data System (ADS)

Stepanova, E. N.; Grabovetskaya, G. P.; Teresov, A. D.; Mishin, I. P.

2018-05-01

Using the methods of electron backscatter diffraction, electron microscopy and X-ray diffraction analysis, it is demonstrated that irradiation of the surface of a submicrocrystalline molybdenum specimen with a pulsed electron beam in a non-melt regime results in the formation of a gradient structure in its bulk. The irradiation temperature is shown to affect the density of defects, the value of stress, and the distributions of grain-boundary misorientations in the surface and bulk of the submicrocrystalline molybdenum specimens.

Large-Scale Diffraction Patterns from Circular Objects

ERIC Educational Resources Information Center

Rinard, Phillip M.

1976-01-01

Investigates quantitatively the diffractions of light by a U.S. penny and an aperture of the same size. Differences noted between the theory and measurements are discussed, with probable causes indicated. (Author/CP)

Detection of expansion at large angle grain boundaries using electron diffraction

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

Balluffi, R.W.; Bristowe, P.D.

1984-02-01

Lamarre and Sass (LS) (Scripta Metall. 17: 1141(1983)) observed a grain boundary electron diffraction effect from a large angle twist boundary which they claim can be used to obtain the volume expansion at the grain boundary in a direction normal to it. This paper considers the case where the intensity from the grain boundary region, is close to lattice reflections on the same element of the boundary diffraction lattice. Analysis of this complex problem show that the simplified model of LS is misleading in this case. (DLC)

Graphene unit cell imaging by holographic coherent diffraction.

PubMed

Longchamp, Jean-Nicolas; Latychevskaia, Tatiana; Escher, Conrad; Fink, Hans-Werner

2013-06-21

We have imaged a freestanding graphene sheet of 210 nm in diameter with 2 Å resolution by combining coherent diffraction and holography with low-energy electrons. The entire sheet is reconstructed from a single diffraction pattern displaying the arrangement of 660.000 individual graphene unit cells at once. Given the fact that electrons with kinetic energies of the order of 100 eV do not damage biological molecules, it will now be a matter of developing methods for depositing individual proteins onto such graphene sheets.

Design and implementation of an optimal laser pulse front tilting scheme for ultrafast electron diffraction in reflection geometry with high temporal resolution.

PubMed

Pennacchio, Francesco; Vanacore, Giovanni M; Mancini, Giulia F; Oppermann, Malte; Jayaraman, Rajeswari; Musumeci, Pietro; Baum, Peter; Carbone, Fabrizio

2017-07-01

Ultrafast electron diffraction is a powerful technique to investigate out-of-equilibrium atomic dynamics in solids with high temporal resolution. When diffraction is performed in reflection geometry, the main limitation is the mismatch in group velocity between the overlapping pump light and the electron probe pulses, which affects the overall temporal resolution of the experiment. A solution already available in the literature involved pulse front tilt of the pump beam at the sample, providing a sub-picosecond time resolution. However, in the reported optical scheme, the tilted pulse is characterized by a temporal chirp of about 1 ps at 1 mm away from the centre of the beam, which limits the investigation of surface dynamics in large crystals. In this paper, we propose an optimal tilting scheme designed for a radio-frequency-compressed ultrafast electron diffraction setup working in reflection geometry with 30 keV electron pulses containing up to 10 5 electrons/pulse. To characterize our scheme, we performed optical cross-correlation measurements, obtaining an average temporal width of the tilted pulse lower than 250 fs. The calibration of the electron-laser temporal overlap was obtained by monitoring the spatial profile of the electron beam when interacting with the plasma optically induced at the apex of a copper needle (plasma lensing effect). Finally, we report the first time-resolved results obtained on graphite, where the electron-phonon coupling dynamics is observed, showing an overall temporal resolution in the sub-500 fs regime. The successful implementation of this configuration opens the way to directly probe structural dynamics of low-dimensional systems in the sub-picosecond regime, with pulsed electrons.

Design and implementation of an optimal laser pulse front tilting scheme for ultrafast electron diffraction in reflection geometry with high temporal resolution

PubMed Central

Pennacchio, Francesco; Vanacore, Giovanni M.; Mancini, Giulia F.; Oppermann, Malte; Jayaraman, Rajeswari; Musumeci, Pietro; Baum, Peter; Carbone, Fabrizio

2017-01-01

Ultrafast electron diffraction is a powerful technique to investigate out-of-equilibrium atomic dynamics in solids with high temporal resolution. When diffraction is performed in reflection geometry, the main limitation is the mismatch in group velocity between the overlapping pump light and the electron probe pulses, which affects the overall temporal resolution of the experiment. A solution already available in the literature involved pulse front tilt of the pump beam at the sample, providing a sub-picosecond time resolution. However, in the reported optical scheme, the tilted pulse is characterized by a temporal chirp of about 1 ps at 1 mm away from the centre of the beam, which limits the investigation of surface dynamics in large crystals. In this paper, we propose an optimal tilting scheme designed for a radio-frequency-compressed ultrafast electron diffraction setup working in reflection geometry with 30 keV electron pulses containing up to 105 electrons/pulse. To characterize our scheme, we performed optical cross-correlation measurements, obtaining an average temporal width of the tilted pulse lower than 250 fs. The calibration of the electron-laser temporal overlap was obtained by monitoring the spatial profile of the electron beam when interacting with the plasma optically induced at the apex of a copper needle (plasma lensing effect). Finally, we report the first time-resolved results obtained on graphite, where the electron-phonon coupling dynamics is observed, showing an overall temporal resolution in the sub-500 fs regime. The successful implementation of this configuration opens the way to directly probe structural dynamics of low-dimensional systems in the sub-picosecond regime, with pulsed electrons. PMID:28713841

Quantitative Analysis of Electron Beam Damage in Organic Thin Films

PubMed Central

2017-01-01

In transmission electron microscopy (TEM) the interaction of an electron beam with polymers such as P3HT:PCBM photovoltaic nanocomposites results in electron beam damage, which is the most important factor limiting acquisition of structural or chemical data at high spatial resolution. Beam effects can vary depending on parameters such as electron dose rate, temperature during imaging, and the presence of water and oxygen in the sample. Furthermore, beam damage will occur at different length scales. To assess beam damage at the angstrom scale, we followed the intensity of P3HT and PCBM diffraction rings as a function of accumulated electron dose by acquiring dose series and varying the electron dose rate, sample preparation, and the temperature during acquisition. From this, we calculated a critical dose for diffraction experiments. In imaging mode, thin film deformation was assessed using the normalized cross-correlation coefficient, while mass loss was determined via changes in average intensity and standard deviation, also varying electron dose rate, sample preparation, and temperature during acquisition. The understanding of beam damage and the determination of critical electron doses provides a framework for future experiments to maximize the information content during the acquisition of images and diffraction patterns with (cryogenic) transmission electron microscopy. PMID:28553431

Development of splitting convergent beam electron diffraction (SCBED).

PubMed

Houdellier, Florent; Röder, Falk; Snoeck, Etienne

2015-12-01

Using a combination of condenser electrostatic biprism with dedicated electron optic conditions for sample illumination, we were able to split a convergent beam electron probe focused on the sample in two half focused probes without introducing any tilt between them. As a consequence, a combined convergent beam electron diffraction pattern is obtained in the back focal plane of the objective lens arising from two different sample areas, which could be analyzed in a single pattern. This splitting convergent beam electron diffraction (SCBED) pattern has been tested first on a well-characterized test sample of Si/SiGe multilayers epitaxially grown on a Si substrate. The SCBED pattern contains information from the strained area, which exhibits HOLZ lines broadening induced by surface relaxation, with fine HOLZ lines observed in the unstrained reference part of the sample. These patterns have been analyzed quantitatively using both parts of the SCBED transmitted disk. The fine HOLZ line positions are used to determine the precise acceleration voltage of the microscope while the perturbed HOLZ rocking curves in the stained area are compared to dynamical simulated ones. The combination of these two information leads to a precise evaluation of the sample strain state. Finally, several SCBED setups are proposed to tackle fundamental physics questions as well as applied materials science ones and demonstrate how SCBED has the potential to greatly expand the range of applications of electron diffraction and electron holography. Copyright © 2015 Elsevier B.V. All rights reserved.

Zemax simulations describing collective effects in transition and diffraction radiation.

PubMed

Bisesto, F G; Castellano, M; Chiadroni, E; Cianchi, A

2018-02-19

Transition and diffraction radiation from charged particles is commonly used for diagnostics purposes in accelerator facilities as well as THz sources for spectroscopy applications. Therefore, an accurate analysis of the emission process and the transport optics is crucial to properly characterize the source and precisely retrieve beam parameters. In this regard, we have developed a new algorithm, based on Zemax, to simulate both transition and diffraction radiation as generated by relativistic electron bunches, therefore considering collective effects. In particular, unlike other previous works, we take into account electron beam physical size and transverse momentum, reproducing some effects visible on the produced radiation, not observable in a single electron analysis. The simulation results have been compared with two experiments showing an excellent agreement.

On the Use of Dynamical Diffraction Theory To Refine Crystal Structure from Electron Diffraction Data: Application to KLa5O5(VO4)2, a Material with Promising Luminescent Properties.

PubMed

Colmont, Marie; Palatinus, Lukas; Huvé, Marielle; Kabbour, Houria; Saitzek, Sébastien; Djelal, Nora; Roussel, Pascal

2016-03-07

A new lanthanum oxide, KLa5O5(VO4)2, was synthesized using a flux growth technique that involved solid-state reaction under an air atmosphere at 900 °C. The crystal structure was solved and refined using an innovative approach recently established and based on three-dimensional (3D) electron diffraction data, using precession of the electron beam and then validated against Rietveld refinement and denisty functional theory (DFT) calculations. It crystallizes in a monoclinic unit cell with space group C2/m and has unit cell parameters of a = 20.2282(14) Å, b = 5.8639(4) Å, c = 12.6060(9) Å, and β = 117.64(1)°. Its structure is built on Cresnel-like two-dimensional (2D) units (La5O5) of 4*3 (OLa4) tetrahedra, which run parallel to (001) plane, being surrounded by isolated VO4 tetrahedra. Four isolated vanadate groups create channels that host K(+) ions. Substitution of K(+) cations by another alkali metal is possible, going from lithium to rubidium. Li substitution led to a similar phase with a primitive monoclinic unit cell. A complementary selected area electron diffraction (SAED) study highlighted diffuse streaks associated with stacking faults observed on high-resolution electron microscopy (HREM) images of the lithium compound. Finally, preliminary catalytic tests for ethanol oxidation are reported, as well as luminescence evidence. This paper also describes how solid-state chemists can take advantages of recent progresses in electron crystallography, assisted by DFT calculations and powder X-ray diffraction (PXRD) refinements, to propose new structural types with potential applications to the physicist community.

Strain analysis from nano-beam electron diffraction: Influence of specimen tilt and beam convergence.

PubMed

Grieb, Tim; Krause, Florian F; Schowalter, Marco; Zillmann, Dennis; Sellin, Roman; Müller-Caspary, Knut; Mahr, Christoph; Mehrtens, Thorsten; Bimberg, Dieter; Rosenauer, Andreas

2018-07-01

Strain analyses from experimental series of nano-beam electron diffraction (NBED) patterns in scanning transmission electron microscopy are performed for different specimen tilts. Simulations of NBED series are presented for which strain analysis gives results that are in accordance with experiment. This consequently allows to study the relation between measured strain and actual underlying strain. A two-tilt method which can be seen as lowest-order electron beam precession is suggested and experimentally implemented. Strain determination from NBED series with increasing beam convergence is performed in combination with the experimental realization of a probe-forming aperture with a cross inside. It is shown that using standard evaluation techniques, the influence of beam convergence on spatial resolution is lower than the influence of sharp rings around the diffraction disc which occur at interfaces and which are caused by the tails of the intensity distribution of the electron probe. Copyright © 2018 Elsevier B.V. All rights reserved.

Applications of the diffraction and interference of light and electronic waves

NASA Astrophysics Data System (ADS)

Bahrim, Cristian; Lanning, Robert

2010-10-01

As part of a NSF sponsored program, called STAIRSTEP, at Lamar University we work on improving the basic knowledge of our physics majors in topics with broader impact in various areas of science and engineering [1]. The purpose is to facilitate a deeper understanding of some fundamental concepts in the field of optics through hands-on experience [2]. We choose to study the interference/diffraction of light and matter waves, because of its fundamental importance in physics with many applications. We target multiple goals in our field of study such as to understand the formation of electronic waves (wave packets) and their interaction with atoms in crystals (electron diffraction); the Fourier analysis of light with applications in spectroscopy, etc. We can show that a crystal lattice Fourier transforms the sinusoidal waves associated to free electrons fired toward the crystal. Our studies led to a simple and instructive recipe for discovering the arrangement of atoms in crystals from the analysis of the diffraction patterns produced by radiation or by electrons transmitted through crystals. [1] Doerschuk P. et al., 39th ASEE/IEEE Frontiers in Education Conference, San Antonio 2009, M3F-1. [2] Bahrim C, Innovation 2006 -- World Innovations in Engineering Education and Research, Chapter 17, iNEER Innovation Series, ISBN 0-9741252-5-3.

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.

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

NASA Astrophysics Data System (ADS)

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

2018-04-01

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

Electron crystallography with the EIGER detector

PubMed Central

Tinti, Gemma; Fröjdh, Erik; van Genderen, Eric; Gruene, Tim; Schmitt, Bernd; de Winter, D. A. Matthijs; Weckhuysen, Bert M.; Abrahams, Jan Pieter

2018-01-01

Electron crystallography is a discipline that currently attracts much attention as method for inorganic, organic and macromolecular structure solution. EIGER, a direct-detection hybrid pixel detector developed at the Paul Scherrer Institut, Switzerland, has been tested for electron diffraction in a transmission electron microscope. EIGER features a pixel pitch of 75 × 75 µm2, frame rates up to 23 kHz and a dead time between frames as low as 3 µs. Cluster size and modulation transfer functions of the detector at 100, 200 and 300 keV electron energies are reported and the data quality is demonstrated by structure determination of a SAPO-34 zeotype from electron diffraction data. PMID:29765609

In situ TEM observation of alpha-particle induced annealing of radiation damage in Durango apatite.

PubMed

Li, Weixing; Shen, Yahui; Zhou, Yueqing; Nan, Shuai; Chen, Chien-Hung; Ewing, Rodney C

2017-10-26

A major issue in thermochronology and U-Th-Pb dating is the effect of radiation damage, created by α-recoils from α-decay events, on the diffusion of radiogenic elements (e.g., He and Pb) in host mineral. Up until now, thermal events have been considered as the only source of energy for the recovery of radiation-damage. However, irradiation, such as from the α-particle of the α-decay event, can itself induce damage recovery. Quantification of radiation-induced recovery caused by α-particles during α-decay events has not been possible, as the recovery process at the atomic-scale has been difficult to observe. Here we present details of the dynamics of the amorphous-to-crystalline transition process during α-particle irradiations using in situ transmission electron microscopy (TEM) and consecutive ion-irradiations: 1 MeV Kr 2+ (simulating α-recoil damage), followed by 400 keV He + (simulating α-particle annealing). Upon the He + irradiation, partial recrystallization of the original, fully-amorphous Durango apatite was clearly evident and quantified based on the gradual appearance of new crystalline domains in TEM images and new diffraction maxima in selected area electron diffraction patterns. Thus, α-particle induced annealing occurs and must be considered in models of α-decay event damage and its effect on the diffusion of radiogenic elements in geochronology and thermochronology.

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

Kanel, S. R.; Clement, T. P.; Barnett, M. O.

Synthetic nano-scale hydroxyapatite (NHA) was prepared and characterized using X-ray diffraction (XRD) and scanning electron microscopy (SEM) methods. The XRD data confirmed that the crystalline structure and chemical composition of NHA correspond to Ca 5 OH(PO 4 ) 3 . The SEM data confirmed the size of NHA to be less than 50 nm. A two-dimensional physical model packed with saturated porous media was used to study the transport characteristics of NHA under constant flow conditions. The data show that the transport patterns of NHA were almost identical to tracer transport patterns. This result indicates that the NHA material can movemore » with water like a tracer, and its movement was neither retarded nor influenced by any physicochemical interactions and/or density effects. We have also tested the reactivity of NHA with 1 mg/L hexavalent uranium (U(VI)) and found that complete removal of U(VI) is possible using 0.5 g/L NHA at pH 5 to 6. Our results demonstrate that NHA has the potential to be injected as a dilute slurry for in situ treatment of U(VI)-contaminated groundwater systems.« less

Non-destructive detection of cross-sectional strain and defect structure in an individual Ag five-fold twinned nanowire by 3D electron diffraction mapping.

PubMed

Fu, Xin; Yuan, Jun

2017-07-24

Coherent x-ray diffraction investigations on Ag five-fold twinned nanowires (FTNWs) have drawn controversial conclusions concerning whether the intrinsic 7.35° angular gap could be compensated homogeneously through phase transformation or inhomogeneously by forming disclination strain field. In those studies, the x-ray techniques only provided an ensemble average of the structural information from all the Ag nanowires. Here, using three-dimensional (3D) electron diffraction mapping approach, we non-destructively explore the cross-sectional strain and the related strain-relief defect structures of an individual Ag FTNW with diameter about 30 nm. The quantitative analysis of the fine structure of intensity distribution combining with kinematic electron diffraction simulation confirms that for such a Ag FTNW, the intrinsic 7.35° angular deficiency results in an inhomogeneous strain field within each single crystalline segment consistent with the disclination model of stress-relief. Moreover, the five crystalline segments are found to be strained differently. Modeling analysis in combination with system energy calculation further indicates that the elastic strain energy within some crystalline segments, could be partially relieved by the creation of stacking fault layers near the twin boundaries. Our study demonstrates that 3D electron diffraction mapping is a powerful tool for the cross-sectional strain analysis of complex 1D nanostructures.

In situ investigation of deformation mechanisms in magnesium-based metal matrix composites

NASA Astrophysics Data System (ADS)

Farkas, Gergely; Choe, Heeman; Máthis, Kristián; Száraz, Zoltán; Noh, Yoonsook; Trojanová, Zuzanka; Minárik, Peter

2015-07-01

We studied the effect of short fibers on the mechanical properties of a magnesium alloy. In particular, deformation mechanisms in a Mg-Al-Sr alloy reinforced with short alumina fibers were studied in situ using neutron diffraction and acoustic emission methods. The fibers' plane orientation with respect to the loading axis was found to be a key parameter, which influences the acting deformation processes, such as twinning or dislocation slip. Furthermore, the twinning activity was much more significant in samples with parallel fiber plane orientation, which was confirmed by both acoustic emission and electron backscattering diffraction results. Neutron diffraction was also used to assist in analyzing the acoustic emission and electron backscattering diffraction results. The simultaneous application of the two in situ methods, neutron diffraction and acoustic emission, was found to be beneficial for obtaining complementary datasets about the twinning and dislocation slip in the magnesium alloys and composites used in this study.

Transmission Electron Microscopy of Single Wall Carbon Nanotube/Polymer Nanocomposites: A First-Principles Study

NASA Technical Reports Server (NTRS)

Sola, Francisco; Xia, Zhenhai; Lebrion-Colon, Marisabel; Meador, Michael A.

2012-01-01

The physics of HRTEM image formation and electron diffraction of SWCNT in a polymer matrix were investigated theoretically on the basis of the multislice method, and the optics of a FEG Super TWIN Philips CM 200 TEM operated at 80 kV. The effect of nanocomposite thickness on both image contrast and typical electron diffraction reflections of nanofillers were explored. The implications of the results on the experimental applicability to study dispersion, chirality and diameter of nanofillers are discussed.

Diffracted diffraction radiation and its application to beam diagnostics

NASA Astrophysics Data System (ADS)

Goponov, Yu. A.; Shatokhin, R. A.; Sumitani, K.; Syshchenko, V. V.; Takabayashi, Y.; Vnukov, I. E.

2018-03-01

We present theoretical considerations for diffracted diffraction radiation and also propose an application of this process to diagnosing ultra-relativistic electron (positron) beams for the first time. Diffraction radiation is produced when relativistic particles move near a target. If the target is a crystal or X-ray mirror, diffraction radiation in the X-ray region is expected to be diffracted at the Bragg angle and therefore be detectable. We present a scheme for applying this process to measurements of the beam angular spread, and consider how to conduct a proof-of-principle experiment for the proposed method.

In-Depth View of the Structure and Growth of SnO2 Nanowires and Nanobrushes.

PubMed

Stuckert, Erin P; Geiss, Roy H; Miller, Christopher J; Fisher, Ellen R

2016-08-31

Strategic application of an array of complementary imaging and diffraction techniques is critical to determine accurate structural information on nanomaterials, especially when also seeking to elucidate structure-property relationships and their effects on gas sensors. In this work, SnO2 nanowires and nanobrushes grown via chemical vapor deposition (CVD) displayed the same tetragonal SnO2 structure as revealed via powder X-ray diffraction bulk crystallinity data. Additional characterization using a range of electron microscopy imaging and diffraction techniques, however, revealed important structure and morphology distinctions between the nanomaterials. Tailoring scanning transmission electron microscopy (STEM) modes combined with transmission electron backscatter diffraction (t-EBSD) techniques afforded a more detailed view of the SnO2 nanostructures. Indeed, upon deeper analysis of individual wires and brushes, we discovered that, despite a similar bulk structure, wires and brushes grew with different crystal faces and lattice spacings. Had we not utilized multiple STEM diffraction modes in conjunction with t-EBSD, differences in orientation related to bristle density would have been overlooked. Thus, it is only through a methodical combination of several structural analysis techniques that precise structural information can be reliably obtained.

Diffraction efficiency of plasmonic gratings fabricated by electron beam lithography using a silver halide film

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

Sudheer,, E-mail: sudheer@rrcat.gov.in, E-mail: sudheer.rrcat@gmail.com; Tiwari, P.; Srivastava, Himanshu

2016-07-28

The silver nanoparticle surface relief gratings of ∼10 μm period are fabricated using electron beam lithography on the silver halide film substrate. Morphological characterization of the gratings shows that the period, the shape, and the relief depth in the gratings are mainly dependent on the number of lines per frame, the spot size, and the accelerating voltage of electron beam raster in the SEM. Optical absorption of the silver nanoparticle gratings provides a broad localized surface plasmon resonance peak in the visible region, whereas the intensity of the peaks depends on the number density of silver nanoparticles in the gratings. Themore » maximum efficiency of ∼7.2% for first order diffraction is observed for the grating fabricated at 15 keV. The efficiency is peaking at 560 nm with ∼380 nm bandwidth. The measured profiles of the diffraction efficiency for the gratings are found in close agreement with the Raman-Nath diffraction theory. This technique provides a simple and efficient method for the fabrication of plasmonic nanoparticle grating structures with high diffraction efficiency having broad wavelength tuning.« less

Robust diamond-like Fe-Si network in the zero-strain Na xFeSiO 4 cathode

DOE PAGES

Ye, Zhuo; Zhao, Xin; Li, Shouding; ...

2016-07-14

Sodium orthosilicates Na 2 MSiO 4 ( M denotes transition metals) have attracted much attention due to the possibility of exchanging two electrons per formula unit. In this work, we report a group of sodium iron orthosilicates Na 2FeSiO 4. Their crystal structures are characterized by a diamond-like Fe-Si network. The Fe-Si network is quite robust against the charge/discharge process, which explains the high structural stability observed in experiment. Furthermore, using the density functional theory within the GGA + U framework and X-ray diffraction studies, the crystal structures and structural stabilities during the sodium extraction/re-insertion process are systematically investigated.

Neutron Diffraction Studies of Some Rare Earth-Transition Metal Deuterides.

DTIC Science & Technology

1986-05-01

RD-A168 M NEUTRON DIFFRACTION STUDIES OF SONE RARE EARTH-TRANSITION METAL DEUTERIDES(U) MISSOURI UNIV-ROLLR MATERIALS RESEARCH CENTER N J JAMES MY 86...REPORT William J. James OTtO -il May 1986 ZLECTEJU U. S. Army Research Office DAAG29-83-K-01 59 ".;’ Graduate Center for Materials Research ...9. PERFORMING ORGANIZATION NAME AND ADDRESS 10. PROGRAM ELEMENT, PROJECT. TASK AREA & WORK UNIT NUMBERS 2* Graduate Center for Materials Research

High current table-top setup for femtosecond gas electron diffraction.

PubMed

Zandi, Omid; Wilkin, Kyle J; Xiong, Yanwei; Centurion, Martin

2017-07-01

We have constructed an experimental setup for gas phase electron diffraction with femtosecond resolution and a high average beam current. While gas electron diffraction has been successful at determining molecular structures, it has been a challenge to reach femtosecond resolution while maintaining sufficient beam current to retrieve structures with high spatial resolution. The main challenges are the Coulomb force that leads to broadening of the electron pulses and the temporal blurring that results from the velocity mismatch between the laser and electron pulses as they traverse the sample. We present here a device that uses pulse compression to overcome the Coulomb broadening and deliver femtosecond electron pulses on a gas target. The velocity mismatch can be compensated using laser pulses with a tilted intensity front to excite the sample. The temporal resolution of the setup was determined with a streak camera to be better than 400 fs for pulses with up to half a million electrons and a kinetic energy of 90 keV. The high charge per pulse, combined with a repetition rate of 5 kHz, results in an average beam current that is between one and two orders of magnitude higher than previously demonstrated.

High current table-top setup for femtosecond gas electron diffraction

DOE PAGES

Zandi, Omid; Wilkin, Kyle J.; Xiong, Yanwei; ...

2017-05-08

Here, we have constructed an experimental setup for gas phase electron diffraction with femtosecond resolution and a high average beam current. While gas electron diffraction has been successful at determining molecular structures, it has been a challenge to reach femtosecond resolution while maintaining sufficient beam current to retrieve structures with high spatial resolution. The main challenges are the Coulomb force that leads to broadening of the electron pulses and the temporal blurring that results from the velocity mismatch between the laser and electron pulses as they traverse the sample. We also present here a device that uses pulse compression tomore » overcome the Coulomb broadening and deliver femtosecond electron pulses on a gas target. The velocity mismatch can be compensated using laser pulses with a tilted intensity front to excite the sample. The temporal resolution of the setup was determined with a streak camera to be better than 400 fs for pulses with up to half a million electrons and a kinetic energy of 90 keV. Finally, the high charge per pulse, combined with a repetition rate of 5 kHz, results in an average beam current that is between one and two orders of magnitude higher than previously demonstrated.« less

Measuring the Shock Stage of Asteroid Regolith Grains by Electron Back-Scattered Diffraction

NASA Technical Reports Server (NTRS)

Zolensky, Michael; Martinez, James; Sitzman, Scott; Mikouchi, Takashi; Hagiya, Kenji; Ohsumi, Kazumasa; Terada, Yasuko; Yagi, Naoto; Komatsu, Mutsumi; Ozawa, Hikaru;

Investigating the Effects of Low Temperature Annealing of Amorphous Corrosion Resistant Alloys.

DTIC Science & Technology

1980-11-01

Ray Diffraction.................................................... 6 Differential Scanning Calorimetry....................................... 9...17 LIST OF FIGURES Figure 1. X- Ray Diffraction Results From Fe32Ni 36Cr 4P 2 B Annealed for One Hour at...Various Temperatures (Cr Ka Radiation) ................................. 7 Figure 2. X- Ray Diffraction Results From FeU2NiaeCr14SieB Annealed for One

Individual analysis of inter and intragrain defects in electrically characterized polycrystalline silicon nanowire TFTs by multicomponent dark-field imaging based on nanobeam electron diffraction two-dimensional mapping

NASA Astrophysics Data System (ADS)

Asano, Takanori; Takaishi, Riichiro; Oda, Minoru; Sakuma, Kiwamu; Saitoh, Masumi; Tanaka, Hiroki

2018-04-01

We visualize the grain structures for individual nanosized thin film transistors (TFTs), which are electrically characterized, with an improved data processing technique for the dark-field image reconstruction of nanobeam electron diffraction maps. Our individual crystal analysis gives the one-to-one correspondence of TFTs with different grain boundary structures, such as random and coherent boundaries, to the characteristic degradations of ON-current and threshold voltage. Furthermore, the local crystalline uniformity inside a single grain is detected as the difference in diffraction intensity distribution.

Mapping 180° polar domains using electron backscatter diffraction and dynamical scattering simulations

DOE PAGES

Burch, Matthew J.; Fancher, Chris M.; Patala, Srikanth; ...

2016-11-18

A novel technique, which directly and nondestructively maps polar domains using electron backscatter diffraction (EBSD) is described and demonstrated. Through dynamical diffraction simulations and quantitative comparison to experimental EBSD patterns, the absolute orientation of a non-centrosymmetric crystal can be determined. With this information, the polar domains of a material can be mapped. The technique is demonstrated by mapping the non-ferroelastic, or 180°, ferroelectric domains in periodically poled LiNbO 3 single crystals. Furthermore, the authors demonstrate the possibility of mapping polarity using this technique in other polar materials system.

Spectroscopic evidence for uranium bearing precipitates in vadose zone sediments at the Hanford 300-area site

USGS Publications Warehouse

Arai, Y.; Marcus, M.A.; Tamura, N.; Davis, J.A.; Zachara, J.M.

2007-01-01

Uranium (U) solid-state speciation in vadose zone sediments collected beneath the former North Process Pond (NPP) in the 300 Area of the Hanford site (Washington) was investigated using multi-scale techniques. In 30 day batch experiments, only a small fraction of total U (???7.4%) was released to artificial groundwater solutions equilibrated with 1% pCO2. Synchrotron-based micro-X-ray fluorescence spectroscopy analyses showed that U was distributed among at least two types of species: (i) U discrete grains associated with Cu and (ii) areas with intermediate U concentrations on grains and grain coatings. Metatorbernite (Cu[UO2]2[PO 4]2??8H2O) and uranophane (Ca[UO 2]2[SiO3(OH)]2?? 5H 2O) at some U discrete grains, and muscovite at U intermediate concentration areas, were identified in synchrotron-based micro-X-ray diffraction. Scanning electron microscopy/energy dispersive X-ray analyses revealed 8-10 ??m size metatorbernite particles that were embedded in C-, Al-, and Si-rich coatings on quartz and albite grains. In ??- and bulk-X-ray absorption structure (??-XAS and XAS) spectroscopy analyses, the structure of metatorbernite with additional U-C and U-U coordination environments was consistently observed at U discrete grains with high U concentrations. The consistency of the ??- and bulk-XAS analyses suggests that metatorbernite may comprise a significant fraction of the total U in the sample. The entrapped, micrometer-sized metatorbernite particles in C-, Al-, and Si-rich coatings, along with the more soluble precipitated uranyl carbonates and uranophane, likely control the long-term release of U to water associated with the vadose zone sediments. ?? 2007 American Chemical Society.

Space charge effects in ultrafast electron diffraction and imaging

NASA Astrophysics Data System (ADS)

Tao, Zhensheng; Zhang, He; Duxbury, P. M.; Berz, Martin; Ruan, Chong-Yu

2012-02-01

Understanding space charge effects is central for the development of high-brightness ultrafast electron diffraction and microscopy techniques for imaging material transformation with atomic scale detail at the fs to ps timescales. We present methods and results for direct ultrafast photoelectron beam characterization employing a shadow projection imaging technique to investigate the generation of ultrafast, non-uniform, intense photoelectron pulses in a dc photo-gun geometry. Combined with N-particle simulations and an analytical Gaussian model, we elucidate three essential space-charge-led features: the pulse lengthening following a power-law scaling, the broadening of the initial energy distribution, and the virtual cathode threshold. The impacts of these space charge effects on the performance of the next generation high-brightness ultrafast electron diffraction and imaging systems are evaluated.

Defect ordering in YBa 2Cu 3O 6.5 and YBa 2Cu 3O 6.6: Synthesis and characterization by neutron and electron diffraction

NASA Astrophysics Data System (ADS)

Lin, Y. P.; Greedan, J. E.; O'Reilly, A. H.; Reimers, J. N.; Stager, C. V.; Post, M. L.

1990-02-01

Polycrystalline samples of YBa 2Cu 3O 6.5 and YBa 2Cu 3O 6.6 were prepared by oxygen titration of YBa 2 Cu 3O 6.0 at 450°C followed by slow cooling to room temperature. Both samples showed evidence for the a' = 2a supercell in individual grains by electron diffraction as reported previously. In addition the superlattice was observed in neutron powder diffraction indicating that the bulk material is also well ordered. In this study the YBa 2Cu 3O 6.6 phase showed longer correlation lengths for ordering along both a* and b* than YBa 2Cu 3O 6.5. For the former compound the powder-averaged, sample-averaged a* correlation distance is 26A˚from neutron diffraction. Analysis of electron diffraction profiles on selected single crystals give correlation lengths along a*, b*, and c* of 100, 200, and 50A˚, respectively. Dark field imaging discloses the presence of striped, ordered domains elongated along b* with a distribution of sizes. Both neutron diffraction and dark field imaging indicate that the volume fraction of the ordered domains is about 50%. A correlation is noted between the Meissner Effect and the extent of defect ordering in the bulk samples of the two phases.

Ultrafast molecular processes mapped by femtosecond x-ray diffraction

NASA Astrophysics Data System (ADS)

Elsaesser, Thomas

2012-02-01

X-ray diffraction with a femtosecond time resolution allows for mapping photoinduced structural dynamics on the length scale of a chemical bond and in the time domain of atomic and molecular motion. In a pump-probe approach, a femtosecond excitation pulse induces structural changes which are probed by diffracting a femtosecond hard x-ray pulse from the excited sample. The transient angular positions and intensities of diffraction peaks give insight into the momentary atomic or molecular positions and into the distribution of electronic charge density. The simultaneous measurement of changes on different diffraction peaks is essential for determining atom positions and charge density maps with high accuracy. Recent progress in the generation of ultrashort hard x-ray pulses (Cu Kα, wavelength λ=0.154 nm) in laser-driven plasma sources has led to the implementation of the powder diffraction and the rotating crystal method with a time resolution of 100 fs. In this contribution, we report new results from powder diffraction studies of molecular materials. A first series of experiments gives evidence of a so far unknown concerted transfer of electrons and protons in ammonium sulfate [(NH4)2SO4], a centrosymmetric structure. Charge transfer from the sulfate groups results in the sub-100 fs generation of a confined electron channel along the c-axis of the unit cell which is stabilized by transferring protons from the adjacent ammonium groups into the channel. Time-dependent charge density maps display a periodic modulation of the channel's charge density by low-frequency lattice motions with a concerted electron and proton motion between the channel and the initial proton binding site. A second study addresses atomic rearrangements and charge dislocations in the non-centrosymmetric potassium dihydrogen phosphate [KH2PO4, KDP]. Photoexcitation generates coherent low-frequency motions along the LO and TO phonon coordinates, leaving the average atomic positions unchanged. The time-dependent maps of electron density demonstrate a concomitant oscillatory relocation of electronic charge with a spatial amplitude of the order of a chemical bond length, two orders of magnitude larger than the vibrational amplitudes. The coherent phonon motions drive the charge relocation, similar to a soft mode driven phase transition between the ferro- and paraelectric phase of KDP.

The commensurate-to-incommensurate phase transition of an organic monolayer: A high resolution LEED analysis of the superstructures of NTCDA on Ag(1 1 1)

NASA Astrophysics Data System (ADS)

Kilian, L.; Stahl, U.; Kossev, I.; Sokolowski, M.; Fink, R.; Umbach, E.

2008-07-01

The structural order of 1,4,9,10-naphthalene-tetracarboxylicacid-dianhydride (NTCDA) monolayers on Ag(1 1 1) has been investigated by spot profile analysis low energy electron diffraction (SPA-LEED). For increasing coverage, we find a sequence of three highly ordered structures: a commensurate structure (α), a uniaxially incommensurate structure (α 2), and an incommensurate structure (β) with coverages of 0.9 ML, 0.95 ML, and 1 (saturated) monolayer (ML), respectively. In the high coverage regime, the structures coexist and a coverage increase causes a change of their relative fractions. The α and β structures were known before [U. Stahl, D. Gador, A. Soukopp, R. Fink, E. Umbach, Surf. Sci. 414 (1998) 423], but the β structure was proposed as commensurate, since its very small misfit with respect to a commensurate structure could not be resolved. This misfit leads to a periodic modulation, causing additional Moiré satellites in the diffraction pattern. This finding demonstrates the importance of high resolution methods for the geometry determination of large organic adsorbates.

Acquisition parameters optimization of a transmission electron forward scatter diffraction system in a cold-field emission scanning electron microscope for nanomaterials characterization.

PubMed

Brodusch, Nicolas; Demers, Hendrix; Trudeau, Michel; Gauvin, Raynald

2013-01-01

Transmission electron forward scatter diffraction (t-EFSD) is a new technique providing crystallographic information with high resolution on thin specimens by using a conventional electron backscatter diffraction (EBSD) system in a scanning electron microscope. In this study, the impact of tilt angle, working distance, and detector distance on the Kikuchi pattern quality were investigated in a cold-field emission scanning electron microscope (CFE-SEM). We demonstrated that t-EFSD is applicable for tilt angles ranging from -20° to -40°. Working distance (WD) should be optimized for each material by choosing the WD for which the EBSD camera screen illumination is the highest, as the number of detected electrons on the screen is directly dependent on the scattering angle. To take advantage of the best performances of the CFE-SEM, the EBSD camera should be close to the sample and oriented towards the bottom to increase forward scattered electron collection efficiency. However, specimen chamber cluttering and beam/mechanical drift are important limitations in the CFE-SEM used in this work. Finally, the importance of t-EFSD in materials science characterization was illustrated through three examples of phase identification and orientation mapping. © Wiley Periodicals, Inc.

Visualization of the ultrafast structural phase transitions in warm dense matter

NASA Astrophysics Data System (ADS)

Mo, Mianzhen

2017-10-01

It is still a great challenge to obtain real-time atomistic-scale information on the structural phase transitions that lead to warm dense matter state. Recent advances in ultrafast electron diffraction (UED) techniques have opened up exciting prospects to unravel the mechanisms of solid-liquid phase transitions under these extreme non-equilibrium conditions. Here we report on precise measurements of melt time dependency on laser excitation energy density that resolve for the first time the transition from heterogeneous to homogeneous melting. This transition appears in both polycrystalline and single-crystal gold nanofilms with distinct measurable differences. These results test predictions from molecular-dynamics simulations with different interatomic potential models. These data further deliver accurate structure factor data to large wavenumbers that allow us to constrain electron-ion equilibration constants. Our results demonstrate electron-phonon coupling strength much weaker than DFT calculations, and contrary to previous results, provide evidence for bond softening. This work is supported by DOE Office of Science, Fusion Energy Science under FWP 100182, and the DOE BES Accelerator and Detector R&D program.

Magnetic coupling of Fe-porphyrin molecules adsorbed on clean and c(2×2) oxygen-reconstructed Co(100) investigated by spin-polarized photoemission spectroscopy

NASA Astrophysics Data System (ADS)

Weber, A. P.; Caruso, A. N.; Vescovo, E.; Ali, Md. E.; Tarafder, K.; Janjua, S. Z.; Sadowski, J. T.; Oppeneer, P. M.

2013-05-01

The spin-polarized electronic structure of iron octaethylporphyrin (FeOEP) molecules adsorbed on a pristine and on a c(2×2) oxygen-reconstructed Co(100) surface has been analyzed by means of spin-polarized photoemission spectroscopy (SPPES) and first-principles density functional theory with the on-site Coulomb repulsion U term (DFT+U) calculations with and without Van der Waals corrections. The aim is to examine the magnetic exchange mechanism between the FeOEP molecules and the Co(100) substrate in the presence or absence of the oxygen mediator. The results demonstrate that the magnetic coupling from the ferromagnetic substrate to the adsorbed FeOEP molecules is ferromagnetic, whereas, the coupling is antiferromagnetic for the FeOEP on the c(2×2)O/Co(100) system. Spin-resolved partial densities of states extracted from ab initio DFT+U modeling are in fairly good comparison with the electronic spectral densities seen in angle-integrated SPPES energy dispersion curves for submonolayer coverages of FeOEP. Through combined analysis of these spectra and theoretical results, we determine that hybridization of 2p orbitals of N and O with Co 3d orbitals facilitates indirect magnetic exchange interactions between Fe and Co, whereas, a direct Fe-Co interaction involving the Fe dz2 orbital is also found for FeOEP on Co. It is observed through SPPES that the spin polarization of the photoemission-visible molecular overlayers decreases to zero as coverage is increased beyond the submonolayer regime, indicating that only interfacial magnetic coupling is at work. Microspot low-energy electron diffraction and low-energy electron microscopy were performed to characterize the physical order of the molecular coverage, revealing that FeOEP structural domains are orders of magnitude greater in size on c(2×2)O/Co(100) than on clean Co(100), which coincides with reduced scattering from the disorder and sharper features seen in SPPES.

Measurements of Auger Electron Diffraction Using a 180° Deflection Toroidal Analyzer

NASA Astrophysics Data System (ADS)

Shiraki, Susumu; Ishii, Hideshi; Nihei, Yoshimasa; Owari, Masanori

A 180° deflection toroidal analyzer is a novel electron spectrometer, which allows the simultaneous registration of the wide range of polar angles in a given azimuth of the sample. Therefore, measurements of photo- and Auger electron intensities over π steradians can be performed rapidly by azimuthal rotation of the sample. Using this analyzer, two-dimensional patterns of electron-beam-excited O KVV and Mg KVV Auger electron diffraction (AED) from a MgO(001) surface were measured in short acquisition times. The AED patterns obtained were compared with theoretical ones calculated by the multiple-scattering scheme. The agreement between experimental and theoretical data was good for both O KVV and Mg KVV transitions.

Single-crystal growth of C u4(OH) 6BrF and universal behavior in quantum spin liquid candidates synthetic barlowite and herbertsmithite

NASA Astrophysics Data System (ADS)

Pasco, C. M.; Trump, B. A.; Tran, Thao T.; Kelly, Z. A.; Hoffmann, C.; Heinmaa, I.; Stern, R.; McQueen, T. M.

2018-04-01

Synthetic barlowite, C u4(OH) 6BrF , has emerged as a new quantum spin liquid (QSL) host, containing kagomé layers of S =1 /2 C u2 + ions separated by interlayer C u2 + ions. Similar to synthetic herbertsmithite, ZnC u3(OH) 6C l2 , it has been reported that Z n2 + substitution for the interlayer C u2 + induces a QSL ground state. Here we report a scalable synthesis of single crystals of C u4(OH) 6BrF . Through x-ray, neutron, and electron diffraction measurements coupled with magic angle spinning 19F and 1H NMR spectroscopy, we resolve the previously reported positional disorder of the interlayer C u2 + ions and find that the structure is best described in the orthorhombic space group, Cmcm, with lattice parameters a =6.665 (13 )Å ,b =11.521 (2 )Å ,c =9.256 (18 )Å , and an ordered arrangement of interlayer C u2 + ions. Infrared spectroscopy measurements of the O—H and F—H stretching frequencies demonstrate that the orthorhombic symmetry persists upon substitution of Z n2 + for C u2 + . Specific heat and magnetic susceptibility measurements of Zn-substituted barlowite, Z nxC u4 -x(OH) 6BrF , reveal striking similarities with the behavior of Z nxC u4 -x(OH) 6C l2 . These parallels imply universal behavior of copper kagomé lattices even in the presence of small symmetry-breaking distortions. Thus, synthetic barlowite demonstrates universality of the physics of synthetic C u2 + kagomé minerals and furthers the development of real QSL states.

Highlighting material structure with transmission electron diffraction correlation coefficient maps.

PubMed

Kiss, Ákos K; Rauch, Edgar F; Lábár, János L

2016-04-01

Correlation coefficient maps are constructed by computing the differences between neighboring diffraction patterns collected in a transmission electron microscope in scanning mode. The maps are shown to highlight material structural features like grain boundaries, second phase particles or dislocations. The inclination of the inner crystal interfaces are directly deduced from the resulting contrast. Copyright © 2016 Elsevier B.V. All rights reserved.

Symposium LL: Nanowires--Synthesis Properties Assembly and Application

DTIC Science & Technology

2010-09-10

dedicated hard x - ray microscopy beamline is operated in partnership with the Advanced Photon Source to provide fluorescence, diffraction, and...characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X - ray diffraction (XRD) measurements, proving it to be...Investigation of Preferred Growth Direction of GaN Nanorods by Synchrotron X - ray Reciprocal Space Mapping. Yuri Sohn1, Sanghwa Lee1, Chinkyo Kim1 and Dong

Quantitative measurements of magnetic vortices using position resolved diffraction in Lorentz STEM

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

Zaluzec, N. J.

2002-03-05

A number of electron column techniques have been developed over the last forty years to permit visualization of magnetic fields in specimens. These include: Fresnel imaging, Differential Phase Contrast, Electron Holography and Lorentz STEM. In this work we have extended the LSTEM methodology using Position Resolved Diffraction (PRD) to quantitatively measure the in-plane electromagnetic fields of thin film materials. The experimental work reported herein has been carried out using the ANL AAEM HB603Z 300 kV FEG instrument 5. In this instrument, the electron optical column was operated in a zero field mode, at the specimen, where the objective lens ismore » turned off and the probe forming lens functions were reallocated to the C1, C2, and C3 lenses. Post specimen lenses (P1, P2, P3, P4) were used to magnify the transmitted electrons to a YAG screen, which was then optically transferred to a Hamamatsu ORCA ER CCD array. This CCD was interfaced to an EmiSpec Data Acquisition System and the data was subsequently transferred to an external computer system for detailed quantitative analysis. In Position Resolved Diffraction mode, we digitally step a focused electron probe across the region of interest of the specimen while at the same time recording the complete diffraction pattern at each point in the scan.« less

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.

Application of a real-space three-dimensional image reconstruction method in the structural analysis of noncrystalline biological macromolecules enveloped by water in coherent x-ray diffraction microscopy.

PubMed

Kodama, Wataru; Nakasako, Masayoshi

2011-08-01

Coherent x-ray diffraction microscopy is a novel technique in the structural analyses of particles that are difficult to crystallize, such as the biological particles composing living cells. As water is indispensable for maintaining particles in functional structures, sufficient hydration of targeted particles is required during sample preparation for diffraction microscopy experiments. However, the water enveloping particles also contributes significantly to the diffraction patterns and reduces the electron-density contrast of the sample particles. In this study, we propose a protocol for the structural analyses of particles in water by applying a three-dimensional reconstruction method in real space for the projection images phase-retrieved from diffraction patterns, together with a developed density modification technique. We examined the feasibility of the protocol through three simulations involving a protein molecule in a vacuum, and enveloped in either a droplet or a cube-shaped water. The simulations were carried out for the diffraction patterns in the reciprocal planes normal to the incident x-ray beam. This assumption and the simulation conditions corresponded to experiments using x-ray wavelengths of shorter than 0.03 Å. The analyses demonstrated that our protocol provided an interpretable electron-density map. Based on the results, we discuss the advantages and limitations of the proposed protocol and its practical application for experimental data. In particular, we examined the influence of Poisson noise in diffraction patterns on the reconstructed three-dimensional electron density in the proposed protocol.

Electromagnetic diffraction radiation of a subwavelength-hole array excited by an electron beam.

PubMed

Liu, Shenggang; Hu, Min; Zhang, Yaxin; Li, Yuebao; Zhong, Renbin

2009-09-01

This paper explores the physics of the electromagnetic diffraction radiation of a subwavelength holes array excited by a set of evanescent waves generated by a line charge of electron beam moving parallel to the array. Activated by a uniformly moving line charge, numerous physical phenomena occur such as the diffraction radiation on both sides of the array as well as the electromagnetic penetration or transmission below or above the cut-off through the holes. As a result the subwavelength holes array becomes a radiation array. Making use of the integral equation with relevant Green's functions, an analytical theory for such a radiation system is built up. The results of the numerical calculations based on the theory agree well with that obtained by the computer simulation. The relation among the effective surface plasmon wave, the electromagnetic penetration or transmission of the holes and the diffraction radiation is revealed. The energy dependence of and the influence of the hole thickness on the diffraction radiation and the electromagnetic penetration or transmission are investigated in detail. Therefore, a distinct diffraction radiation phenomenon is discovered.

Dark-field transmission electron microscopy and the Debye-Waller factor of graphene

PubMed Central

Hubbard, William A.; White, E. R.; Dawson, Ben; Lodge, M. S.; Ishigami, Masa; Regan, B. C.

2014-01-01

Graphene's structure bears on both the material's electronic properties and fundamental questions about long range order in two-dimensional crystals. We present an analytic calculation of selected area electron diffraction from multi-layer graphene and compare it with data from samples prepared by chemical vapor deposition and mechanical exfoliation. A single layer scatters only 0.5% of the incident electrons, so this kinematical calculation can be considered reliable for five or fewer layers. Dark-field transmission electron micrographs of multi-layer graphene illustrate how knowledge of the diffraction peak intensities can be applied for rapid mapping of thickness, stacking, and grain boundaries. The diffraction peak intensities also depend on the mean-square displacement of atoms from their ideal lattice locations, which is parameterized by a Debye-Waller factor. We measure the Debye-Waller factor of a suspended monolayer of exfoliated graphene and find a result consistent with an estimate based on the Debye model. For laboratory-scale graphene samples, finite size effects are sufficient to stabilize the graphene lattice against melting, indicating that ripples in the third dimension are not necessary. PMID:25242882

Extracting conformational structure information of benzene molecules via laser-induced electron diffraction

DOE PAGES

Ito, Yuta; Wang, Chuncheng; Le, Anh-Thu; ...

2016-05-01

Here, we have measured the angular distributions of high energy photoelectrons of benzene molecules generated by intense infrared femtosecond laser pulses. These electrons arise from the elastic collisions between the benzene ions with the previously tunnel-ionized electrons that have been driven back by the laser field. Theory shows that laser-free elastic differential cross sections (DCSs) can be extracted from these photoelectrons, and the DCS can be used to retrieve the bond lengths of gas-phase molecules similar to the conventional electron diffraction method. From our experimental results, we have obtained the C-C and C-H bond lengths of benzene with a spatialmore » resolution of about 10 pm. Our results demonstrate that laser induced electron diffraction (LIED) experiments can be carried out with the present-day ultrafast intense lasers already. Looking ahead, with aligned or oriented molecules, more complete spatial information of the molecule can be obtained from LIED, and applying LIED to probe photo-excited molecules, a “molecular movie” of the dynamic system may be created with sub-A°ngstrom spatial and few-ten femtosecond temporal resolutions.« less

Dark-field transmission electron microscopy and the Debye-Waller factor of graphene.

PubMed

Shevitski, Brian; Mecklenburg, Matthew; Hubbard, William A; White, E R; Dawson, Ben; Lodge, M S; Ishigami, Masa; Regan, B C

2013-01-15

Graphene's structure bears on both the material's electronic properties and fundamental questions about long range order in two-dimensional crystals. We present an analytic calculation of selected area electron diffraction from multi-layer graphene and compare it with data from samples prepared by chemical vapor deposition and mechanical exfoliation. A single layer scatters only 0.5% of the incident electrons, so this kinematical calculation can be considered reliable for five or fewer layers. Dark-field transmission electron micrographs of multi-layer graphene illustrate how knowledge of the diffraction peak intensities can be applied for rapid mapping of thickness, stacking, and grain boundaries. The diffraction peak intensities also depend on the mean-square displacement of atoms from their ideal lattice locations, which is parameterized by a Debye-Waller factor. We measure the Debye-Waller factor of a suspended monolayer of exfoliated graphene and find a result consistent with an estimate based on the Debye model. For laboratory-scale graphene samples, finite size effects are sufficient to stabilize the graphene lattice against melting, indicating that ripples in the third dimension are not necessary.

Flat ion milling: a powerful tool for preparation of cross-sections of lead-silver alloys.

PubMed

Brodusch, Nicolas; Boisvert, Sophie; Gauvin, Raynald

2013-06-01

While conventional mechanical and chemical polishing results in stress, deformation and polishing particles embedded on the surface, flat milling with Ar+ ions erodes the material with no mechanical artefacts. This flat milling process is presented as an alternative method to prepare a Pb-Ag alloy cross-section for scanning electron microscopy. The resulting surface is free of scratches with very little to no stress induced, so that electron diffraction and channelling contrast are possible. The results have shown that energy dispersive spectrometer (EDS) mapping, electron channelling contrast imaging and electron backscatter diffraction can be conducted with only one sample preparation step. Electron diffraction patterns acquired at 5 keV possessed very good pattern quality, highlighting an excellent surface condition. An orientation map was acquired at 20 keV with an indexing rate of 90.1%. An EDS map was performed at 5 keV, and Pb-Ag precipitates of sizes lower than 100 nm were observed. However, the drawback of the method is the generation of a noticeable surface topography resulting from the interaction of the ion beam with a polycrystalline and biphasic sample.

Facile green synthesis of zinc oxide nanoparticles using Ulva lactuca seaweed extract and evaluation of their photocatalytic, antibiofilm and insecticidal activity.

PubMed

Ishwarya, Ramachandran; Vaseeharan, Baskaralingam; Kalyani, Subramanian; Banumathi, Balan; Govindarajan, Marimuthu; Alharbi, Naiyf S; Kadaikunnan, Shine; Al-Anbr, Mohammed N; Khaled, Jamal M; Benelli, Giovanni

2018-01-01

The bioactivity of semiconductor nanocomplexes has been poorly studied in the field of pesticide science. In this research, the synthesis of zinc nanoparticles was accomplished through new effortless green chemistry process, using the Ulva lactuca seaweed extract as a reducing and capping agent. The production of U. lactuca-fabricated ZnO nanoparticles (Ul-ZnO Nps) was characterized by powder X-ray diffraction (XRD), UV-visible, Fourier transform infrared (FTIR) spectroscopy, selected area electron diffraction (SAED) analysis and transmission electron microscopy (TEM). The U. lactuca-fabricated ZnO NPs were tested for their photodegradative action against organic dyes, as well as for antibiofilm and larvicidal activities. The UV visible absorbance spectrum of Ul-ZnO NPs exhibited the absorbance band at 325nm and TEM highlighted average crystallite sizes of nanoparticles of 10-50nm. Methylene blue (MB) dye was efficiently corrupted under sunlight in presence of Ul-ZnO NPs. Excellent bactericidal activity was shown by the Ul-ZnO Nps on Gram positive (Bacillus licheniformis and Bacillus pumilis) and Gram negative (Escherichia coliand Proteus vulgaris) bacteria. High antibiofilm potential was noted under both dark and sunlight conditions. The impact of a single treatment with Ul-ZnO NPs on biofilm architecture was also analyzed by confocal laser scanning microscopy (CLSM) on both Gram positive and Gram negative bacteria. Moreover, Ul-ZnO NPs led to 100% mortality of Aedes aegypti fourth instar larvae at the concentration of 50μg/ml within 24h. The effects of ZnO nanoparticle-based treatment on mosquito larval morphology and histology were monitored. Overall, based on our results, we believe that the synthesis of multifunctional Ul-ZnO Nps using widely available seaweed products can be promoted as a potential eco-friendly option to chemical methods currently used for nanosynthesis of antimicrobials and insecticides. Copyright © 2017 Elsevier B.V. All rights reserved.

Predicting In-Situ X-ray Diffraction for the SrTiO3/Liquid Interface from First Principles

NASA Astrophysics Data System (ADS)

Letchworth-Weaver, Kendra; Gunceler, Deniz; Sundararaman, Ravishankar; Huang, Xin; Brock, Joel; Arias, T. A.

2013-03-01

Recent advances in experimental techniques, such as in-situ x-ray diffraction, allow researchers to probe the solid-liquid interface in electrochemical systems under operating conditions. These advances offer an unprecedented opportunity for theory to predict properties of electrode materials in aqueous environments and inform the design of energy conversion and storage devices. To compare with experiment, these theoretical studies require microscopic details of both the liquid and the electrode surface. Joint Density Functional Theory (JDFT), a computationally efficient alternative to molecular dynamics, couples a classical density-functional, which captures molecular structure of the liquid, to a quantum-mechanical functional for the electrode surface. We present a JDFT exploration of SrTiO3, which can catalyze solar-driven water splitting, in an electrochemical environment. We determine the geometry of the polar SrTiO3 surface and the equilibrium structure of the contacting liquid, as well as the influence of the liquid upon the electronic structure of the surface. We then predict the effect of the fluid environment on x-ray diffraction patterns and compare our predictions to in-situ measurements performed at the Cornell High Energy Synchrotron Source (CHESS). This material is based upon work supported by the Energy Materials Center at Cornell (EMC2), an Energy Frontier Research Center funded by the U.S. Department of Energy.

Ultra-high Resolution Coherent X-ray Imaging of Nano-Materials

NASA Astrophysics Data System (ADS)

Shapiro, David

A revolution is underway in the field of x-ray microscopy driven by the develop of experimental, theoretical and computational means of producing a complete description of coherent imaging systems from x-ray diffraction data. The methods being developed not only allow for full quantification and removal of all optical aberrations but also extension of the numerical aperture to the diffraction limit. One such method under intensive development is x-ray ptychography. This is a scanned probe method that reconstructs a scattering object and its illumination from coherent diffraction data. Within the first few years of development at the Advanced Light Source (ALS), Lawrence Berkeley National Laboratory, this method has already achieved the highest resolution x-ray images ever recorded in two, three and four dimensions. With the ability of x-rays to penetrate significantly more matter than electrons, their short wavelength and their sensitivity to chemical and magnetic states of matter, x-ray ptychography is set to revolutionize how we see the nano-scale world. In this presentation I will briefly describe the technical framework for how various methods work and will give a detailed account of a practical implementation at the ALS along with various scientific applications. The Advanced Light Source is supported by the Director, Office of Science, Office of Basic Energy Sciences, of the U.S. Department of Energy under Contract No. DE-AC02-05CH11231.

The behavior of single-crystal silicon to dynamic loading using in-situ X-ray diffraction and phase contrast imaging

NASA Astrophysics Data System (ADS)

Lee, Hae Ja; Xing, Zhou; Galtier, Eric; Arnold, Brice; Granados, Eduardo; Brown, Shaughnessy B.; Tavella, Franz; McBride, Emma; Fry, Alan; Nagler, Bob; Schropp, Andreas; Seiboth, Frank; Samberg, Dirk; Schroer, Christian; Gleason, Arianna E.; Higginbotham, Andrew

Hydrostatic and uniaxial compression studies have revealed that crystalline silicon undergoes phase transitions from a cubic diamond structure to a variety of phases including orthorhombic Imma phase, body-centered tetragonal phase, and a hexagonal primitive phase. The dynamic response of silicon at high pressure, however, is not well understood. Phase contrast imaging has proven to be a powerful tool for probing density changes caused by the shock propagation into a material. In order to characterize the elastic and phase transitions, we image shock waves in Si with high spatial resolution using the LCLS X-ray free electron laser and Matter in Extreme Conditions instrument. In this study, the long pulse optical laser with pseudo-flat top shape creates high pressures up to 60 GPa. We measure the crystal structure by observing X-ray diffraction orthogonal to the shock propagation direction over a range of pressures. We describe the capability of simultaneously performing phase contrast imaging and in situ X-ray diffraction during shock loading and discuss the dynamic response of Si in high-pressure phases Use of the Linac Coherent Light Source (LCLS), SLAC National Accelerator Laboratory, is supported by the U.S. Department of Energy, Office of Science, Office of Basic Energy Sciences under Contract No. DE-AC02-76SF00515. The MEC instrument is supported by.

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

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

Yun, Di, E-mail: diyun1979@xjtu.edu.cn; Xi'an Jiao Tong University, 28 Xian Ning West Road, Xi'an 710049; Mo, Kun

2015-12-15

U–Mo metallic alloys have been extensively used for the Reduced Enrichment for Research and Test Reactors (RERTR) program, which is now known as the Office of Material Management and Minimization under the Conversion Program. This fuel form has also recently been proposed as fast reactor metallic fuels in the recent DOE Ultra-high Burnup Fast Reactor project. In order to better understand the behavior of U–10Mo fuels within the fast reactor temperature regime, a series of annealing and characterization experiments have been performed. Annealing experiments were performed in situ at the Intermediate Voltage Electron Microscope (IVEM-Tandem) facility at Argonne National Laboratorymore » (ANL). An electro-polished U–10Mo alloy fuel specimen was annealed in situ up to 700 °C. At an elevated temperature of about 540 °C, the U–10Mo specimen underwent a relatively slow microstructure transition. Nano-sized grains were observed to emerge near the surface. At the end temperature of 700 °C, the near-surface microstructure had evolved to a nano-crystalline state. In order to clarify the nature of the observed microstructure, Laue diffraction and powder diffraction experiments were carried out at beam line 34-ID of the Advanced Photon Source (APS) at ANL. Phases present in the as-annealed specimen were identified with both Laue diffraction and powder diffraction techniques. The U–10Mo was found to recrystallize due to thermally-induced recrystallization driven by a high density of pre-existing dislocations. A separate in situ annealing experiment was carried out with a Focused Ion Beam processed (FIB) specimen. A similar microstructure transition occurred at a lower temperature of about 460 °C with a much faster transition rate compared to the electro-polished specimen. - Highlights: • TEM annealing experiments were performed in situ at the IVEM facility up to fast reactor temperature. • At 540 °C, the U-10Mo specimen underwent a slow microstructure transition where nano-sized grains were observed to emerge. • UO{sub 2} phase exists at the thin area of the as-annealed specimen whereas U-10Mo γ phase dominated at the thicker part. • Bcc γ U-10Mo recrystallized to become nano-meter sized crystallites near the specimen surface. • A separateannealing experiment was conducted with a FIB processed specimen where similar transition occurred at a lower temperature of 460 °C with a faster rate.« less

Soft-template synthesis of single-crystalline CdS dendrites.

PubMed

Niu, Haixia; Yang, Qing; Tang, Kaibin; Xie, Yi; Zhu, Yongchun

2006-01-01

The single-crystalline CdS dendrites have been fabricated from the reaction of CdCl2 and thiourea at 180 degrees C, in which glycine was employed as a soft template. The obtained products were explored by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and selected area electronic diffraction. The optical properties of CdS dendrites have been investigated by ultraviolet and visible light (UV-vis) and photoluminescence techniques. The investigations indicated that the dendrites were grown due to the anisotropic properties enhanced by the use of Glycine in the route.

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

NASA Astrophysics Data System (ADS)

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

2006-11-01

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

Neutron powder diffraction study on the iron-based nitride superconductor ThFeAsN

NASA Astrophysics Data System (ADS)

Mao, Huican; Wang, Cao; Maynard-Casely, Helen E.; Huang, Qingzhen; Wang, Zhicheng; Cao, Guanghan; Li, Shiliang; Luo, Huiqian

2017-03-01

We report neutron diffraction and transport results on the newly discovered superconducting nitride ThFeAsN with T_c= 30 \\text{K} . No magnetic transition, but a weak structural distortion around 160 K, is observed by cooling from 300 K to 6 K. Analysis on the resistivity, Hall transport and crystal structure suggests that this material behaves as an electron optimally doped pnictide superconductor due to extra electrons from nitrogen deficiency or oxygen occupancy at the nitrogen site, which, together with the low arsenic height, may enhance the electron itinerancy and reduce the electron correlations, thus suppressing the static magnetic order.

Ultrafast electron diffraction study of ab-plane dynamics in superconducting Bi2Sr<2CaCu2O8+d

NASA Astrophysics Data System (ADS)

Konstantinova, Tatiana; Reid, Alexander; Wu, Lijun; Durr, Hermann; Wang, Xijie; Zhu, Yimei

The role of phonons and other collective modes in cooperative electron phenomena in high-TC cuprate superconductors is an extensively interesting topic. Time-resolved experiments provide temporal hierarchy of the bosonic modes interacting with electrons. However, majority of research in this field explore dynamics of electronic states and can only make indirect conclusion about involvement of the lattice. We report time-resolved study of optimally doped Bi2Sr2CaCu2O8+d lattice response to photo-excitation by means of ultrafast electron diffraction that is directly sensitive to atomic motion. Data analysis utilizing Bloch-wave calculation of diffraction peak intensity allows separation of Cu-O in-plane vibration building up on the sub picosecond time scale from the low energy phonon population growth with a much slower rate. This study confirms the assumption of strong electron coupling to the Cu-O plane phonons. This work was supported by the US DOE, Office of Science, Basic Energy Science, Materials Science and Engineering Division under Contract No: DE-AC02-98CH10886; DOE LDRD funding under contract DE-AC02-76SF00515 and BNL.

α-Phase transformation kinetics of U – 8 wt% Mo established by in situ neutron diffraction

DOE PAGES

Garlea, Elena; Steiner, M. A.; Calhoun, C. A.; ...

2016-05-08

The α-phase transformation kinetics of as-cast U - 8 wt% Mo below the eutectoid temperature have been established by in situ neutron diffraction. α-phase weight fraction data acquired through Rietveld refinement at five different isothermal hold temperatures can be modeled accurately utilizing a simple Johnson-Mehl-Avrami-Kolmogorov impingement-based theory, and the results are validated by a corresponding evolution in the γ-phase lattice parameter during transformation that follows Vegard’s law. Neutron diffraction data is used to produce a detailed Time-Temperature-Transformation diagram that improves upon inconsistencies in the current literature, exhibiting a minimum transformation start time of 40 min at temperatures between 500 °Cmore » and 510 °C. Lastly, the transformation kinetics of U – 8 wt% Mo can vary significantly from as-cast conditions after extensive heat treatments, due to homogenization of the typical dendritic microstructure which possesses non-negligible solute segregation.« less

Radius anomaly in the diffraction model for heavy-ion elastic scattering

NASA Astrophysics Data System (ADS)

Pandey, L. N.; Mukherjee, S. N.

1984-04-01

The elastic scattering of heavy ions, 20Ne on 208Pb, 20Ne on 235U, 84Kr on 208Pb, and 84Kr on 232Th, is examined within the framework of Frahn's diffraction model. An analysis of the experiment using the "quarter point recipe" of the expected Fresnel cross sections yields a larger radius for 208Pb than the radii for 235U and 232Th. It is shown that inclusion of the nuclear deformation in the model removes the above anomaly in the radii, and the assumption of smooth cutoff of the angular momentum simultaneously leads to a better fit to elastic scattering data, compared to those obtained by the earlier workers on the assumption of sharp cutoff. [NUCLEAR REACTIONS Elastic scattering, 20Ne+208Pb (161.2 MeV), 20Ne+235U (175 MeV), 84Kr+208Pb (500 MeV), 84Kr+232Th (500 MeV), diffraction model, nuclear deformation.

Editorial: Focus on X-ray Beams with High Coherence

NASA Astrophysics Data System (ADS)

Robinson, Ian; Gruebel, Gerhard; Mochrie, Simon

2010-03-01

This editorial serves as the preface to a special issue of New Journal of Physics, which collects together solicited papers on a common subject, x-ray beams with high coherence. We summarize the issue's content, and explain why there is so much current interest both in the sources themselves and in the applications to the study of the structure of matter and its fluctuations (both spontaneous and driven). As this collection demonstrates, the field brings together accelerator physics in the design of new sources, particle physics in the design of detectors, and chemical and materials scientists who make use of the coherent beams produced. Focus on X-ray Beams with High Coherence Contents Femtosecond pulse x-ray imaging with a large field of view B Pfau, C M Günther, S Schaffert, R Mitzner, B Siemer, S Roling, H Zacharias, O Kutz, I Rudolph, R Treusch and S Eisebitt The FERMI@Elettra free-electron-laser source for coherent x-ray physics: photon properties, beam transport system and applications E Allaria, C Callegari, D Cocco, W M Fawley, M Kiskinova, C Masciovecchio and F Parmigiani Beyond simple exponential correlation functions and equilibrium dynamics in x-ray photon correlation spectroscopy Anders Madsen, Robert L Leheny, Hongyu Guo, Michael Sprung and Orsolya Czakkel The Coherent X-ray Imaging (CXI) instrument at the Linac Coherent Light Source (LCLS) Sébastien Boutet and Garth J Williams Dynamics and rheology under continuous shear flow studied by x-ray photon correlation spectroscopy Andrei Fluerasu, Pawel Kwasniewski, Chiara Caronna, Fanny Destremaut, Jean-Baptiste Salmon and Anders Madsen Exploration of crystal strains using coherent x-ray diffraction Wonsuk Cha, Sanghoon Song, Nak Cheon Jeong, Ross Harder, Kyung Byung Yoon, Ian K Robinson and Hyunjung Kim Coherence properties of the European XFEL G Geloni, E Saldin, L Samoylova, E Schneidmiller, H Sinn, Th Tschentscher and M Yurkov Fresnel coherent diffractive imaging: treatment and analysis of data G J Williams, H M Quiney, A G Peele and K A Nugent Imaging of complex density in silver nanocubes by coherent x-ray diffraction R Harder, M Liang, Y Sun, Y Xia and I K Robinson Methodology for studying strain inhomogeneities in polycrystalline thin films during in situ thermal loading using coherent x-ray diffraction N Vaxelaire, H Proudhon, S Labat, C Kirchlechner, J Keckes, V Jacques, S Ravy, S Forest and O Thomas Ptychographic coherent diffractive imaging of weakly scattering specimens Martin Dierolf, Pierre Thibault, Andreas Menzel, Cameron M Kewish, Konstantins Jefimovs, Ilme Schlichting, Konstanze von König, Oliver Bunk and Franz Pfeiffer Dose requirements for resolving a given feature in an object by coherent x-ray diffraction imaging Andreas Schropp and Christian G Schroer FLASH: new opportunities for (time-resolved) coherent imaging of nanostructures R Treusch and J Feldhaus Structure of a single particle from scattering by many particles randomly oriented about an axis: toward structure solution without crystallization? D K Saldin, V L Shneerson, M R Howells, S Marchesini, H N Chapman, M Bogan, D Shapiro, R A Kirian, U Weierstall, K E Schmidt and J C H Spence Analysis of strain and stacking faults in single nanowires using Bragg coherent diffraction imaging V Favre-Nicolin, F Mastropietro, J Eymery, D Camacho, Y M Niquet, B M Borg, M E Messing, L-E Wernersson, R E Algra, E P A M Bakkers, T H Metzger, R Harder and I K Robinson Coherent science at the SwissFEL x-ray laser B D Patterson, R Abela, H-H Braun, U Flechsig, R Ganter, Y Kim, E Kirk, A Oppelt, M Pedrozzi, S Reiche, L Rivkin, Th Schmidt, B Schmitt, V N Strocov, S Tsujino and A F Wrulich Energy recovery linac (ERL) coherent hard x-ray sources Donald H Bilderback, Joel D Brock, Darren S Dale, Kenneth D Finkelstein, Mark A Pfeifer and Sol M Gruner Statistical and coherence properties of radiation from x-ray free-electron lasers E L Saldin, E A Schneidmiller and M V Yurkov Microscopic return point memory in Co/Pd multilayer films K A Seu, R Su, S Roy, D Parks, E Shipton, E E Fullerton and S D Kevan Holographic and diffractive x-ray imaging using waveguides as quasi-point sources K Giewekemeyer, H Neubauer, S Kalbfleisch, S P Krüger and T Salditt Mapping the conformations of biological assemblies P Schwander, R Fung, G N Phillips Jr and A Ourmazd Imaging the displacement field within epitaxial nanostructures by coherent diffraction: a feasibility study Ana Diaz, Virginie Chamard, Cristian Mocuta, Rogerio Magalhães-Paniago, Julian Stangl, Dina Carbone, Till H Metzger and Günther Bauer The potential for two-dimensional crystallography of membrane proteins at future x-ray free-electron laser sources Cameron M Kewish, Pierre Thibault, Oliver Bunk and Franz Pfeiffer Coherence properties of hard x-ray synchrotron sources and x-ray free-electron lasers I A Vartanyants and A Singer Coherent imaging of biological samples with femtosecond pulses at the free-electron laser FLASH A P Mancuso, Th Gorniak, F Staier, O M Yefanov, R Barth, C Christophis, B Reime, J Gulden, A Singer, M E Pettit, Th Nisius, Th Wilhein, C Gutt, G Grübel, N Guerassimova, R Treusch, J Feldhaus, S Eisebitt, E Weckert, M Grunze, A Rosenhahn and I A Vartanyants

Three-dimensional electron diffraction as a complementary technique to powder X-ray diffraction for phase identification and structure solution of powders.

PubMed

Yun, Yifeng; Zou, Xiaodong; Hovmöller, Sven; Wan, Wei

2015-03-01

Phase identification and structure determination are important and widely used techniques in chemistry, physics and materials science. Recently, two methods for automated three-dimensional electron diffraction (ED) data collection, namely automated diffraction tomography (ADT) and rotation electron diffraction (RED), have been developed. Compared with X-ray diffraction (XRD) and two-dimensional zonal ED, three-dimensional ED methods have many advantages in identifying phases and determining unknown structures. Almost complete three-dimensional ED data can be collected using the ADT and RED methods. Since each ED pattern is usually measured off the zone axes by three-dimensional ED methods, dynamic effects are much reduced compared with zonal ED patterns. Data collection is easy and fast, and can start at any arbitrary orientation of the crystal, which facilitates automation. Three-dimensional ED is a powerful technique for structure identification and structure solution from individual nano- or micron-sized particles, while powder X-ray diffraction (PXRD) provides information from all phases present in a sample. ED suffers from dynamic scattering, while PXRD data are kinematic. Three-dimensional ED methods and PXRD are complementary and their combinations are promising for studying multiphase samples and complicated crystal structures. Here, two three-dimensional ED methods, ADT and RED, are described. Examples are given of combinations of three-dimensional ED methods and PXRD for phase identification and structure determination over a large number of different materials, from Ni-Se-O-Cl crystals, zeolites, germanates, metal-organic frameworks and organic compounds to intermetallics with modulated structures. It is shown that three-dimensional ED is now as feasible as X-ray diffraction for phase identification and structure solution, but still needs further development in order to be as accurate as X-ray diffraction. It is expected that three-dimensional ED methods will become crucially important in the near future.

Auger electron diffraction study of the growth of Fe(001) films on ZnSe(001)

NASA Astrophysics Data System (ADS)

Jonker, B. T.; Prinz, G. A.

1991-03-01

The growth of Fe films on ZnSe(001) epilayers and bulk GaAs(001) substrates has been studied to determine the mode of film growth, the formation of the interface, and the structure of the overlayer at the 1-10 monolayer level. Auger electron diffraction (AED), x-ray photoelectron spectroscopy (XPS), and reflection high-energy electron diffraction data are obtained for incremental deposition of the Fe(001) overlayer. The coverage dependence of the AED forward scattering peaks reveals a predominantly layer-by-layer mode of film growth at 175 °C on ZnSe, while a more three-dimensional growth mode occurs on the oxide-desorbed GaAs(001) substrate. XPS studies of the semiconductor 3d levels indicate that the Fe/ZnSe interface is less reactive than the Fe/GaAs interface.

Determination of dislocation density by electron backscatter diffraction and X-ray line profile analysis in ferrous lath martensite

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

Berecz, Tibor, E-mail: berecz@eik.bme.hu; Jenei, Péter, E-mail: jenei@metal.elte.hu; Csóré, András, E-mail: csorean@gmail.com

2016-03-15

The microstructure and the dislocation density in as-quenched ferrous lath martensite were studied by different methods. The blocks, packets and variants formed due to martensitic transformation were identified and their sizes were determined by electron backscatter diffraction (EBSD). Concomitant transmission electron microscopy (TEM) investigation revealed that the laths contain subgrains with the size between 50 and 100 nm. A novel evaluation procedure of EBSD images was elaborated for the determination of the density and the space distribution of geometrically necessary dislocations from the misorientation distribution. The total dislocation density obtained by X-ray diffraction line profile analysis was in good agreementmore » with the value determined by EBSD, indicating that the majority of dislocations formed due to martensitic transformation during quenching are geometrically necessary dislocations.« less

Room Temperature Ferromagnetism of Fe Doped Indium Tin Oxide Based on Dispersed Fe3O4 Nanoparticles

NASA Astrophysics Data System (ADS)

Okada, Koichi; Kohiki, Shigemi; Nishi, Sachio; Shimooka, Hirokazu; Deguchi, Hiroyuki; Mitome, Masanori; Bando, Yoshio; Shishido, Toetsu

2007-09-01

Transmission electron microscopy revealed that Fe3O4 nanoparticles with diameter of ≈200 nm dispersed in Fe doped indium tin oxide (Fe@ITO) powders exhibiting co-occurrence of room temperature ferromagnetism and superparamagnetism. Although we observed no X-ray diffraction peak from Fe related compounds for Fe0.19@ITO (ITO: In1.9Sn0.1O3) powders, the powders showed both hysteresis loop in field dependent magnetization at 300 K and divergence of zero-field-cooled magnetization from field-cooled magnetization. Scanning transmission electron microscopy with energy dispersive X-ray spectroscopy demonstrated that the nanoparticle with diameter of ≈200 nm consists of Fe and oxygen. Transmission electron diffraction revealed that crystal structure of the nanoparticle is inverse spinel type Fe3O4. The Fe3O4 crystalline phase by electron diffraction is consistent with the saturation magnetization of 1.3 μB/Fe and magnetic anomaly at ≈110 K observed for the powders.

Ultrafast structural dynamics of boron nitride nanotubes studied using transmitted electrons.

PubMed

Li, Zhongwen; Sun, Shuaishuai; Li, Zi-An; Zhang, Ming; Cao, Gaolong; Tian, Huanfang; Yang, Huaixin; Li, Jianqi

2017-09-14

We investigate the ultrafast structural dynamics of multi-walled boron nitride nanotubes (BNNTs) upon femtosecond optical excitation using ultrafast electron diffraction in a transmission electron microscope. Analysis of the time-resolved (100) and (002) diffraction profiles reveals highly anisotropic lattice dynamics of BNNTs, which can be attributed to the distinct nature of the chemical bonds in the tubular structure. Moreover, the changes in (002) diffraction positions and intensities suggest that the lattice response of BNNTs to the femtosecond laser excitation involves a fast and a slow lattice dynamic process. The fast process with a time constant of about 8 picoseconds can be understood to be a result of electron-phonon coupling, while the slow process with a time constant of about 100 to 300 picoseconds depending on pump laser fluence is tentatively associated with an Auger recombination effect. In addition, we discuss the power-law relationship of a three-photon absorption process in the BNNT nanoscale system.

Free-electron-laser coherent diffraction images of individual drug-carrying liposome particles in solution.

PubMed

Huang, Chi-Feng; Liang, Keng S; Hsu, Tsui-Ling; Lee, Tsung-Tse; Chen, Yi-Yun; Yang, Shun-Min; Chen, Hsiang-Hsin; Huang, Shih-Hsin; Chang, Wei-Hau; Lee, Ting-Kuo; Chen, Peilin; Peng, Kuei-En; Chen, Chien-Chun; Shi, Cheng-Zhi; Hu, Yu-Fang; Margaritondo, Giorgio; Ishikawa, Tetsuya; Wong, Chi-Huey; Hwu, Y

2018-02-08

Using the excellent performances of a SACLA (RIKEN/HARIMA, Japan) X-ray free electron laser (X-FEL), coherent diffraction imaging (CDI) was used to detect individual liposome particles in water, with or without inserted doxorubicin nanorods. This was possible because of the electron density differences between the carrier, the liposome, and the drug. The result is important since liposome nanocarriers at present dominate drug delivery systems. In spite of the low cross-section of the original ingredients, the diffracted intensity of drug-free liposomes was sufficient for spatial reconstruction yielding quantitative structural information. For particles containing doxorubicin, the structural parameters of the nanorods could be extracted from CDI. Furthermore, the measurement of the electron density of the solution enclosed in each liposome provides direct evidence of the incorporation of ammonium sulphate into the nanorods. Overall, ours is an important test for extending the X-FEL analysis of individual nanoparticles to low cross-sectional systems in solution, and also for its potential use to optimize the manufacturing of drug nanocarriers.

In cellulo serial crystallography of alcohol oxidase crystals inside yeast cells

DOE PAGES

Jakobi, Arjen J.; Passon, Daniel M.; Knoops, Kevin; ...

2016-03-01

The possibility of using femtosecond pulses from an X-ray free-electron laser to collect diffraction data from protein crystals formed in their native cellular organelle has been explored. X-ray diffraction of submicrometre-sized alcohol oxidase crystals formed in peroxisomes within cells of genetically modified variants of the methylotrophic yeast Hansenula polymorpha is reported and characterized. Furthermore, the observations are supported by synchrotron radiation-based powder diffraction data and electron microscopy. Based on these findings, the concept of in cellulo serial crystallography on protein targets imported into yeast peroxisomes without the need for protein purification as a requirement for subsequent crystallization is outlined.

In cellulo serial crystallography of alcohol oxidase crystals inside yeast cells

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

Jakobi, Arjen J.; Passon, Daniel M.; Knoops, Kevin

The possibility of using femtosecond pulses from an X-ray free-electron laser to collect diffraction data from protein crystals formed in their native cellular organelle has been explored. X-ray diffraction of submicrometre-sized alcohol oxidase crystals formed in peroxisomes within cells of genetically modified variants of the methylotrophic yeast Hansenula polymorpha is reported and characterized. Furthermore, the observations are supported by synchrotron radiation-based powder diffraction data and electron microscopy. Based on these findings, the concept of in cellulo serial crystallography on protein targets imported into yeast peroxisomes without the need for protein purification as a requirement for subsequent crystallization is outlined.

In cellulo serial crystallography of alcohol oxidase crystals inside yeast cells

PubMed Central

Jakobi, Arjen J.; Passon, Daniel M.; Knoops, Kèvin; Stellato, Francesco; Liang, Mengning; White, Thomas A.; Seine, Thomas; Messerschmidt, Marc; Chapman, Henry N.; Wilmanns, Matthias

2016-01-01

The possibility of using femtosecond pulses from an X-ray free-electron laser to collect diffraction data from protein crystals formed in their native cellular organelle has been explored. X-ray diffraction of submicrometre-sized alcohol oxidase crystals formed in peroxisomes within cells of genetically modified variants of the methylotrophic yeast Hansenula polymorpha is reported and characterized. The observations are supported by synchrotron radiation-based powder diffraction data and electron microscopy. Based on these findings, the concept of in cellulo serial crystallography on protein targets imported into yeast peroxisomes without the need for protein purification as a requirement for subsequent crystallization is outlined. PMID:27006771

Identification of simultaneous U(VI) sorption complexes and U(IV) nanoprecipitates on the magnetite (111) surface.

PubMed

Singer, David M; Chatman, Shawn M; Ilton, Eugene S; Rosso, Kevin M; Banfield, Jillian F; Waychunas, Glenn A

2012-04-03

Sequestration of uranium (U) by magnetite is a potentially important sink for U in natural and contaminated environments. However, molecular-scale controls that favor U(VI) uptake including both adsorption of U(VI) and reduction to U(IV) by magnetite remain poorly understood, in particular, the role of U(VI)-CO(3)-Ca complexes in inhibiting U(VI) reduction. To investigate U uptake pathways on magnetite as a function of U(VI) aqueous speciation, we performed batch sorption experiments on (111) surfaces of natural single crystals under a range of solution conditions (pH 5 and 10; 0.1 mM U(VI); 1 mM NaNO(3); and with or without 0.5 mM CO(3) and 0.1 mM Ca) and characterized surface-associated U using grazing incidence extended X-ray absorption fine structure spectroscopy (GI-EXAFS), grazing incidence X-ray diffraction (GI-XRD), and scanning electron microscopy (SEM). In the absence of both carbonate ([CO(3)](T), denoted here as CO(3)) and calcium (Ca), or in the presence of CO(3) only, coexisting adsorption of U(VI) surface species and reduction to U(IV) occurs at both pH 5 and 10. In the presence of both Ca and CO(3), only U(VI) adsorption (VI) occurs. When U reduction occurs, nanoparticulate UO(2) forms only within and adjacent to surface microtopographic features such as crystal boundaries and cracks. This result suggests that U reduction is limited to defect-rich surface regions. Further, at both pH 5 and 10 in the presence of both CO(3) and Ca, U(VI)-CO(3)-Ca ternary surface species develop and U reduction is inhibited. These findings extend the range of conditions under which U(VI)-CO(3)-Ca complexes inhibit U reduction.

Diffraction-controlled backscattering threshold and application to Raman gap

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

Rose, Harvey A.; Theoretical Division, Los Alamos National Laboratory, Los Alamos, New Mexico 87544; Mounaix, Philippe

2011-04-15

In most classic analytical models of linear stimulated scatter, light diffraction is omitted, a priori. However, modern laser optic typically includes a variant of the random phase plate [Y. Kato et al., Phys. Rev. Lett. 53, 1057 (1984)], resulting in diffraction limited laser intensity fluctuations - or localized speckles - which may result in explosive reflectivity growth as the average laser intensity approaches a critical value [H. A. Rose and D. F. DuBois, Phys. Rev. Lett. 72, 2883 (1994)]. Among the differences between stimulated Raman scatter (SRS) and stimulated Brillouin scatter is that the SRS scattered light diffracts more stronglymore » than the laser light with increase of electron density. This weakens the tendency of the SRS light to closely follow the most amplified paths, diminishing gain. Let G{sub 0} be the one-dimensional power gain exponent of the stimulated scatter. In this paper we show that differential diffraction gives rise to an increase of G{sub 0} at the SRS physical threshold with increase of electron density up to a drastic disruption of SRS as electron density approaches one fourth of its critical value from below. For three wave interaction lengths not small compared to a speckle length, this is a physically robust Raman gap mechanism.« less

Nanoscale monoclinic domains in epitaxial SrRuO{sub 3} thin films deposited by pulsed laser deposition

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

Ghica, C., E-mail: cghica@infim.ro; Negrea, R. F.; Nistor, L. C.

2014-07-14

In this paper, we analyze the structural distortions observed by transmission electron microscopy in thin epitaxial SrRuO{sub 3} layers used as bottom electrodes in multiferroic coatings onto SrTiO{sub 3} substrates for future multiferroic devices. Regardless of the nature and architecture of the multilayer oxides deposited on the top of the SrRuO{sub 3} thin films, selected area electron diffraction patterns systematically revealed the presence of faint diffraction spots appearing in forbidden positions for the SrRuO{sub 3} orthorhombic structure. High-resolution transmission electron microscopy (HRTEM) combined with Geometric Phase Analysis (GPA) evidenced the origin of these forbidden diffraction spots in the presence ofmore » structurally disordered nanometric domains in the SrRuO{sub 3} bottom layers, resulting from a strain-driven phase transformation. The local high compressive strain (−4% ÷ −5%) measured by GPA in the HRTEM images induces a local orthorhombic to monoclinic phase transition by a cooperative rotation of the RuO{sub 6} octahedra. A further confirmation of the origin of the forbidden diffraction spots comes from the simulated diffraction patterns obtained from a monoclinic disordered SrRuO{sub 3} structure.« less

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.

Role of Emission Character in Auger Electron Diffraction

NASA Astrophysics Data System (ADS)

Idzerda, Y. U.

A review of the interpretation of the angle-dependent Auger intensity pattern by both Auger electron diffraction (AED), which is concerned with identifying the nearby atomic structure, and angle-resolved Auger electron spectroscopy (ARAES), which is concerned with identifying the character of the emitted electron source function, is presented. The importance of the emission character of the Auger electron (in terms of its angular momentum, l, and its magnetic quantum number, m) in understanding the generation of the AED and ARAES patterns is described. Understanding of how the various direct and secondary mechanisms for the Auger electron generation can affect the populations of these states can also be used to help identify the multiplet structure within the Auger lineshape as well as elucidate the core hole generation process.

Characterization of the carbides and the martensite phase in powder-metallurgy high-speed steel

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

Godec, Matjaz, E-mail: matjaz.godec@imt.si; Batic, Barbara Setina; Mandrino, Djordje

2010-04-15

A microstructural characterization of the powder-metallurgy high-speed-steel S390 Microclean was performed based on an elemental distribution of the carbide phase as well as crystallographic analyses. The results showed that there were two types of carbides present: vanadium-rich carbides, which were not chemically homogeneous and exhibited a tungsten-enriched or tungsten-depleted central area; and chemically homogeneous tungsten-rich M{sub 6}C-type carbides. Despite the possibility of chemical inhomogenities, the crystallographic orientation of each of the carbides was shown to be uniform. Using electron backscatter diffraction the vanadium-rich carbides were determined to be either cubic VC or hexagonal V{sub 6}C{sub 5}, while the tungsten-rich carbidesmore » were M{sub 6}C. The electron backscatter diffraction results were also verified using X-ray diffraction. Several electron backscatter diffraction pattern maps were acquired in order to define the fraction of each carbide phase as well as the amount of martensite phase. The fraction of martensite was estimated using band-contrast images, while the fraction of carbides was calculated using the crystallographic data.« less

Structural dynamics of surfaces by ultrafast electron crystallography: experimental and multiple scattering theory.

PubMed

Schäfer, Sascha; Liang, Wenxi; Zewail, Ahmed H

2011-12-07

Recent studies in ultrafast electron crystallography (UEC) using a reflection diffraction geometry have enabled the investigation of a wide range of phenomena on the femtosecond and picosecond time scales. In all these studies, the analysis of the diffraction patterns and their temporal change after excitation was performed within the kinematical scattering theory. In this contribution, we address the question, to what extent dynamical scattering effects have to be included in order to obtain quantitative information about structural dynamics. We discuss different scattering regimes and provide diffraction maps that describe all essential features of scatterings and observables. The effects are quantified by dynamical scattering simulations and examined by direct comparison to the results of ultrafast electron diffraction experiments on an in situ prepared Ni(100) surface, for which structural dynamics can be well described by a two-temperature model. We also report calculations for graphite surfaces. The theoretical framework provided here allows for further UEC studies of surfaces especially at larger penetration depths and for those of heavy-atom materials. © 2011 American Institute of Physics

Multiobjective optimizations of a novel cryocooled dc gun based ultrafast electron diffraction beam line

NASA Astrophysics Data System (ADS)

Gulliford, Colwyn; Bartnik, Adam; Bazarov, Ivan

2016-09-01

We present the results of multiobjective genetic algorithm optimizations of a single-shot ultrafast electron diffraction beam line utilizing a 225 kV dc gun with a novel cryocooled photocathode system and buncher cavity. Optimizations of the transverse projected emittance as a function of bunch charge are presented and discussed in terms of the scaling laws derived in the charge saturation limit. Additionally, optimization of the transverse coherence length as a function of final rms bunch length at the sample location have been performed for three different sample radii: 50, 100, and 200 μ m , for two final bunch charges: 1 05 electrons (16 fC) and 1 06 electrons (160 fC). Example optimal solutions are analyzed, and the effects of disordered induced heating estimated. In particular, a relative coherence length of Lc ,x/σx=0.27 nm /μ m was obtained for a final bunch charge of 1 05 electrons and final bunch length of σt≈100 fs . For a final charge of 1 06 electrons the cryogun produces Lc ,x/σx≈0.1 nm /μ m for σt≈100 - 200 fs and σx≥50 μ m . These results demonstrate the viability of using genetic algorithms in the design and operation of ultrafast electron diffraction beam lines.

Constitutional self-organization of adenine-uracil-derived hybrid materials.

PubMed

Arnal-Hérault, Carole; Barboiu, Mihai; Pasc, Andreea; Michau, Mathieu; Perriat, Pascal; van der Lee, Arie

2007-01-01

The alkoxysilane nucleobase adenine (A) and uracil (U) precursors described in this paper generate in solution a complex library of hydrogen-bonded aggregates, which can be expressed in the solid state as discrete higher oligomers. The different interconverting outputs that nucleobases may form by oligomerization define a dynamic polyfunctional diversity that may be "extracted selectively" in solid state by sol-gel transcription, under the intrinsic stability of the system. After the sol-gel process, unique constitutional preference for specific geometries in hybrid materials is consistent with a preferential arrangement of nucleobase systems, favoring the self-assembly by the Hoogsteen geometry. FTIR and NMR spectroscopy and X-ray powder diffraction experiments demonstrate the formation of self-organized hybrid supramolecular materials. Electron microscopy reveals the micrometric platelike morphology of the hybrid materials. The M(A-U) hybrid material is nanostructured in ordered circular domains of 5 nm in diameter of alternative light and dark rows with an one-dimensional periodicity of 3.5 A.

2017 Report for New LANL Physical Vapor Deposition Capability

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

Roman, Audrey Rae; Zhao, Xinxin; Bond, Evelyn M.

There is an urgent need at LANL to achieve uniform, thin film actinide targets that are essential for nuclear physics experiments. The target preparation work is currently performed externally by Professor Walter Loveland at Oregon State University, who has made various evaporated actinide targets such as Th and U for use on several nuclear physics measurements at LANSCE. We are developing a vapor deposition capability, with the goal of evaporating Th and U in the Actinide Research Facility (ARF) at TA-48. In the future we plan to expand this work to evaporating transuranic elements, such as Pu. The ARF ismore » the optimal location for evaporating actinides because this lab is specifically dedicated to actinide research. There are numerous instruments in the ARF that can be used to provide detailed characterization of the evaporated thin films such as: Table top Scanning Electron Microscope, In-situ X-Ray Diffraction, and 3D Raman spectroscopy. These techniques have the ability to determine the uniformity, surface characterization, and composition of the deposits.« less

Quantum games with a multi-slit electron diffraction set-up

NASA Astrophysics Data System (ADS)

Iqbal, A.

2003-05-01

A set-up is proposed to play a quantum version of the famous bimatrix game of Prisoners' Dilemma. Multi-slit electron diffraction with each player's pure strategy consisting of opening one of the two slits at his/her disposal are essential features of the set-up. Instead of entanglement the association of waves with travelling material objects is suggested as another resource to play quantum games.

Measurement and Interpretation of Diffuse Scattering in X-Ray Diffraction for Macromolecular Crystallography

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

Wall, Michael E.

X-ray diffraction from macromolecular crystals includes both sharply peaked Bragg reflections and diffuse intensity between the peaks. The information in Bragg scattering reflects the mean electron density in the unit cells of the crystal. The diffuse scattering arises from correlations in the variations of electron density that may occur from one unit cell to another, and therefore contains information about collective motions in proteins.

X-ray laser–induced electron dynamics observed by femtosecond diffraction from nanocrystals of Buckminsterfullerene

PubMed Central

Abbey, Brian; Dilanian, Ruben A.; Darmanin, Connie; Ryan, Rebecca A.; Putkunz, Corey T.; Martin, Andrew V.; Wood, David; Streltsov, Victor; Jones, Michael W. M.; Gaffney, Naylyn; Hofmann, Felix; Williams, Garth J.; Boutet, Sébastien; Messerschmidt, Marc; Seibert, M. Marvin; Williams, Sophie; Curwood, Evan; Balaur, Eugeniu; Peele, Andrew G.; Nugent, Keith A.; Quiney, Harry M.

2016-01-01

X-ray free-electron lasers (XFELs) deliver x-ray pulses with a coherent flux that is approximately eight orders of magnitude greater than that available from a modern third-generation synchrotron source. The power density of an XFEL pulse may be so high that it can modify the electronic properties of a sample on a femtosecond time scale. Exploration of the interaction of intense coherent x-ray pulses and matter is both of intrinsic scientific interest and of critical importance to the interpretation of experiments that probe the structures of materials using high-brightness femtosecond XFEL pulses. We report observations of the diffraction of extremely intense 32-fs nanofocused x-ray pulses by a powder sample of crystalline C60. We find that the diffraction pattern at the highest available incident power significantly differs from the one obtained using either third-generation synchrotron sources or XFEL sources operating at low output power and does not correspond to the diffraction pattern expected from any known phase of crystalline C60. We interpret these data as evidence of a long-range, coherent dynamic electronic distortion that is driven by the interaction of the periodic array of C60 molecular targets with intense x-ray pulses of femtosecond duration. PMID:27626076

A pseudo-tetragonal tungsten bronze superstructure: a combined solution of the crystal structure of K6.4(Nb,Ta)(36.3)O94 with advanced transmission electron microscopy and neutron diffraction.

PubMed

Paria Sena, Robert; Babaryk, Artem A; Khainakov, Sergiy; Garcia-Granda, Santiago; Slobodyanik, Nikolay S; Van Tendeloo, Gustaaf; Abakumov, Artem M; Hadermann, Joke

2016-01-21

The crystal structure of the K6.4Nb28.2Ta8.1O94 pseudo-tetragonal tungsten bronze-type oxide was determined using a combination of X-ray powder diffraction, neutron diffraction and transmission electron microscopy techniques, including electron diffraction, high angle annular dark field scanning transmission electron microscopy (HAADF-STEM), annular bright field STEM (ABF-STEM) and energy-dispersive X-ray compositional mapping (STEM-EDX). The compound crystallizes in the space group Pbam with unit cell parameters a = 37.468(9) Å, b = 12.493(3) Å, c = 3.95333(15) Å. The structure consists of corner sharing (Nb,Ta)O6 octahedra forming trigonal, tetragonal and pentagonal tunnels. All tetragonal tunnels are occupied by K(+) ions, while 1/3 of the pentagonal tunnels are preferentially occupied by Nb(5+)/Ta(5+) and 2/3 are occupied by K(+) in a regular pattern. A fractional substitution of K(+) in the pentagonal tunnels by Nb(5+)/Ta(5+) is suggested by the analysis of the HAADF-STEM images. In contrast to similar structures, such as K2Nb8O21, also parts of the trigonal tunnels are fractionally occupied by K(+) cations.

Structural phase transitions and time-resolved dynamics of solid-supported interfacial methanol observed by reflection electron diffraction

NASA Astrophysics Data System (ADS)

Yang, Ding-Shyue; He, Xing; Wu, Chengyi

Due to their large scattering cross sections with matter, electrons are suitable for contactless probing of solid-supported surface assemblies, especially in a reflection geometry. Direct visualization of assembly structures through electron diffraction further enables studies of ultrafast structural dynamics through the pump-probe scheme as well as discoveries of hidden phase changes in equilibrium that have been obscure in spectroscopic measurements. In this presentation, we report our first observation of unique two-stage transformations of interfacial methanol on smooth hydrophobic surfaces. The finding may reconcile the inconsistent previous reports of the crystallization temperature using various indirect methods. Dynamically, energy transfer across a solid-molecule interface following photoexcitation of the substrate is found to be highly dependent on the structure of interfacial methanol. If it is only 2-dimensionally ordered, as the film thickness increases, a prolonged time in the decrease of diffraction intensity is seen, signifying an inefficient vibrational coupling in the surface normal direction. Implications of the dynamics results and an outlook of interfacial studies using time-resolved and averaged electron diffraction will be discussed. We gratefully acknowledge the support from the R. A. Welch Foundation (Grant No. E-1860), the Donors of the American Chemical Society Petroleum Research Fund (ACS-PRF), and the University of Houston.

Optimizing disk registration algorithms for nanobeam electron diffraction strain mapping

DOE PAGES

Pekin, Thomas C.; Gammer, Christoph; Ciston, Jim; ...

2017-01-28

Scanning nanobeam electron diffraction strain mapping is a technique by which the positions of diffracted disks sampled at the nanoscale over a crystalline sample can be used to reconstruct a strain map over a large area. However, it is important that the disk positions are measured accurately, as their positions relative to a reference are directly used to calculate strain. Here in this study, we compare several correlation methods using both simulated and experimental data in order to directly probe susceptibility to measurement error due to non-uniform diffracted disk illumination structure. We found that prefiltering the diffraction patterns with amore » Sobel filter before performing cross correlation or performing a square-root magnitude weighted phase correlation returned the best results when inner disk structure was present. Lastly, we have tested these methods both on simulated datasets, and experimental data from unstrained silicon as well as a twin grain boundary in 304 stainless steel.« less

Direct single-shot phase retrieval from the diffraction pattern of separated objects

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

Leshem, Ben; Xu, Rui; Dallal, Yehonatan

The non-crystallographic phase problem arises in numerous scientific and technological fields. An important application is coherent diffractive imaging. Recent advances in X-ray free-electron lasers allow capturing of the diffraction pattern from a single nanoparticle before it disintegrates, in so-called ‘diffraction before destruction’ experiments. Presently, the phase is reconstructed by iterative algorithms, imposing a non-convex computational challenge, or by Fourier holography, requiring a well-characterized reference field. Here we present a convex scheme for single-shot phase retrieval for two (or more) sufficiently separated objects, demonstrated in two dimensions. In our approach, the objects serve as unknown references to one another, reducing themore » phase problem to a solvable set of linear equations. We establish our method numerically and experimentally in the optical domain and demonstrate a proof-of-principle single-shot coherent diffractive imaging using X-ray free-electron lasers pulses. Lastly, our scheme alleviates several limitations of current methods, offering a new pathway towards direct reconstruction of complex objects.« less

Direct single-shot phase retrieval from the diffraction pattern of separated objects

DOE PAGES

Leshem, Ben; Xu, Rui; Dallal, Yehonatan; ...

2016-02-22

The non-crystallographic phase problem arises in numerous scientific and technological fields. An important application is coherent diffractive imaging. Recent advances in X-ray free-electron lasers allow capturing of the diffraction pattern from a single nanoparticle before it disintegrates, in so-called ‘diffraction before destruction’ experiments. Presently, the phase is reconstructed by iterative algorithms, imposing a non-convex computational challenge, or by Fourier holography, requiring a well-characterized reference field. Here we present a convex scheme for single-shot phase retrieval for two (or more) sufficiently separated objects, demonstrated in two dimensions. In our approach, the objects serve as unknown references to one another, reducing themore » phase problem to a solvable set of linear equations. We establish our method numerically and experimentally in the optical domain and demonstrate a proof-of-principle single-shot coherent diffractive imaging using X-ray free-electron lasers pulses. Lastly, our scheme alleviates several limitations of current methods, offering a new pathway towards direct reconstruction of complex objects.« less

Three-dimensional reconstruction for coherent diffraction patterns obtained by XFEL.

PubMed

Nakano, Miki; Miyashita, Osamu; Jonic, Slavica; Song, Changyong; Nam, Daewoong; Joti, Yasumasa; Tama, Florence

2017-07-01

The three-dimensional (3D) structural analysis of single particles using an X-ray free-electron laser (XFEL) is a new structural biology technique that enables observations of molecules that are difficult to crystallize, such as flexible biomolecular complexes and living tissue in the state close to physiological conditions. In order to restore the 3D structure from the diffraction patterns obtained by the XFEL, computational algorithms are necessary as the orientation of the incident beam with respect to the sample needs to be estimated. A program package for XFEL single-particle analysis based on the Xmipp software package, that is commonly used for image processing in 3D cryo-electron microscopy, has been developed. The reconstruction program has been tested using diffraction patterns of an aerosol nanoparticle obtained by tomographic coherent X-ray diffraction microscopy.

Three dimensional X-ray Diffraction Contrast Tomography Reconstruction of Polycrystalline Strontium Titanate during Sintering and Electron Backscatter Diffraction Validation

NASA Astrophysics Data System (ADS)

Syha, M.; Rheinheimer, W.; Loedermann, B.; Graff, A.; Trenkle, A.; Baeurer, M.; Weygand, D.; Ludwig, W.; Gumbsch, P.

The microstructural evolution of polycrystalline strontium titanate was investigated in three dimensions (3D) using X-ray diffraction contrast tomography (DCT) before and after ex-situ annealing at 1600°C. Post-annealing, the specimen was additionally subjected to phase contrast tomography (PCT) in order to finely resolve the porosities. The resulting microstructure reconstructions were studied with special emphasis on morphology and interface orientation during microstructure evolution. Subsequently, cross-sections of the specimen were studied using electron backscatter diffraction (EBSD). Corresponding cross-sections through the 3D reconstruction were identified and the quality of the reconstruction is validated with special emphasis on the spatial resolution at the grain boundaries, the size and location of pores contained in the material and the accuracy of the orientation determination.

Three-dimensional nanostructure determination from a large diffraction data set recorded using scanning electron nanodiffraction.

PubMed

Meng, Yifei; Zuo, Jian-Min

2016-09-01

A diffraction-based technique is developed for the determination of three-dimensional nanostructures. The technique employs high-resolution and low-dose scanning electron nanodiffraction (SEND) to acquire three-dimensional diffraction patterns, with the help of a special sample holder for large-angle rotation. Grains are identified in three-dimensional space based on crystal orientation and on reconstructed dark-field images from the recorded diffraction patterns. Application to a nanocrystalline TiN thin film shows that the three-dimensional morphology of columnar TiN grains of tens of nanometres in diameter can be reconstructed using an algebraic iterative algorithm under specified prior conditions, together with their crystallographic orientations. The principles can be extended to multiphase nanocrystalline materials as well. Thus, the tomographic SEND technique provides an effective and adaptive way of determining three-dimensional nanostructures.

The Evolution of Surface Symmetry in Femtosecond Laser-Induced Transient States of Matter

NASA Astrophysics Data System (ADS)

Garnett, Joy Carleen

Gallium arsenide and other III-V materials are well known for their excellent optical and electronic properties and have led to the development of high-performance photovoltaic cells1,2, photoelectrochemical water splitting3,4, and light emitting diodes (LEDs)5. Several combinations of III-V semiconductors are now being considered as potentially attractive alternatives to silicon for these applications. However, further development requires fundamental understanding of processes that govern light-matter interactions. Specifically, surface strain and ultrafast dynamics are of great interest to the optoelectronic industry. Strained semiconductor surfaces dominate the design of optoelectronics and III-V semiconductor-based LEDs. Currently, the structures of strained surfaces are well characterized with x-ray diffraction (XRD)6 and electron crystallography7-9. However, optically-induced electronic behavior at these interfaces are not fully understood. This has the been one of the stimulants for the research in this dissertation. To further explore opticallyinduced electronic behavior at strained interfaces, I have asked the following questions: 1. How does static optoelectronic behavior change as a function of strain? 2. How does surface symmetry and electronic motion change with respect to strain? 3. How do atomic bonds change as a function of strain? Another main research goal of this work is to understand ultrafast subpicosecond processes after pulsed laser excitation. The knowledge of ultrafast processes dominates the design of devices in industries that require high temporal and spectral resolution. Ultrafast atomic motion has been the major focus of subpicosecond structural dynamics. Currently, these dynamics upon photoexcitation are well characterized with experimental methods such as ultrafast x-ray diffraction (U-XRD), ultrafast electron diffraction (UED), and ultrafast electron crystallography (UEC). However, ultrafast atomic motion does not occur alone. The bonds connecting these moving atoms are also affected during this process. The correlation between structural and electronic dynamics is not well understood. To further explore correlated structural and electronic behavior upon ultrafast laser excitation, I have asked the following questions: 1. How does subpicosecond optoelectronic behavior change as a function of time after femtosecond pulse photoexcitation? 2. How does subpicosecond surface symmetry and electronic motion change with respect to time after femtosecond pulse photoexcitation? 3. How do atomic bonds change as a function of time after femtosecond pulse photoexcitation? To address these questions, I used experimental methods sensitive to both atomic motions and electronic responses: polarization-resolved second harmonic generation (PRSHG) and timeresolved, polarization-resolved second harmonic generation (TRPRSHG). The dissertation covers application of these techniques to III-V semiconductors: gallium arsenide (GaAs), gallium antimonide (GaSb), and aluminum gallium arsenide (AlGaAs). This dissertation is organized as follows. Chapter 2 presents the background of electronic band structures, ultrafast relaxation processes, and the origin of nonlinear optics from the perspectives of classical and quantum mechanics. It thus provides a framework for the static and transient nonlinear optical processes observed in III-V semiconductors under ultrafast pulse excitation. Next, Chapter 3 motivates the use of the experimental and analytical methods as applied to the experimental and theoretical studies outlined in Chapters 4 and 5. Chapter 4 is devoted to the understanding of polarization-resolved second-order nonlinear optical responses of various strained III-V semiconductor heterostructures resulting from defect-conducive growth conditions. Simplified phenomenological expressions for the polarization-resolved second harmonic generation (PRSHG) are first derived using tensor analysis. Afterwards, these expressions are used to fit experimental data. The developed formalism is tested under different conditions to gauge the fit robustness and sensitivity to mechanical and electronic changes in strained IIIV semiconductors. Along that same vein, Chapter 5 extends this analytical fit to describe ultrafast PRSHG responses of GaAs (100) as a function of transient changes in the interatomic potential within the first picosecond after photoexcitation. Finally, the dissertation concludes with Chapter 6 addressing possible directions for future work. The chapter begins with a description of studies to further test the sensitivity and robustness of the PRSHG phenomenological fit and how it can be used to characterize more classes of materials.

Structure determination of Ba5AlF13 by coupling electron, synchrotron and neutron powder diffraction, solid-state NMR and ab initio calculations.

PubMed

Martineau, Charlotte; Allix, Mathieu; Suchomel, Matthew R; Porcher, Florence; Vivet, François; Legein, Christophe; Body, Monique; Massiot, Dominique; Taulelle, Francis; Fayon, Franck

2016-10-04

The room temperature structure of Ba 5 AlF 13 has been investigated by coupling electron, synchrotron and neutron powder diffraction, solid-state high-resolution NMR ( 19 F and 27 Al) and first principles calculations. An initial structural model has been obtained from electron and synchrotron powder diffraction data, and its main features have been confirmed by one- and two-dimensional NMR measurements. However, DFT GIPAW calculations of the 19 F isotropic shieldings revealed an inaccurate location of one fluorine site (F3, site 8a), which exhibited unusual long F-Ba distances. The atomic arrangement was reinvestigated using neutron powder diffraction data. Subsequent Fourier maps showed that this fluorine atom occupies a crystallographic site of lower symmetry (32e) with partial occupancy (25%). GIPAW computations of the NMR parameters validate the refined structural model, ruling out the presence of local static disorder and indicating that the partial occupancy of this F site reflects a local motional process. Visualisation of the dynamic process was then obtained from the Rietveld refinement of neutron diffraction data using an anharmonic description of the displacement parameters to account for the thermal motion of the mobile fluorine. The whole ensemble of powder diffraction and NMR data, coupled with first principles calculations, allowed drawing an accurate structural model of Ba 5 AlF 13 , including site-specific dynamical disorder in the fluorine sub-network.

The structure of denisovite, a fibrous nanocrystalline polytypic disordered ‘very complex’ silicate, studied by a synergistic multi-disciplinary approach employing methods of electron crystallography and X-ray powder diffraction

PubMed Central

Schowalter, Marco; Schmidt, Martin U.; Czank, Michael; Depmeier, Wulf; Rosenauer, Andreas

2017-01-01

Denisovite is a rare mineral occurring as aggregates of fibres typically 200–500 nm diameter. It was confirmed as a new mineral in 1984, but important facts about its chemical formula, lattice parameters, symmetry and structure have remained incompletely known since then. Recently obtained results from studies using microprobe analysis, X-ray powder diffraction (XRPD), electron crystallography, modelling and Rietveld refinement will be reported. The electron crystallography methods include transmission electron microscopy (TEM), selected-area electron diffraction (SAED), high-angle annular dark-field imaging (HAADF), high-resolution transmission electron microscopy (HRTEM), precession electron diffraction (PED) and electron diffraction tomography (EDT). A structural model of denisovite was developed from HAADF images and later completed on the basis of quasi-kinematic EDT data by ab initio structure solution using direct methods and least-squares refinement. The model was confirmed by Rietveld refinement. The lattice parameters are a = 31.024 (1), b = 19.554 (1) and c = 7.1441 (5) Å, β = 95.99 (3)°, V = 4310.1 (5) Å3 and space group P12/a1. The structure consists of three topologically distinct dreier silicate chains, viz. two xonotlite-like dreier double chains, [Si6O17]10−, and a tubular loop-branched dreier triple chain, [Si12O30]12−. The silicate chains occur between three walls of edge-sharing (Ca,Na) octahedra. The chains of silicate tetrahedra and the octahedra walls extend parallel to the z axis and form a layer parallel to (100). Water molecules and K+ cations are located at the centre of the tubular silicate chain. The latter also occupy positions close to the centres of eight-membered rings in the silicate chains. The silicate chains are geometrically constrained by neighbouring octahedra walls and present an ambiguity with respect to their z position along these walls, with displacements between neighbouring layers being either Δz = c/4 or −c/4. Such behaviour is typical for polytypic sequences and leads to disorder along [100]. In fact, the diffraction pattern does not show any sharp reflections with l odd, but continuous diffuse streaks parallel to a* instead. Only reflections with l even are sharp. The diffuse scattering is caused by (100) nano­lamellae separated by stacking faults and twin boundaries. The structure can be described according to the order–disorder (OD) theory as a stacking of layers parallel to (100). PMID:28512570

For Brighter Electron Sources: A Cryogenically Cooled Photocathode and DC Photogun

NASA Astrophysics Data System (ADS)

Lee, Hyeri

Electron beams produced by photoinjectors have a wide range of applications including colliders for high energy and nuclear physics experiments, Free Electron Lasers (FEL), Energy Recovery Linacs (ERL), and Ultrafast Electron Diffraction (UED) with a variety of uses. These applications have been made possible by recent advancement in photocathode and photoinjector research. The key factor is building a compact high-brightness electron source with high voltage and electric field at the photocathode to maximize the electron emission and minimize emittance growth due to space-charge effect. Achieving high brightness from a compact source is a challenging task because it involves an often-conflicting interplay between various requirements imposed by photoemission, acceleration, and beam dynamics. This thesis presents three important results; (i) cryogenically cooled photocathode. From 300K to 90 K, the MTE reduction has been measured from 38 +/- meV to 22 +/- 1meV. (ii) transmission photocathode. MTEs generated from the photocathode operated in transmission mode is smaller by 20% in comparison with the reflection mode operation, which is accompanied by a corresponding QE decrease of about a factor of 2. (iii) a new design of a DC photoemission gun and beamline constructed at Cornell University, along with demonstration of a cryogenically cooled photocathode and transmission photocathode. This photoemission gun can operate at 200kV at both room temperature (RT) and cryogenic temperature (low T) with a corresponding electric field of 10MV/m.

Publications - GMC 145 | Alaska Division of Geological & Geophysical

Science.gov Websites

DGGS GMC 145 Publication Details Title: Analytical results of x-ray diffraction studies on tuff beds , Analytical results of x-ray diffraction studies on tuff beds from core of the following 5 NPRA wells: U.S

Interpreting U-Pb data from primary and secondary features in lunar zircon

NASA Astrophysics Data System (ADS)

Grange, M. L.; Pidgeon, R. T.; Nemchin, A. A.; Timms, N. E.; Meyer, C.

2013-01-01

In this paper, we describe primary and secondary microstructures and textural characteristics found in lunar zircon and discuss the relationships between these features and the zircon U-Pb isotopic systems and the significance of these features for understanding lunar processes. Lunar zircons can be classified according to: (i) textural relationships between zircon and surrounding minerals in the host breccias, (ii) the internal microstructures of the zircon grains as identified by optical microscopy, cathodoluminescence (CL) imaging and electron backscattered diffraction (EBSD) mapping and (iii) results of in situ ion microprobe analyses of the Th-U-Pb isotopic systems. Primary zircon can occur as part of a cogenetic mineral assemblage (lithic clast) or as an individual mineral clast and is unzoned, or has sector and/or oscillatory zoning. The age of primary zircon is obtained when multiple ion microprobe analyses across the polished surface of the grain give reproducible and essentially concordant data. A secondary set of microstructures, superimposed on primary zircon, include localised recrystallised domains, localised amorphous domains, crystal-plastic deformation, planar deformation features and fractures, and are associated with impact processes. The first two secondary microstructures often yield internally consistent and close to concordant U-Pb ages that we interpret as dating impact events. Others secondary microstructures such as planar deformation features, crystal-plastic deformation and micro-fractures can provide channels for Pb diffusion and result in partial resetting of the U-Pb isotopic systems.

X-ray Spectropolarimetry of Z-pinch Plasmas with a Single-Crystal Technique

NASA Astrophysics Data System (ADS)

Wallace, Matt; Haque, Showera; Neill, Paul; Pereira, Nino; Presura, Radu

2017-10-01

When directed beams of energetic electrons exist in a plasma the resulting x-rays emitted by the plasma can be partially polarized. This makes plasma x-ray polarization spectroscopy, spectropolarimetry, useful for revealing information about the anisotropy of the electron velocity distribution. X-ray spectropolarimetry has indeed been used for this in both space and laboratory plasmas. X-ray polarization measurements are typically performed employing two crystals, both at a 45° Bragg angle. A single-crystal spectropolarimeter can replace two crystal schemes by utilizing two matching sets of internal planes for polarization-splitting. The polarization-splitting planes diffract the incident x-rays into two directions that are perpendicular to each other and the incident beam as well, so the two sets of diffracted x-rays are linearly polarized perpendicularly to each other. An X-cut quartz crystal with surface along the [11-20] planes and a paired set of [10-10] planes in polarization-splitting orientation is now being used on aluminum z-pinches at the University of Nevada, Reno. Past x-ray polarization measurements have been reserved for point-like sources. Recently a slotted collimating aperture has been used to maintain the required geometry for polarization-splitting enabling the spectropolarimetry of extended sources. The design of a single-crystal x-ray spectropolarimeter and experimental results will be presented. Work was supported by U.S. DOE, NNSA Grant DE-NA0001834 and cooperative agreement DE-FC52-06NA27616.

The biomineralization process of uranium(VI) by Saccharomyces cerevisiae - transformation from amorphous U(VI) to crystalline chernikovite.

PubMed

Shen, Yanghao; Zheng, Xinyan; Wang, Xiaoyu; Wang, Tieshan

2018-05-01

Microorganisms play a significant role in uranium(VI) biogeochemistry and influence U(VI) transformation through biomineralization. In the present work, the process of uranium mineralization was investigated by Saccharomyces cerevisiae. The toxicity experiments showed that the viability of cell was not significantly affected by 100 mg L -1 U(VI) under 4 days of exposure time. The batch experiments showed that the phosphate concentration and pH value increased over time during U(VI) adsorption. Meanwhile, thermodynamic calculations demonstrated that the adsorption system was supersaturated with respect to UO 2 HPO 4 . The X-ray powder diffraction spectroscopy (XRD), field emission scanning electron microscopy (FE-SEM) equipped with energy dispersive spectroscopy (EDX), Fourier transform infrared spectroscopy (FTIR), and X-ray photoelectron spectroscopy (XPS) analyses indicated that the U(VI) was first attached onto the cell surface and reacted with hydroxyl, carboxyl, and phosphate groups through electrostatic interactions and complexation. As the immobilization of U(VI) transformed it from the ionic to the amorphous state, lamellar uranium precipitate was formed on the cell surface. With the prolongation of time, the amorphous uranium compound disappeared, and there were some crystalline substances observed extracellularly, which were well-characterized as tetragonal-chernikovite. Furthermore, the size of chernikovite was regulated at nano-level by cells, and the perfect crystal was formed finally. These findings provided an understanding of the non-reductive transformation process of U(VI) from the amorphous to crystalline state within microbe systems, which would be beneficial for the U(VI) treatment and reuse of nuclides and heavy metals.

Preparation of curcumin self-micelle solid dispersion with enhanced bioavailability and cytotoxic activity by mechanochemistry.

PubMed

Zhang, Qihong; Polyakov, Nikolay E; Chistyachenko, Yulia S; Khvostov, Mikhail V; Frolova, Tatjana S; Tolstikova, Tatjana G; Dushkin, Alexandr V; Su, Weike

2018-11-01

An amorphous solid dispersion (SD) of curcumin (Cur) with disodium glycyrrhizin (Na 2 GA) was prepared by mechanical ball milling. Curcumin loaded micelles were self-formed by Na 2 GA when SD dissolved in water. The physical properties of Cur SD in solid state were characterized by differential scanning calorimetry, X-ray diffraction studies, and scanning electron microscope. The characteristics of the sample solutions were analyzed by reverse phase HPLC, UV-visible spectroscopy, 1 H NMR spectroscopy, gel permeation LC, and transmission electron microscopy. In vitro cytotoxic tests demonstrated that Cur SD induced higher cytotoxicity against glioblastoma U-87 MG cells than free Cur. Besides, an improvement of membrane permeability of Cur SD was confirmed by parallel artificial membrane permeability assay. Further pharmacokinetic study of this SD formulation in rat showed a significant ∼19-fold increase of bioavailability as comparing to free Cur. Thus, Cur SD provide a more potent and efficacious formulation for Cur oral delivery.

Realizing Ultrafast Electron Pulse Self-Compression by Femtosecond Pulse Shaping Technique.

PubMed

Qi, Yingpeng; Pei, Minjie; Qi, Dalong; Yang, Yan; Jia, Tianqing; Zhang, Shian; Sun, Zhenrong

2015-10-01

Uncorrelated position and velocity distribution of the electron bunch at the photocathode from the residual energy greatly limit the transverse coherent length and the recompression ability. Here we first propose a femtosecond pulse-shaping method to realize the electron pulse self-compression in ultrafast electron diffraction system based on a point-to-point space-charge model. The positively chirped femtosecond laser pulse can correspondingly create the positively chirped electron bunch at the photocathode (such as metal-insulator heterojunction), and such a shaped electron pulse can realize the self-compression in the subsequent propagation process. The greatest advantage for our proposed scheme is that no additional components are introduced into the ultrafast electron diffraction system, which therefore does not affect the electron bunch shape. More importantly, this scheme can break the limitation that the electron pulse via postphotocathode static compression schemes is not shorter than the excitation laser pulse due to the uncorrelated position and velocity distribution of the initial electron bunch.

Dynamics of reflection high-energy electron diffraction intensity oscillations during molecular beam epitaxial growth of GaAs on (111)B GaAs substrates

NASA Astrophysics Data System (ADS)

Yen, M. Y.; Haas, T. W.

1990-06-01

We have observed intensity oscillations in reflection high-energy electron diffraction during molecular beam epitaxial growth of GaAs on (111)B GaAs substrates. These oscillations only exist over a narrow range of growth conditions and their behavior is strongly dependent on the migration kinetics of group III and the molecular dissociative reaction of group V elements.

Stress Corrosion Cracking Facet Crystallography of Ti-8Al-1Mo-1V (Preprint)

DTIC Science & Technology

2011-05-01

fractography and electron backscatter diffraction. The results indicate that most facets are formed nearly perpendicular to the loading direction on...of Ti-8Al- 1Mo-1V have been characterized using quantitative fractography and electron backscatter diffraction. The results indicate that most facets...EBSD and quantitative tilt fractography [27;29] allow for determination of the crystallographic fracture plane to an accuracy between 1o [29] and

Nanostructure size determination in p-type porous silicon by the use of transmission electron diffraction image processing

NASA Astrophysics Data System (ADS)

Ramirez-Porras, A.

2005-06-01

The structure of p-type porous silicon (PS) has been investigated by the use of transmission electron diffraction (TED) microscopy and image processing. The results suggest the presence of well oriented crystalline phases and polycrystalline phases characterized by random orientation. These phases are believed to be formed by spheres with a mean diameter of 4.3 nm and a standard deviation of 1.3 nm.

Crystallographic data processing for free-electron laser sources

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

White, Thomas A., E-mail: taw@physics.org; Barty, Anton; Stellato, Francesco

2013-07-01

A processing pipeline for diffraction data acquired using the ‘serial crystallography’ methodology with a free-electron laser source is described with reference to the crystallographic analysis suite CrystFEL and the pre-processing program Cheetah. A processing pipeline for diffraction data acquired using the ‘serial crystallography’ methodology with a free-electron laser source is described with reference to the crystallographic analysis suite CrystFEL and the pre-processing program Cheetah. A detailed analysis of the nature and impact of indexing ambiguities is presented. Simulations of the Monte Carlo integration scheme, which accounts for the partially recorded nature of the diffraction intensities, are presented and show thatmore » the integration of partial reflections could be made to converge more quickly if the bandwidth of the X-rays were to be increased by a small amount or if a slight convergence angle were introduced into the incident beam.« less

A method to correct coordinate distortion in EBSD maps

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

Zhang, Y.B., E-mail: yubz@dtu.dk; Elbrønd, A.; Lin, F.X.

2014-10-15

Drift during electron backscatter diffraction mapping leads to coordinate distortions in resulting orientation maps, which affects, in some cases significantly, the accuracy of analysis. A method, thin plate spline, is introduced and tested to correct such coordinate distortions in the maps after the electron backscatter diffraction measurements. The accuracy of the correction as well as theoretical and practical aspects of using the thin plate spline method is discussed in detail. By comparing with other correction methods, it is shown that the thin plate spline method is most efficient to correct different local distortions in the electron backscatter diffraction maps. -more » Highlights: • A new method is suggested to correct nonlinear spatial distortion in EBSD maps. • The method corrects EBSD maps more precisely than presently available methods. • Errors less than 1–2 pixels are typically obtained. • Direct quantitative analysis of dynamic data are available after this correction.« less

Reflection high energy electron diffraction observation of surface mass transport at the two- to three-dimensional growth transition of InAs on GaAs(001)

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

Patella, F.; Arciprete, F.; Fanfoni, M.

2005-12-19

We have followed by reflection high-energy electron diffraction the nucleation of InAs quantum dots on GaAs(001), grown by molecular-beam epitaxy with growth interruptions. Surface mass transport gives rise, at the critical InAs thickness, to a huge nucleation of three-dimensional islands within 0.2 monolayers (ML). Such surface mass diffusion has been evidenced by observing the transition of the reflection high-energy electron diffraction pattern from two- to three-dimensional during the growth interruption after the deposition of 1.59 ML of InAs. It is suggested that the process is driven by the As{sub 2} adsorption-desorption process and by the lowering of the In bindingmore » energy due to compressive strain. The last condition is met first in the region surrounding dots at step edges where nucleation predominantly occurs.« less

Trans-pent-2-ene. Electron diffraction, vibrational analysis and molecular mechanics

NASA Astrophysics Data System (ADS)

Ter Brake, J. H. M.; Mijlhoff, F. C.

1981-12-01

The molecular structure of trans-pent-2-ene has been investigated, using electron diffraction, vibrational analysis and molecular mechanics. It is possible to Fit a model, describing trans-pent-2-ene as a semi-rigid molecule with one conformer only, to the electron diffraction data. However, molecular mechanics shows that trans-pent-2-ene is not a semi-rigid molecule. The large-amplitude motion is described, using all pseudo-conformers at 10° intervals around the circle of rotation. The resulting rα structure is: r[-C-C] = 148.4(1), r[-CC-] = 133.4(2), r[-C-C-] = 157.6(5), r[C-H] = 108.2(1)pm; ∠[-C-CC-] = 125.4(3), ∠[C-C-C-] = 115.6(6), ∠[-C-C-H] = 12.7(6), ∠[-CC-H] = 129(2)°. Standard deviations given in parentheses refer to the last significant digit.

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

PubMed

Kumar, Vineet

2011-12-01

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

Experimental determination of spin-dependent electron density by joint refinement of X-ray and polarized neutron diffraction data.

PubMed

Deutsch, Maxime; Claiser, Nicolas; Pillet, Sébastien; Chumakov, Yurii; Becker, Pierre; Gillet, Jean Michel; Gillon, Béatrice; Lecomte, Claude; Souhassou, Mohamed

2012-11-01

New crystallographic tools were developed to access a more precise description of the spin-dependent electron density of magnetic crystals. The method combines experimental information coming from high-resolution X-ray diffraction (XRD) and polarized neutron diffraction (PND) in a unified model. A new algorithm that allows for a simultaneous refinement of the charge- and spin-density parameters against XRD and PND data is described. The resulting software MOLLYNX is based on the well known Hansen-Coppens multipolar model, and makes it possible to differentiate the electron spins. This algorithm is validated and demonstrated with a molecular crystal formed by a bimetallic chain, MnCu(pba)(H(2)O)(3)·2H(2)O, for which XRD and PND data are available. The joint refinement provides a more detailed description of the spin density than the refinement from PND data alone.

Electron transfer in a virtual quantum state of LiBH4 induced by strong optical fields and mapped by femtosecond x-ray diffraction.

PubMed

Stingl, J; Zamponi, F; Freyer, B; Woerner, M; Elsaesser, T; Borgschulte, A

2012-10-05

Transient polarizations connected with a spatial redistribution of electronic charge in a mixed quantum state are induced by optical fields of high amplitude. We determine for the first time the related transient electron density maps, applying femtosecond x-ray powder diffraction as a structure probe. The prototype ionic material LiBH4 driven nonresonantly by an intense sub-40 fs optical pulse displays a large-amplitude fully reversible electron transfer from the BH4(-) anion to the Li+ cation during excitation. Our results establish this mechanism as the source of the strong optical polarization which agrees quantitatively with theoretical estimates.

Diffractive optical elements on non-flat substrates using electron beam lithography

NASA Technical Reports Server (NTRS)

Maker, Paul D. (Inventor); Muller, Richard E. (Inventor); Wilson, Daniel W. (Inventor)

2002-01-01

The present disclosure describes a technique for creating diffraction gratings on curved surfaces with electron beam lithography. The curved surface can act as an optical element to produce flat and aberration-free images in imaging spectrometers. In addition, the fabrication technique can modify the power structure of the grating orders so that there is more energy in the first order than for a typical grating. The inventors noticed that by using electron-beam lithography techniques, a variety of convex gratings that are well-suited to the requirements of imaging spectrometers can be manufactured.

Elastic scattering of low energy electrons in partially ionized dense semiclassical plasma

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

Dzhumagulova, K. N., E-mail: dzhumagulova.karlygash@gmail.com; Shalenov, E. O.; Ramazanov, T. S.

2015-08-15

Elastic scattering of electrons by hydrogen atoms in a dense semiclassical hydrogen plasma for low impact energies has been studied. Differential scattering cross sections were calculated within the effective model of electron-atom interaction taking into account the effect of screening as well as the quantum mechanical effect of diffraction. The calculations were carried out on the basis of the phase-function method. The influence of the diffraction effect on the Ramsauer–Townsend effect was studied on the basis of a comparison with results made within the effective polarization model of the Buckingham type.

Convergent beam electron-diffraction investigation of lattice mismatch and static disorder in GaAs/GaAs1-xNx intercalated GaAs/GaAs1-xNx:H heterostructures

NASA Astrophysics Data System (ADS)

Frabboni, S.; Grillo, V.; Gazzadi, G. C.; Balboni, R.; Trotta, R.; Polimeni, A.; Capizzi, M.; Martelli, F.; Rubini, S.; Guzzinati, G.; Glas, F.

2012-09-01

Hydrogen incorporation in diluted nitride semiconductors dramatically modifies the electronic and structural properties of the crystal through the creation of nitrogen-hydrogen complexes. We report a convergent beam electron-diffraction characterization of diluted nitride semiconductor-heterostructures patterned at a sub-micron scale and selectively exposed to hydrogen. We present a method to determine separately perpendicular mismatch and static disorder in pristine and hydrogenated heterostructures. The roles of chemical composition and strain on static disorder have been separately assessed.

Electron irradiation induced effects on the physico-chemical properties of L-Arginine Maleate Dihydrate (LAMD) single crystals

NASA Astrophysics Data System (ADS)

Thomas, Prince; Dhole, S. D.; Joseph, Ginson P.

2018-07-01

Single crystals of L-Arginine Maleate Dihydrate (LAMD) have been synthesized by slow solvent evaporation technique and irradiated with 6 MeV electrons at fluences of 0.5 ×1015e /cm2 , 1.0 ×1015e /cm2 and 1.5 ×1015e /cm2 . The Powder X-ray Diffraction (PXRD) studies showed that the intensity of the diffraction peaks of the Electron Beam (EB) irradiated crystals decreases with irradiation fluence. The electron irradiation induced effects on the optical parameters such as cut-off wavelength, band gap, Urbach energy and refractive index have been studied and the results are tabulated. The electronic parameters such as valence electron plasma energy, ℏωp , Penn gap, Ep , Fermi energy, EF and Electronic polarizability, α for pure and irradiated LAMD crystals are calculated. The electrical and thermal properties of the pure and irradiated LAMD crystals are also investigated.

Compression of high-density 0.16 pC electron bunches through high field gradients for ultrafast single shot electron diffraction: The Compact RF Gun

PubMed Central

Daoud, Hazem; Floettmann, Klaus; Dwayne Miller, R. J.

2017-01-01

We present an RF gun design for single shot ultrafast electron diffraction experiments that can produce sub-100 fs high-charge electron bunches in the 130 keV energy range. Our simulations show that our proposed half-cell RF cavity is capable of producing 137 keV, 27 fs rms (60 fs FWHM), 106 electron bunches with an rms spot size of 276 μm and a transverse coherence length of 2.0 nm. The required operation power is 9.2 kW, significantly lower than conventional rf cavity designs and a key design feature. This electron source further relies on high electric field gradients at the cathode to simultaneously accelerate and compress the electron bunch to open up new space-time resolution domains for atomically resolved dynamics. PMID:28428973

Uranium silicide pellet fabrication by powder metallurgy for accident tolerant fuel evaluation and irradiation

DOE PAGES

Harp, Jason Michael; Lessing, Paul Alan; Hoggan, Rita Elaine

2015-06-21

In collaboration with industry, Idaho National Laboratory is investigating uranium silicide for use in future light water reactor fuels as a more accident resistant alternative to uranium oxide base fuels. Specifically this project was focused on producing uranium silicide (U 3Si 2) pellets by conventional powder metallurgy with a density greater than 94% of the theoretical density. This work has produced a process to consistently produce pellets with the desired density through careful optimization of the process. Milling of the U 3Si 2 has been optimized and high phase purity U 3Si 2 has been successfully produced. Results are presentedmore » from sintering studies and microstructural examinations that illustrate the need for a finely ground reproducible particle size distribution in the source powder. The optimized process was used to produce pellets for the Accident Tolerant Fuel-1 irradiation experiment. The average density of these pellets was 11.54 ±0.06 g/cm 3. Additional characterization of the pellets by scaning electron microscopy and X-ray diffraction has also been performed. As a result, pellets produced in this work have been encapsulated for irradiation, and irradiation in the Advanced Test Reactor is expected soon.« less

Magnetic and microwave properties of U-type hexaferrite films with high remanence and low ferromagnetic resonance linewidth

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

Su, Zhijuan; Bennett, Steven; Hu, Bolin

2014-05-07

U-type barium hexaferrite films (Ba{sub 4}Ni{sub 1.4}Co{sub 0.6}Fe{sub 36}O{sub 60}) were deposited on (0001) sapphire substrates by pulsed laser deposition. Microstructure and magnetic properties of the films were characterized by X-ray diffraction, scanning electron microscopy and vibrating sample magnetometry. Ferromagnetic resonance (FMR) measurements were performed at X-band. The results indicate an anisotropy field of ∼8 kOe, and the saturation magnetization (4πM{sub s}) of ∼3.6 kG. An optimal post-deposition annealing of films results in a strong (0 0 n) crystallographic texture and a high hysteresis loop squareness (M{sub r}/M{sub s} = 92%) leading to self biased properties. Furthermore, the highly self-biased ferrite films exhibitedmore » an FMR linewidth of ∼200 Oe. The U-type hexaferrite films having low microwave loss, low magnetic anisotropy field, and high squareness are a suitable alternative to Sc or In doped BaM ferrites that have been the choice material for self-biased microwave devices at X-band frequencies.« less

Uranium silicide pellet fabrication by powder metallurgy for accident tolerant fuel evaluation and irradiation

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

Harp, Jason Michael; Lessing, Paul Alan; Hoggan, Rita Elaine

In collaboration with industry, Idaho National Laboratory is investigating uranium silicide for use in future light water reactor fuels as a more accident resistant alternative to uranium oxide base fuels. Specifically this project was focused on producing uranium silicide (U 3Si 2) pellets by conventional powder metallurgy with a density greater than 94% of the theoretical density. This work has produced a process to consistently produce pellets with the desired density through careful optimization of the process. Milling of the U 3Si 2 has been optimized and high phase purity U 3Si 2 has been successfully produced. Results are presentedmore » from sintering studies and microstructural examinations that illustrate the need for a finely ground reproducible particle size distribution in the source powder. The optimized process was used to produce pellets for the Accident Tolerant Fuel-1 irradiation experiment. The average density of these pellets was 11.54 ±0.06 g/cm 3. Additional characterization of the pellets by scaning electron microscopy and X-ray diffraction has also been performed. As a result, pellets produced in this work have been encapsulated for irradiation, and irradiation in the Advanced Test Reactor is expected soon.« less

Impact of the cation distribution homogeneity on the americium oxidation state in the U0.54Pu0.45Am0.01O2-x mixed oxide

NASA Astrophysics Data System (ADS)

Vauchy, Romain; Robisson, Anne-Charlotte; Martin, Philippe M.; Belin, Renaud C.; Aufore, Laurence; Scheinost, Andreas C.; Hodaj, Fiqiri

2015-01-01

The impact of the cation distribution homogeneity of the U0.54Pu0.45Am0.01O2-x mixed oxide on the americium oxidation state was studied by coupling X-ray diffraction (XRD), electron probe micro analysis (EPMA) and X-ray absorption spectroscopy (XAS). Oxygen-hypostoichiometric Am-bearing uranium-plutonium mixed oxide pellets were fabricated by two different co-milling based processes in order to obtain different cation distribution homogeneities. The americium was generated from β- decay of 241Pu. The XRD analysis of the obtained compounds did not reveal any structural difference between the samples. EPMA, however, revealed a high homogeneity in the cation distribution for one sample, and substantial heterogeneity of the U-Pu (so Am) distribution for the other. The difference in cation distribution was linked to a difference in Am chemistry as investigated by XAS, with Am being present at mixed +III/+IV oxidation state in the heterogeneous compound, whereas only Am(IV) was observed in the homogeneous compound. Previously reported discrepancies on Am oxidation states can hence be explained by cation distribution homogeneity effects.

Nano-Scale Hydroxyapatite: Synthesis, Two-Dimensional Transport Experiments, and Application for Uranium Remediation

DOE PAGES

Kanel, S. R.; Clement, T. P.; Barnett, M. O.; ...

2011-01-01

Synthetic nano-scale hydroxyapatite (NHA) was prepared and characterized using X-ray diffraction (XRD) and scanning electron microscopy (SEM) methods. The XRD data confirmed that the crystalline structure and chemical composition of NHA correspond to Ca 5 OH(PO 4 ) 3 . The SEM data confirmed the size of NHA to be less than 50 nm. A two-dimensional physical model packed with saturated porous media was used to study the transport characteristics of NHA under constant flow conditions. The data show that the transport patterns of NHA were almost identical to tracer transport patterns. This result indicates that the NHA material can movemore » with water like a tracer, and its movement was neither retarded nor influenced by any physicochemical interactions and/or density effects. We have also tested the reactivity of NHA with 1 mg/L hexavalent uranium (U(VI)) and found that complete removal of U(VI) is possible using 0.5 g/L NHA at pH 5 to 6. Our results demonstrate that NHA has the potential to be injected as a dilute slurry for in situ treatment of U(VI)-contaminated groundwater systems.« less

Effect of thermo-mechanical processing on microstructure and mechanical properties of U - Nb - Zr alloys: Part 2 - U - 3 wt % Nb - 9 wt % Zr and U - 9 wt% Nb - 3 wt% Zr

NASA Astrophysics Data System (ADS)

Morais, Nathanael Wagner Sales; Lopes, Denise Adorno; Schön, Cláudio Geraldo

2018-04-01

The present work is the second and final part of an extended investigation on Usbnd Nb - Zr alloys. It investigates the effect of mechanical processing routes on microstructure of alloys U - 3 wt % Nb - 9 wt % Zr and U - 9 wt% Nb - 3 wt% Zr, through X-ray diffraction and scanning electron microscopy, completing the investigation, which started with alloy U - 6 wt% Nb - 6 wt% Zr in part 1. Mechanical properties are determined using microhardness and bending tests and correlated with the developed microstructures. The results show that processing sequence, in particular the inclusion of a 1000 °C heat treatment step, affects significantly the microstructure and mechanical properties of these alloys alloy in different ways. Microstructural characterization shows that both alloys present significant volume fraction of precipitates of a body-centered cubic (BCC) γ-Nb-Zr rich phase in addition the uranium-rich matrix. Bending tests show that sample ductility does not correlate necessarily with hardness and that the key factor appears to be the amount of the γ-Nb-Zr precipitates, which controls the matrix microstructure. Samples with a monoclinic α″ cellular microstructure and/or with the tetragonally-distorted BCC phase (γ0), although not strictly ductile, showed the largest allowed strains-before-break and complete elastic recovery of the broken pieces, pointing out to the macroscopic observation of superelasticity.

Ballistic protons in incoherent exclusive vector meson production as a measure of rare parton fluctuations at an electron-ion collider

DOE PAGES

Lappi, T.; Venugopalan, R.; Mantysaari, H.

2015-02-25

We argue that the proton multiplicities measured in Roman pot detectors at an electron ion collider can be used to determine centrality classes in incoherent diffractive scattering. Incoherent diffraction probes the fluctuations in the interaction strengths of multi-parton Fock states in the nuclear wavefunctions. In particular, the saturation scale that characterizes this multi-parton dynamics is significantly larger in central events relative to minimum bias events. As an application, we examine the centrality dependence of incoherent diffractive vector meson production. We identify an observable which is simultaneously very sensitive to centrality triggered parton fluctuations and insensitive to details of the model.

Tests of Si(111)-7 × 7 structural models by comparison with transmission electron diffraction patterns

NASA Astrophysics Data System (ADS)

McRae, E. G.; Petroff, P. M.

1984-11-01

Several structural models of the Si(111)-7 × 7 surface are tested by comparing calculated and observed transmission electron diffraction (TED) patterns. The models comprise "adatom" models where the unit mesh contains 12 adatoms or atom clusters in a locally (2 × 2) arrangement, and "triangle-dimer" models where the unit mesh contains 9 dimers or pairs of dimers bordering a triangular subunit of the unit mesh. The distribution of diffraction intensity among fractional-order spots is calculated kinematically and compared with TED patterns observed by Petroff and Wilson and others. No agreement is found for adatom models. Good but not perfect agreement is found for one triangle-dimer model.

Thin Film Research. Volume 1

DTIC Science & Technology

1985-05-30

Order (FECO) ......... 23 3. X -Ray Diffraction ............................... 26 4. Transmission Electron Microscopy (TEM) ............... 26 5...remained amorphous after bombardment, as evidenced by X - ray diffraction, and showed no other changes. 0 (2) For Sb203, the crystallite size was reduced...main effect on MgF2 was the reduction in crystallite size. The films were too thir. for meaningful x - ray diffraction analysis. Durability and

Understanding Intense Laser Interactions with Solid Density Plasma

DTIC Science & Technology

2017-01-04

obtain the time-dependent diffraction efficiency. Further improvements may lead to femtosecond temporal resolution, with negligible pump-probe jitter...with negligible pump-probe jitter being possible with future laser- wakefield-accelerator ultrafast-electron-diffraction schemes. Distribution

Diffractive Optical Elements for Spectral Imaging

NASA Technical Reports Server (NTRS)

Wilson, D.; Maker, P.; Muller, R.; Mourolis, P.; Descour, M.; Volin, C.; Dereniak, E.

2000-01-01

Diffractive optical elements fabricated on flat and non-flat substrates frequently act as dispersive elements in imaging spectrometers. We describe the design and electron-beam fabrication of blazed and computer-generated-hologram gratings for slit and tomographic imaging spectrometer.

Diffractive Optical Elements for Spectral Imaging

NASA Technical Reports Server (NTRS)

Wilson, D.; Maker, P.; Muller, R.; Maker, P.; Mouroulis, P.; Descour, M.; Volin, C.; Dereniak, E.

2000-01-01

Diffractive optical elements fabricated on flat and non-flat substrates frequently act as dispersive elements in imaging spectrometers. We describe the design and electron-beam fabrication of blazed and computer-generated-hologram gratings for slit and tomographic imaging spectrometers.

Three-dimensional nanostructure determination from a large diffraction data set recorded using scanning electron nanodiffraction

DOE PAGES

Meng, Yifei; Zuo, Jian -Min

2016-07-04

A diffraction-based technique is developed for the determination of three-dimensional nanostructures. The technique employs high-resolution and low-dose scanning electron nanodiffraction (SEND) to acquire three-dimensional diffraction patterns, with the help of a special sample holder for large-angle rotation. Grains are identified in three-dimensional space based on crystal orientation and on reconstructed dark-field images from the recorded diffraction patterns. Application to a nanocrystalline TiN thin film shows that the three-dimensional morphology of columnar TiN grains of tens of nanometres in diameter can be reconstructed using an algebraic iterative algorithm under specified prior conditions, together with their crystallographic orientations. The principles can bemore » extended to multiphase nanocrystalline materials as well. Furthermore, the tomographic SEND technique provides an effective and adaptive way of determining three-dimensional nanostructures.« less

Understanding deformation with high angular resolution electron backscatter diffraction (HR-EBSD)

NASA Astrophysics Data System (ADS)

Britton, T. B.; Hickey, J. L. R.

2018-01-01

High angular resolution electron backscatter diffraction (HR-EBSD) affords an increase in angular resolution, as compared to ‘conventional’ Hough transform based EBSD, of two orders of magnitude, enabling measurements of relative misorientations of 1 x 10-4 rads (~ 0.006°) and changes in (deviatoric) lattice strain with a precision of 1 x 10-4. This is achieved through direct comparison of two or more diffraction patterns using sophisticated cross-correlation based image analysis routines. Image shifts between zone axes in the two-correlated diffraction pattern are measured with sub-pixel precision and this realises the ability to measure changes in interplanar angles and lattice orientation with a high degree of sensitivity. These shifts are linked to strains and lattice rotations through simple geometry. In this manuscript, we outline the basis of the technique and two case studies that highlight its potential to tackle real materials science challenges, such as deformation patterning in polycrystalline alloys.

Thermal analysis, X-ray powder diffraction and electron microscopy data related with the production of 1:1 Caffeine:Glutaric Acid cocrystals.

PubMed

Duarte, Íris; Andrade, Rita; Pinto, João F; Temtem, Márcio

2016-09-01

The data presented in this article are related to the production of 1:1 Caffeine:Glutaric Acid cocrystals as part of the research article entitled "Green production of cocrystals using a new solvent-free approach by spray congealing" (Duarte et al., 2016) [1]. More specifically, here we present the thermal analysis and the X-ray powder diffraction data for pure Glutaric Acid, used as a raw material in [1]. We also include the X-ray powder diffraction and electron microscopy data obtained for the 1:1 Caffeine:Glutaric Acid cocrystal (form II) produced using the cooling crystallization method reported in "Operating Regions in Cooling Cocrystallization of Caffeine and Glutaric Acid in Acetonitrile" (Yu et al., 2010) [2]. Lastly, we show the X-ray powder diffraction data obtained for assessing the purity of the 1:1 Caffeine:Glutaric cocrystals produced in [1].

Enhancing resolution in coherent x-ray diffraction imaging.

PubMed

Noh, Do Young; Kim, Chan; Kim, Yoonhee; Song, Changyong

2016-12-14

Achieving a resolution near 1 nm is a critical issue in coherent x-ray diffraction imaging (CDI) for applications in materials and biology. Albeit with various advantages of CDI based on synchrotrons and newly developed x-ray free electron lasers, its applications would be limited without improving resolution well below 10 nm. Here, we review the issues and efforts in improving CDI resolution including various methods for resolution determination. Enhancing diffraction signal at large diffraction angles, with the aid of interference between neighboring strong scatterers or templates, is reviewed and discussed in terms of increasing signal-to-noise ratio. In addition, we discuss errors in image reconstruction algorithms-caused by the discreteness of the Fourier transformations involved-which degrade the spatial resolution, and suggest ways to correct them. We expect this review to be useful for applications of CDI in imaging weakly scattering soft matters using coherent x-ray sources including x-ray free electron lasers.

High-Resolution Infrared and Electron-Diffraction Studies of Trimethylenecyclopropane ([3]-Radialene)

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

Wright, Corey; Holmes, Joshua; Nibler, Joseph W.

2013-05-16

Combined high-resolution spectroscopic, electron-diffraction, and quantum theoretical methods are particularly advantageous for small molecules of high symmetry and can yield accurate structures that reveal subtle effects of electron delocalization on molecular bonds. The smallest of the radialene compounds, trimethylenecyclopropane, [3]-radialene, has been synthesized and examined in the gas phase by these methods. The first high-resolution infrared spectra have been obtained for this molecule of D3h symmetry, leading to an accurate B0 rotational constant value of 0.1378629(8) cm-1, within 0.5% of the value obtained from electronic structure calculations (density functional theory (DFT) B3LYP/cc-pVTZ). This result is employed in an analysis ofmore » electron-diffraction data to obtain the rz bond lengths (in Å): C-H = 1.072 (17), C-C = 1.437 (4), and C=C = 1.330 (4). The analysis does not lead to an accurate value of the HCH angle; however, from comparisons of theoretical and experimental angles for similar compounds, the theoretical prediction of 117.5° is believed to be reliable to within 2°. The effect of electron delocalization in radialene is to reduce the single C-C bond length by 0.07 Å compared to that in cyclopropane.« less

In-situ magnetization/heating electron holography to study the magnetic ordering in arrays of nickel metallic nanowires.

PubMed

Ortega, Eduardo; Santiago, Ulises; Giuliani, Jason G; Monton, Carlos; Ponce, Arturo

2018-05-01

Magnetic nanostructures of different size, shape, and composition possess a great potential to improve current technologies like data storage and electromagnetic sensing. In thin ferromagnetic nanowires, their magnetization behavior is dominated by the competition between magnetocrystalline anisotropy (related to the crystalline structure) and shape anisotropy. In this way electron diffraction methods like precession electron diffraction (PED) can be used to link the magnetic behavior observed by Electron Holography (EH) with its crystallinity. Using off-axis electron holography under Lorentz conditions, we can experimentally determine the magnetization distribution over neighboring nanostructures and their diamagnetic matrix. In the case of a single row of nickel nanowires within the alumina template, the thin TEM samples showed a dominant antiferromagnetic arrangement demonstrating long-range magnetostatic interactions playing a major role.

In-situ magnetization/heating electron holography to study the magnetic ordering in arrays of nickel metallic nanowires

NASA Astrophysics Data System (ADS)

Ortega, Eduardo; Santiago, Ulises; Giuliani, Jason G.; Monton, Carlos; Ponce, Arturo

2018-05-01

Magnetic nanostructures of different size, shape, and composition possess a great potential to improve current technologies like data storage and electromagnetic sensing. In thin ferromagnetic nanowires, their magnetization behavior is dominated by the competition between magnetocrystalline anisotropy (related to the crystalline structure) and shape anisotropy. In this way electron diffraction methods like precession electron diffraction (PED) can be used to link the magnetic behavior observed by Electron Holography (EH) with its crystallinity. Using off-axis electron holography under Lorentz conditions, we can experimentally determine the magnetization distribution over neighboring nanostructures and their diamagnetic matrix. In the case of a single row of nickel nanowires within the alumina template, the thin TEM samples showed a dominant antiferromagnetic arrangement demonstrating long-range magnetostatic interactions playing a major role.

System and method for compressive scanning electron microscopy

DOEpatents

Reed, Bryan W

2015-01-13

A scanning transmission electron microscopy (STEM) system is disclosed. The system may make use of an electron beam scanning system configured to generate a plurality of electron beam scans over substantially an entire sample, with each scan varying in electron-illumination intensity over a course of the scan. A signal acquisition system may be used for obtaining at least one of an image, a diffraction pattern, or a spectrum from the scans, the image, diffraction pattern, or spectrum representing only information from at least one of a select subplurality or linear combination of all pixel locations comprising the image. A dataset may be produced from the information. A subsystem may be used for mathematically analyzing the dataset to predict actual information that would have been produced by each pixel location of the image.

Visible diffraction from quasi-crystalline arrays of carbon nanotubes

NASA Astrophysics Data System (ADS)

Butler, Timothy P.; Butt, Haider; Wilkinson, Timothy D.; Amaratunga, Gehan A. J.

2015-08-01

Large area arrays of vertically-aligned carbon nanotubes (VACNTs) are patterned in a quasi-crystalline Penrose tile arrangement through electron beam lithography definition of Ni catalyst dots and subsequent nanotube growth by plasma-enhanced chemical vapour deposition. When illuminated with a 532 nm laser beam high-quality and remarkable diffraction patterns are seen. The diffraction is well matched to theoretical calculations which assume apertures to be present at the location of the VACNTs for transmitted light. The results show that VACNTs act as diffractive elements in reflection and can be used as spatially phased arrays for producing tailored diffraction patterns.

The continuous reinvention of diffractive optics

NASA Astrophysics Data System (ADS)

Kress, Bernard C.

2004-02-01

We show in this paper how the field of diffractive optics has moved during these past twenty years from academic research to main stream industry and consumer electronics. We analyze the main driving forces, the various enabling technologies and techniques for both design, fabrication and mass production of diffractive optics, and the successive markets in which this technology has been able to provide economically viable solutions to specific industrials needs. More specifically, we will see how niche applications making use of special features of diffractive optics seem to survive the applications involving the same diffractives, issued from the successive main technology driven investment bubbles.

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

Häusler, I., E-mail: ines.haeusler@bam.de; Dörfel, I., E-mail: Ilona.doerfel@bam.de; Peplinski, B., E-mail: Burkhard.peplinski@bam.de

A model system was used to simulate the properties of tribofilms which form during automotive braking. The model system was prepared by ball milling of a blend of 70 vol.% iron oxides, 15 vol.% molybdenum disulfide and 15 vol.% graphite. The resulting mixture was characterized by X-ray powder diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and various transmission electron microscopic (TEM) methods, including energy dispersive X-ray spectroscopy (EDXS), high resolution investigations (HRTEM) with corresponding simulation of the HRTEM images, diffraction methods such as scanning nano-beam electron diffraction (SNBED) and selected area electron diffraction (SAED). It could be shown that the ballmore » milling caused a reduction of the grain size of the initial components to the nanometer range. Sometimes even amorphization or partial break-down of the crystal structure was observed for MoS{sub 2} and graphite. Moreover, chemical reactions lead to a formation of surface coverings of the nanoparticles by amorphous material, molybdenum oxides, and iron sulfates as derived from XPS. - Highlights: • Ball milling of iron oxides, MoS{sub 2}, and graphite to simulate a tribofilm • Increasing coefficient of friction after ball milling of the model blend • Drastically change of the diffraction pattern of the powder mixture • TEM & XPS showed the components of the milled mixture and the process during milling. • MoS{sub 2} and graphite suffered a loss in translation symmetry or became amorphous.« less

When holography meets coherent diffraction imaging.

PubMed

Latychevskaia, Tatiana; Longchamp, Jean-Nicolas; Fink, Hans-Werner

2012-12-17

The phase problem is inherent to crystallographic, astronomical and optical imaging where only the intensity of the scattered signal is detected and the phase information is lost and must somehow be recovered to reconstruct the object's structure. Modern imaging techniques at the molecular scale rely on utilizing novel coherent light sources like X-ray free electron lasers for the ultimate goal of visualizing such objects as individual biomolecules rather than crystals. Here, unlike in the case of crystals where structures can be solved by model building and phase refinement, the phase distribution of the wave scattered by an individual molecule must directly be recovered. There are two well-known solutions to the phase problem: holography and coherent diffraction imaging (CDI). Both techniques have their pros and cons. In holography, the reconstruction of the scattered complex-valued object wave is directly provided by a well-defined reference wave that must cover the entire detector area which often is an experimental challenge. CDI provides the highest possible, only wavelength limited, resolution, but the phase recovery is an iterative process which requires some pre-defined information about the object and whose outcome is not always uniquely-defined. Moreover, the diffraction patterns must be recorded under oversampling conditions, a pre-requisite to be able to solve the phase problem. Here, we report how holography and CDI can be merged into one superior technique: holographic coherent diffraction imaging (HCDI). An inline hologram can be recorded by employing a modified CDI experimental scheme. We demonstrate that the amplitude of the Fourier transform of an inline hologram is related to the complex-valued visibility, thus providing information on both, the amplitude and the phase of the scattered wave in the plane of the diffraction pattern. With the phase information available, the condition of oversampling the diffraction patterns can be relaxed, and the phase problem can be solved in a fast and unambiguous manner. We demonstrate the reconstruction of various diffraction patterns of objects recorded with visible light as well as with low-energy electrons. Although we have demonstrated our HCDI method using laser light and low-energy electrons, it can also be applied to any other coherent radiation such as X-rays or high-energy electrons.

Dose-dependent high-resolution electron ptychography

NASA Astrophysics Data System (ADS)

D'Alfonso, A. J.; Allen, L. J.; Sawada, H.; Kirkland, A. I.

2016-02-01

Recent reports of electron ptychography at atomic resolution have ushered in a new era of coherent diffractive imaging in the context of electron microscopy. We report and discuss electron ptychography under variable electron dose conditions, exploring the prospects of an approach which has considerable potential for imaging where low dose is needed.

A general way for quantitative magnetic measurement by transmitted electrons

NASA Astrophysics Data System (ADS)

Song, Dongsheng; Li, Gen; Cai, Jianwang; Zhu, Jing

2016-01-01

EMCD (electron magnetic circular dichroism) technique opens a new door to explore magnetic properties by transmitted electrons. The recently developed site-specific EMCD technique makes it possible to obtain rich magnetic information from the Fe atoms sited at nonequivalent crystallographic planes in NiFe2O4, however it is based on a critical demand for the crystallographic structure of the testing sample. Here, we have further improved and tested the method for quantitative site-specific magnetic measurement applicable for more complex crystallographic structure by using the effective dynamical diffraction effects (general routine for selecting proper diffraction conditions, making use of the asymmetry of dynamical diffraction for design of experimental geometry and quantitative measurement, etc), and taken yttrium iron garnet (Y3Fe5O12, YIG) with more complex crystallographic structure as an example to demonstrate its applicability. As a result, the intrinsic magnetic circular dichroism signals, spin and orbital magnetic moment of iron with site-specific are quantitatively determined. The method will further promote the development of quantitative magnetic measurement with high spatial resolution by transmitted electrons.

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.

Harnessing AIA Diffraction Patterns to Determine Flare Footpoint Temperatures

NASA Astrophysics Data System (ADS)

Bain, H. M.; Schwartz, R. A.; Torre, G.; Krucker, S.; Raftery, C. L.

2014-12-01

In the "Standard Flare Model" energy from accelerated electrons is deposited at the footpoints of newly reconnected flare loops, heating the surrounding plasma. Understanding the relation between the multi-thermal nature of the footpoints and the energy flux from accelerated electrons is therefore fundamental to flare physics. Extreme ultraviolet (EUV) images of bright flare kernels, obtained from the Atmospheric Imaging Assembly (AIA) onboard the Solar Dynamics Observatory, are often saturated despite the implementation of automatic exposure control. These kernels produce diffraction patterns often seen in AIA images during the most energetic flares. We implement an automated image reconstruction procedure, which utilizes diffraction pattern artifacts, to de-saturate AIA images and reconstruct the flare brightness in saturated pixels. Applying this technique to recover the footpoint brightness in each of the AIA EUV passbands, we investigate the footpoint temperature distribution. Using observations from the Ramaty High Energy Solar Spectroscopic Imager (RHESSI), we will characterize the footpoint accelerated electron distribution of the flare. By combining these techniques, we investigate the relation between the nonthermal electron energy flux and the temperature response of the flare footpoints.

Magnetotransport and Heat Capacity in Ternary Compounds U3M2M‧3‧, M=Al, Ga; M=Si, Ge

NASA Astrophysics Data System (ADS)

Troć, R.; Rogl, P.; Tran, V. H.; Czopnik, A.

2001-05-01

We report detailed studies of magnetization, electrical resistivity, magnetoresistivity, and heat capacity performed on the novel family of intermetallic compounds U3M2M‧3, (M=Al, Ga, and M‧=Si, Ge). The present measurements support the earlier conclusions about the ferrimagnetic properties of silicides and ferromagnetic properties of germanides. The resistivity for both compounds U3{Al,Ga}2Si3 exhibits below TC a pronounced maximum observed for the first time in an actinoid-ferrimagnet, probably caused by (a) the reduction of the number of effective conduction carriers or (b) a SDW-type of spin-disorder scattering of electrons. Both low-temperature resistivity (except for U3Ga2Si3) and heat capacity may be described by a T-dependence involving a small gap Δ on the order of 30-50 K in the magnon dispersion. The Cp/T values at 2 K are enhanced and point to a medium-heavy fermion character of all these ternaries. Magnetoresistance for ferrimagnetic U3{Al,Ga}2Si3 is rather small but positive in correspondence of antiferromagnetic interactions. In correspondence to the ferromagnetic materials, negative magnetoresistance is encountered for U3{Al,Ga}2Ge3. Specific features in the temperature dependence of magnetoresistivity Δρ/ρ at various fields confirm the sinusoidal modulation of the magnetic structure for U3Al2Ge3 between 40 and 60 K. Also, such data for U3Ga2Ge3 present strong indications for a similar magnetic modulation between 63 and 93 K, yet to be discovered by neutron diffraction experiments. In addition, the transition at 63 K is furthermore well resolved in the specific heat data of U3Ga2Ge3.

Digital diffractive optics: Have diffractive optics entered mainstream industry yet?

NASA Astrophysics Data System (ADS)

Kress, Bernard; Hejmadi, Vic

2010-05-01

When a new technology is integrated into industry commodity products and consumer electronic devices, and sold worldwide in retail stores, it is usually understood that this technology has then entered the realm of mainstream technology and therefore mainstream industry. Such a leap however does not come cheap, as it has a double edge sword effect: first it becomes democratized and thus massively developed by numerous companies for various applications, but also it becomes a commodity, and thus gets under tremendous pressure to cut down its production and integration costs while not sacrificing to performance. We will show, based on numerous examples extracted from recent industry history, that the field of Diffractive Optics is about to undergo such a major transformation. Such a move has many impacts on all facets of digital diffractive optics technology, from the optical design houses to the micro-optics foundries (for both mastering and volume replication), to the final product integrators or contract manufacturers. The main causes of such a transformation are, as they have been for many other technologies in industry, successive technological bubbles which have carried and lifted up diffractive optics technology within the last decades. These various technological bubbles have been triggered either by real industry needs or by virtual investment hype. Both of these causes will be discussed in the paper. The adjective ""digital"" in "digital diffractive optics" does not refer only, as it is done in digital electronics, to the digital functionality of the element (digital signal processing), but rather to the digital way they are designed (by a digital computer) and fabricated (as wafer level optics using digital masking techniques). However, we can still trace a very strong similarity between the emergence of micro-electronics from analog electronics half a century ago, and the emergence of digital optics from conventional optics today.

Single-pulse enhanced coherent diffraction imaging of bacteria with an X-ray free-electron laser

NASA Astrophysics Data System (ADS)

Fan, Jiadong; Sun, Zhibin; Wang, Yaling; Park, Jaehyun; Kim, Sunam; Gallagher-Jones, Marcus; Kim, Yoonhee; Song, Changyong; Yao, Shengkun; Zhang, Jian; Zhang, Jianhua; Duan, Xiulan; Tono, Kensuke; Yabashi, Makina; Ishikawa, Tetsuya; Fan, Chunhai; Zhao, Yuliang; Chai, Zhifang; Gao, Xueyun; Earnest, Thomas; Jiang, Huaidong

2016-09-01

High-resolution imaging offers one of the most promising approaches for exploring and understanding the structure and function of biomaterials and biological systems. X-ray free-electron lasers (XFELs) combined with coherent diffraction imaging can theoretically provide high-resolution spatial information regarding biological materials using a single XFEL pulse. Currently, the application of this method suffers from the low scattering cross-section of biomaterials and X-ray damage to the sample. However, XFELs can provide pulses of such short duration that the data can be collected using the “diffract and destroy” approach before the effects of radiation damage on the data become significant. These experiments combine the use of enhanced coherent diffraction imaging with single-shot XFEL radiation to investigate the cellular architecture of Staphylococcus aureus with and without labeling by gold (Au) nanoclusters. The resolution of the images reconstructed from these diffraction patterns were twice as high or more for gold-labeled samples, demonstrating that this enhancement method provides a promising approach for the high-resolution imaging of biomaterials and biological systems.

Comparison of quartz crystallographic preferred orientations identified with optical fabric analysis, electron backscatter and neutron diffraction techniques.

PubMed

Hunter, N J R; Wilson, C J L; Luzin, V

2017-02-01

Three techniques are used to measure crystallographic preferred orientations (CPO) in a naturally deformed quartz mylonite: transmitted light cross-polarized microscopy using an automated fabric analyser, electron backscatter diffraction (EBSD) and neutron diffraction. Pole figure densities attributable to crystal-plastic deformation are variably recognizable across the techniques, particularly between fabric analyser and diffraction instruments. Although fabric analyser techniques offer rapid acquisition with minimal sample preparation, difficulties may exist when gathering orientation data parallel with the incident beam. Overall, we have found that EBSD and fabric analyser techniques are best suited for studying CPO distributions at the grain scale, where individual orientations can be linked to their source grain or nearest neighbours. Neutron diffraction serves as the best qualitative and quantitative means of estimating the bulk CPO, due to its three-dimensional data acquisition, greater sample area coverage, and larger sample size. However, a number of sampling methods can be applied to FA and EBSD data to make similar approximations. © 2016 The Authors Journal of Microscopy © 2016 Royal Microscopical Society.

Single-pulse enhanced coherent diffraction imaging of bacteria with an X-ray free-electron laser

PubMed Central

Fan, Jiadong; Sun, Zhibin; Wang, Yaling; Park, Jaehyun; Kim, Sunam; Gallagher-Jones, Marcus; Kim, Yoonhee; Song, Changyong; Yao, Shengkun; Zhang, Jian; Zhang, Jianhua; Duan, Xiulan; Tono, Kensuke; Yabashi, Makina; Ishikawa, Tetsuya; Fan, Chunhai; Zhao, Yuliang; Chai, Zhifang; Gao, Xueyun; Earnest, Thomas; Jiang, Huaidong

2016-01-01

High-resolution imaging offers one of the most promising approaches for exploring and understanding the structure and function of biomaterials and biological systems. X-ray free-electron lasers (XFELs) combined with coherent diffraction imaging can theoretically provide high-resolution spatial information regarding biological materials using a single XFEL pulse. Currently, the application of this method suffers from the low scattering cross-section of biomaterials and X-ray damage to the sample. However, XFELs can provide pulses of such short duration that the data can be collected using the “diffract and destroy” approach before the effects of radiation damage on the data become significant. These experiments combine the use of enhanced coherent diffraction imaging with single-shot XFEL radiation to investigate the cellular architecture of Staphylococcus aureus with and without labeling by gold (Au) nanoclusters. The resolution of the images reconstructed from these diffraction patterns were twice as high or more for gold-labeled samples, demonstrating that this enhancement method provides a promising approach for the high-resolution imaging of biomaterials and biological systems. PMID:27659203

Single-pulse enhanced coherent diffraction imaging of bacteria with an X-ray free-electron laser.

PubMed

Fan, Jiadong; Sun, Zhibin; Wang, Yaling; Park, Jaehyun; Kim, Sunam; Gallagher-Jones, Marcus; Kim, Yoonhee; Song, Changyong; Yao, Shengkun; Zhang, Jian; Zhang, Jianhua; Duan, Xiulan; Tono, Kensuke; Yabashi, Makina; Ishikawa, Tetsuya; Fan, Chunhai; Zhao, Yuliang; Chai, Zhifang; Gao, Xueyun; Earnest, Thomas; Jiang, Huaidong

2016-09-23

High-resolution imaging offers one of the most promising approaches for exploring and understanding the structure and function of biomaterials and biological systems. X-ray free-electron lasers (XFELs) combined with coherent diffraction imaging can theoretically provide high-resolution spatial information regarding biological materials using a single XFEL pulse. Currently, the application of this method suffers from the low scattering cross-section of biomaterials and X-ray damage to the sample. However, XFELs can provide pulses of such short duration that the data can be collected using the "diffract and destroy" approach before the effects of radiation damage on the data become significant. These experiments combine the use of enhanced coherent diffraction imaging with single-shot XFEL radiation to investigate the cellular architecture of Staphylococcus aureus with and without labeling by gold (Au) nanoclusters. The resolution of the images reconstructed from these diffraction patterns were twice as high or more for gold-labeled samples, demonstrating that this enhancement method provides a promising approach for the high-resolution imaging of biomaterials and biological systems.

Relativistic Transparency Experiments at the Trident Laser

NASA Astrophysics Data System (ADS)

Cobble, J. A.; Palaniyappan, S.; Gautier, D. C.; Kim, Y. H.; Clark, D. D.; Johnson, R. P.; Shimada, T.; Fernandez, J. C.; Herrmann, H. W.

2013-10-01

With near-diffraction-limited irradiance of 3 × 1020 W/cm2 on target and prelase contrast better than 10-9, we have accessed the regime of relativistic transparency (RT) at the Trident Laser. The goal was to assess electron debris emitted from the target rear surface with phase-contrast imaging (PCI) and current density measurements (hence, the total electron current). Companion diagnostics show whether the experiments are in the target-normal-sheath-acceleration mode or in the RT regime. The superb laser contrast allows us to shoot targets as thin as 50 nm. PCI at 527 nm is temporally resolved to 600 fs. It has shown the evolution of electron behavior over tens of ps, including thermal electrons accompanying the ion jet, accelerated to many tens of MeV earlier in time. Faraday-cup measurements indicate the transfer of many uC of charge during the laser drive. As a ride-along experiment using a gas Cherenkov detector (GCD), we have detected gamma rays of energy >5 MeV. This radiation has a prompt component and a lesser source, driven by accelerated ions, that is time resolved by the GCD. The ion time of flight is compared to Thomson parabola data. Electron energy spectra are also collected. This work has been performed under the auspices of the US DOE contract number DE-AC52-06NA25396.

Green synthesis of BiVO4 nanorods via aqueous extracts of Callistemon viminalis

NASA Astrophysics Data System (ADS)

Mohamed, H. E. A.; Sone, B. T.; Fuku, X. G.; Dhlamini, M. S.; Maaza, M.

2018-05-01

Nowadays, the development of efficient green chemistry methods for synthesis of metal oxides nanoparticles has become a major focus of researchers. These methods are being investigated in order to find an eco-friendly technique for production of well-characterized nanoparticles. In this contribution we report for the first time, the synthesis and structural characterization of n-type Bismuth vanadate (BiVO4) nanoparticles using aqueous extracts of Callistemon viminalis as a chelating agent. To ascertain the formation of BiVO4, X-Ray diffraction analysis (XRD), Scanning Electron Microscopy (SEM), High Resolution Transmission Electron Microscopy (TEM), Selected Area Electron Diffraction (SAED), Electron Dispersion X-ray Spectroscopy (EDS), Fourier Transform Infra-red Spectroscopy (FTIR), and Photoluminescence spectroscopy (PL) were carried out.

Large-scale synthesis of monodisperse magnesium ferrite via an environmentally friendly molten salt route.

PubMed

Lou, Zhengsong; He, Minglong; Wang, Ruikun; Qin, Weiwei; Zhao, Dejian; Chen, Changle

2014-02-17

Sub-micrometer-sized magnesium ferrite spheres consisting of uniform small particles have been prepared using a facile, large-scale solid-state reaction employing a molten salt technique. Extensive structural characterization of the as-prepared samples has been performed using scanning electron microscope, transmission electron microscopy, high-resolution transmission electron microscopy, selected area electron diffraction, and X-ray diffraction. The yield of the magnesium ferrite sub-micrometer spheres is up to 90%, and these sub-micrometer spheres are made up of square and rectangular nanosheets. The magnetic properties of magnesium ferrite sub-micrometer spheres are investigated, and the magnetization saturation value is about 24.96 emu/g. Moreover, the possible growth mechanism is proposed based on the experimental results.

Direct observation of anti-phase boundaries in heteroepitaxy of GaSb thin films grown on Si(001) by transmission electron microscopy

NASA Astrophysics Data System (ADS)

Woo, S. Y.; Hosseini Vajargah, S.; Ghanad-Tavakoli, S.; Kleiman, R. N.; Botton, G. A.

2012-10-01

Unambiguous identification of anti-phase boundaries (APBs) in heteroepitaxial films of GaSb grown on Si has been so far elusive. In this work, we present conventional transmission electron microscopy (TEM) diffraction contrast imaging using superlattice reflections, in conjunction with convergent beam electron diffraction analysis, to determine a change in polarity across APBs in order to confirm the presence of anti-phase disorder. In-depth analysis of anti-phase disorder is further supported with atomic resolution high-angle annular dark-field scanning transmission electron microscopy. The nature of APBs in GaSb is further elucidated by a comparison to previous results for GaAs epilayers grown on Si.

Heterogeneous to homogeneous melting transition visualized with ultrafast electron diffraction

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

None

The ultrafast laser excitation of matters leads to non-equilibrium states with complex solid-liquid phase transition dynamics. We used electron diffraction at mega-electronvolt energies to visualize the ultrafast melting of gold on the atomic scale length. For energy densities approaching the irreversible melting regime, we first observed heterogeneous melting on time scales of 100 ps to 1000 ps, transitioning to homogeneous melting that occurs catastrophically within 10-20 ps at higher energy densities. We showed evidence for the heterogeneous coexistence of solid and liquid. We determined the ion and electron temperature evolution and found superheated conditions. Our results constrain the electron-ion couplingmore » rate, determine the Debye temperature and reveal the melting sensitivity to nucleation seeds.« less

Structural, thermodynamic, and electronic properties of Laves-phase NbMn2 from first principles, x-ray diffraction, and calorimetric experiments

NASA Astrophysics Data System (ADS)

Yan, X.; Chen, Xing-Qiu; Michor, H.; Wolf, W.; Witusiewicz, V. T.; Bauer, E.; Podloucky, R.; Rogl, P.

2018-03-01

By combining theoretical density functional theory (DFT) and experimental studies, structural and magnetic phase stabilities and electronic structural, elastic, and vibrational properties of the Laves-phase compound NbMn2 have been investigated for the C14, C15, and C36 crystal structures. At low temperatures C14 is the ground-state structure, with ferromagnetic and antiferromagnetic orderings being degenerate in energy. The degenerate spin configurations result in a rather large electronic density of states at Fermi energy for all magnetic cases, even for the spin-polarized DFT calculations. Based on the DFT-derived phonon dispersions and densities of states, temperature-dependent free energies were derived for the ferromagnetic and antiferromagnetic C14 phase, demonstrating that the spin-configuration degeneracy possibly exists up to finite temperatures. The heat of formation Δ298H0=-45.05 ±3.64 kJ (molf .u .NbMn2) -1 was extracted from drop isoperibolic calorimetry in a Ni bath. The DFT-derived enthalpy of formation of NbMn2 is in good agreement with the calorimetric measurements. Second-order elastic constants for NbMn2 as well as for related compounds were calculated.

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

Chang, Y.L.; Chen, P.Y.; Tsai, Y.T.

The crystallography of lenticular martensite, which formed in coarse austenite grains (size about 80 μm) after subzero treatment at − 196 °C (liquid nitrogen) for different holding times, was investigated using electron backscatter diffraction (EBSD). For the sample treated with 15 min of isothermal holding, more than 50 martensite plates (with a thickness of larger than 1 μm) that formed within a coarse austenite grain were employed to obtain the pole figures. The pole figures clearly indicated that the individual plate of lenticular martensite approximately adopted the Kurdjumov–Sachs (K–S) orientation relationship with respect to the austenite matrix. For the samplemore » treated with 30 s of isothermal holding, a few martensite plates that formed in variant pairings in a coarse austenite grain were analyzed. The results showed that zigzag couplings (including spear couplings), the major product of plate martensite, had an absolute dominance of a specific variant pair (V1/V17). The orientation gradient within a lenticular martensite plate was also measured using convergent beam electron diffraction (CBED). The evidence strongly suggests that the spread in diffracted intensity within pole figures is related to the misorientation gradient within the lenticular martensite plate. - Highlights: • The orientation relationship between lenticular martensite and austenite was investigated by pole figures via Electron Backscatter Diffraction (EBSD). • The initial stage of lenticular martensite formation was investigated, excluding interference from hard impingement. • In addition to EBSD, convergent beam electron diffraction (CBED) was used to measure the misorientation angle from the midrib to the untwinned region in lenticular martensite plate. • Zigzag couplings (including spear couplings), the major product of plate martensite, had an absolute dominance of a specific variant pair (V1/V17).« less

The molecular and crystal structure of dextrans: a combined electron and X-ray diffraction study. II. A low temperature, hydrated polymorph.

PubMed

Guizard, C; Chanzy, H; Sarko, A

1985-06-05

The crystal and molecular structure of a dextran hydrate has been determined through combined electron and X-ray diffraction analysis, aided by stereochemical model refinement. A total of 65 hk0 electron diffraction intensities were measured on frozen single crystals held at the temperature of liquid nitrogen, to a resolution limit of 1.6 A. The X-ray intensities were measured from powder patterns recorded from collections of the single crystals. The structure crystallizes in a monoclinic unit cell with parameters a = 25.71 A, b = 10.21 A, c (chain axis) = 7.76 A and beta = 91.3 degrees. The space group is P2(1) with b axis unique. The unit cell contains six chains and eight water molecules, with three chains of the same polarity and four water molecules constituting the asymmetric unit. Along the chain direction the asymmetric unit is a dimer residue; however, the individual glucopyranose residues are very nearly related by a molecular 2-fold screw axis. The conformation of the chain is very similar to that in the anhydrous structure, but the chain packing differs in the two structures in that the rotational positions of the chains about the helix axes (the chain setting angles) are considerably different. The chains still pack in the form of sheets that are separated by water molecules. The difference in the chain setting angles between the anhydrous and hydrate structures corresponds to the angle between like unit cell axes observed in the diffraction diagrams recorded from hybrid crystals containing both polymorphs. Despite some beam damage effects, the structure was determined to a satisfactory degree of agreement, with the residuals R''(electron diffraction) = 0.258 and R(X-ray) = 0.127.

Diffraction and pulse slippage in the Boeing 1 kW FEL oscillator

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

Blau, J.; Wong, R.K.; Colson, W.B.

1995-12-31

A four-dimensional simulation in x, y, z, and t, including betatron motion of the electrons, is used to study the combined effects of diffraction, pulse slippage and desynchronism in the Boeing 1 kW FEL oscillator.

Start-to-end simulation of single-particle imaging using ultra-short pulses at the European X-ray Free-Electron Laser

DOE PAGES

Fortmann-Grote, Carsten; Buzmakov, Alexey; Jurek, Zoltan; ...

2017-09-01

Single-particle imaging with X-ray free-electron lasers (XFELs) has the potential to provide structural information at atomic resolution for non-crystalline biomolecules. This potential exists because ultra-short intense pulses can produce interpretable diffraction data notwithstanding radiation damage. This paper explores the impact of pulse duration on the interpretability of diffraction data using comprehensive and realistic simulations of an imaging experiment at the European X-ray Free-Electron Laser. In conclusion, it is found that the optimal pulse duration for molecules with a few thousand atoms at 5 keV lies between 3 and 9 fs.

Micro-emulsion-assisted synthesis of ZnS nanospheres and their photocatalytic activity

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

Li Yao; He Xiaoyan; Cao Minhua

2008-11-03

ZnS nanospheres with rough surface were synthesized by using a micro-emulsion-assisted solvothemal process. The molar ratio of [water]/[surfactant] played an important role in controlling the size of the ZnS nanospheres. X-ray powder diffraction (XRD), transmission electron microscopy (TEM), field emission-scanning electron microscope (FE-SEM), and selected area electron diffraction (SAED) were used for the characterization of the resulting ZnS nanospheres. A possible formation mechanism was proposed. These ZnS nanospheres exhibited a good photocatalytic activity for degradation of an aqueous p-nitrophenol solution and the total organic carbon (TOC) of the degradation product has also been investigated.

Start-to-end simulation of single-particle imaging using ultra-short pulses at the European X-ray Free-Electron Laser

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

Fortmann-Grote, Carsten; Buzmakov, Alexey; Jurek, Zoltan

Single-particle imaging with X-ray free-electron lasers (XFELs) has the potential to provide structural information at atomic resolution for non-crystalline biomolecules. This potential exists because ultra-short intense pulses can produce interpretable diffraction data notwithstanding radiation damage. This paper explores the impact of pulse duration on the interpretability of diffraction data using comprehensive and realistic simulations of an imaging experiment at the European X-ray Free-Electron Laser. In conclusion, it is found that the optimal pulse duration for molecules with a few thousand atoms at 5 keV lies between 3 and 9 fs.

Surface Diagnostics in Tribology Technology and Advanced Coatings Development

NASA Technical Reports Server (NTRS)

Miyoshi, Kazuhisa

1999-01-01

This paper discusses the methodologies used for surface property measurement of thin films and coatings, lubricants, and materials in the field of tribology. Surface diagnostic techniques include scanning electron microscopy, transmission electron microscopy, atomic force microscopy, stylus profilometry, x-ray diffraction, electron diffraction, Raman spectroscopy, Rutherford backscattering, elastic recoil spectroscopy, and tribology examination. Each diagnostic technique provides specific measurement results in its own unique way. In due course it should be possible to coordinate the different pieces of information provided by these diagnostic techniques into a coherent self-consistent description of the surface properties. Examples are given on the nature and character of thin diamond films.

Comparison of dislocation content measured with transmission electron microscopy and micro-Laue diffraction based streak analysis

DOE PAGES

Zhang, C.; Balachandran, S.; Eisenlohr, P.; ...

2017-10-04

The subsurface dislocation content in a Ti-5Al-2.5Sn (wt%) uniaxial tension sample deformed at ambient temperature was characterized by peak streak analysis of micro-Laue diffraction patterns collected non-destructively by differential aperture X-raymicroscopy, and with focused ion beam transmission electron microscopy of material in the same volume. This comparison reveals that micro-Laue diffraction streak analysis based on an edge dislocation assumption can accurately identify the dominant dislocation slip system history (Burgers vector and plane observed by TEM), despite the fact that dislocations have predominantly screw character. As a result, other dislocations identified by TEM were not convincingly discernible from the peak streakmore » analysis.« less

Comparison of dislocation content measured with transmission electron microscopy and micro-Laue diffraction based streak analysis

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

Zhang, C.; Balachandran, S.; Eisenlohr, P.

The subsurface dislocation content in a Ti-5Al-2.5Sn (wt%) uniaxial tension sample deformed at ambient temperature was characterized by peak streak analysis of micro-Laue diffraction patterns collected non-destructively by differential aperture X-raymicroscopy, and with focused ion beam transmission electron microscopy of material in the same volume. This comparison reveals that micro-Laue diffraction streak analysis based on an edge dislocation assumption can accurately identify the dominant dislocation slip system history (Burgers vector and plane observed by TEM), despite the fact that dislocations have predominantly screw character. As a result, other dislocations identified by TEM were not convincingly discernible from the peak streakmore » analysis.« less

High resolution electron backscatter diffraction (EBSD) data from calcite biominerals in recent gastropod shells.

PubMed

Pérez-Huerta, Alberto; Dauphin, Yannicke; Cuif, Jean Pierre; Cusack, Maggie

2011-04-01

Electron backscatter diffraction (EBSD) is a microscopy technique that reveals in situ crystallographic information. Currently, it is widely used for the characterization of geological materials and in studies of biomineralization. Here, we analyze high resolution EBSD data from biogenic calcite in two mollusk taxa, Concholepas and Haliotis, previously used in the understanding of complex biomineralization and paleoenvironmental studies. Results indicate that Concholepas has less ordered prisms than in Haliotis, and that in Concholepas the level of order is not homogenous in different areas of the shell. Overall, the usefulness of data integration obtained from diffraction intensity and crystallographic orientation maps, and corresponding pole figures, is discussed as well as its application to similar studies. © 2010 Elsevier Ltd. All rights reserved.

Investigations in space-related molecular biology. [cryo-electron microscopic and diffraction studies on terrestrial and extraterrestrial specimens

NASA Technical Reports Server (NTRS)

Fernandez-Moran, H.; Pritzker, A. N.

1974-01-01

Improved instrumentation and preparation techniques for high resolution, high voltage cryo-electron microscopic and diffraction studies on terrestrial and extraterrestrial specimens are reported. Computer correlated ultrastructural and biochemical work on hydrated and dried cell membranes and related biological systems provided information on membrane organization, ice crystal formation and ordered water, RNA virus linked to cancer, lunar rock samples, and organometallic superconducting compounds. Apollo 11, 12, 14, and 15 specimens were analyzed

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

Ultrafast large-amplitude relocation of electronic charge in ionic crystals

PubMed Central

Zamponi, Flavio; Rothhardt, Philip; Stingl, Johannes; Woerner, Michael; Elsaesser, Thomas

2012-01-01

The interplay of vibrational motion and electronic charge relocation in an ionic hydrogen-bonded crystal is mapped by X-ray powder diffraction with a 100 fs time resolution. Photoexcitation of the prototype material KH2PO4 induces coherent low-frequency motions of the PO4 tetrahedra in the electronically excited state of the crystal while the average atomic positions remain unchanged. Time-dependent maps of electron density derived from the diffraction data demonstrate an oscillatory relocation of electronic charge with a spatial amplitude two orders of magnitude larger than the underlying vibrational lattice motions. Coherent longitudinal optical and tranverse optical phonon motions that dephase on a time scale of several picoseconds, drive the charge relocation, similar to a soft (transverse optical) mode driven phase transition between the ferro- and paraelectric phase of KH2PO4. PMID:22431621

Application of Brazilian kaolinite clay as adsorbent to removal of U(VI) from aqueous solution: Kinetic and thermodynamic of cation-basic interactions

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

Guerra, Denis L., E-mail: denis@cpd.ufmt.b; Leidens, Victor L.; Viana, Rubia R.

2010-05-15

The compound N{sup 1}-[3-(trimethoxysilyl)propyl]diethylenetriamine was anchored onto Amazon kaolinite surface by heterogeneous route. The modified and natural kaolinite samples were characterized by transmission electron microscopy, scanning electron microscopic, X-ray diffraction, and nuclear magnetic nuclei of {sup 29}Si and {sup 13}C. The well-defined peaks obtained in the {sup 13}C NMR spectrum in the 5.0-62.1 ppm region confirmed the attachment of organic functional groups as pendant chains bonded into the porous clay. The ability of these materials to remove U(VI) from aqueous solution was followed by a series of adsorption isotherms adjusted to a Sips equation at room temperature and pH 4.0.more » The kinetic parameters analyzed by the Lagergren and Elovich models gave a good fit for a pseudo-second order reaction with k{sub 2} values 16.0 and 25.1 mmol g{sup -1} min{sup -1} ranges for natural and modified kaolinite clays, respectively. The energetic effects caused by metal ion adsorption were determined through calorimetric titrations. - Graphical abstract: This investigation reports the use of original and modified kaolinites as alternative absorbents. The compound N-[3-trimethoxysilyl)propyl]diethylenetriamine was anchored onto Amazon kaolinite surface by heterogeneous route.« less

Amazon kaolinite functionalized with diethylenetriamine moieties for U(VI) removal: thermodynamic of cation-basic interactions.

PubMed

Guerra, Denis L; Leidens, Victor L; Viana, Rúbia R; Airoldi, Claudio

2010-08-15

The compound N-[3-(trimethoxysilyl)propyl]diethylenetriamine (MPDET) was anchored onto Amazon kaolinite surface (KLT) by heterogeneous route. The modified and natural kaolinite clay samples were characterized by transmission electron microscopy (TEM), scanning electron microscopic (SEM), N(2) adsorption, powder X-ray diffraction, thermal analysis, ion exchange capacities, and nuclear magnetic nuclei of (29)Si and (13)C. The well-defined peaks obtained in the (13)C NMR spectrum in the 5.0-62.1 ppm region confirmed the attachment of organic functional groups as pendant chains bonded into the porous clay. The adsorption of uranyl on natural (KLT) and modified (KLT(MPDET)) kaolinite clays was investigated as a function of the solution pH, metal concentration, temperature, and ionic strength. The ability of these materials to remove U(VI) from aqueous solution was followed by a series of adsorption isotherms adjusted to a Sips equation at room temperature and pH 4.0. The maximum number of moles adsorbed was determined to be 8.37 x 10(-3) and 13.87 x 10(-3) mmol g(-1) for KLT and KLT(MPDET) at 298 K, respectively. The energetic effects (Delta(int)H, Delta(int)G, and Delta(int)S) caused by metal cations adsorption were determined through calorimetric titrations. Copyright 2010. Published by Elsevier B.V.

New modes of electron microscopy for materials science enabled by fast direct electron detectors

NASA Astrophysics Data System (ADS)

Minor, Andrew

There is an ongoing revolution in the development of electron detector technology that has enabled modes of electron microscopy imaging that had only before been theorized. The age of electron microscopy as a tool for imaging is quickly giving way to a new frontier of multidimensional datasets to be mined. These improvements in electron detection have enabled cryo-electron microscopy to resolve the three-dimensional structures of non-crystalized proteins, revolutionizing structural biology. In the physical sciences direct electron detectors has enabled four-dimensional reciprocal space maps of materials at atomic resolution, providing all the structural information about nanoscale materials in one experiment. This talk will highlight the impact of direct electron detectors for materials science, including a new method of scanning nanobeam diffraction. With faster detectors we can take a series of 2D diffraction patterns at each position in a 2D STEM raster scan resulting in a four-dimensional data set. For thin film analysis, direct electron detectors hold the potential to enable strain, polarization, composition and electrical field mapping over relatively large fields of view, all from a single experiment.

Joint Services Electronics Program.

DTIC Science & Technology

1985-12-01

NavyOffice of Naval Research 800 Ouincy Street Arlington, Virginia -*i. I. This document has been approved I-- for pjiblic release and salo; its C=3...Type of Report & Period Covered.- Department of the Navy Annual Report - Office of Naval Research Oct. 1984- Sept. 1985 . 800 Quincy Street 14...TECHNOLOGY TRANSITION 1 III. RESEARCH SUMMARY 10 A. DIFFRACTION STUDIES/ 10 - - 4.4 1. Diffraction by Non-Conducting Surfaces 10 (a) Diffraction by a

Quantitative theory of diffraction by cylindrical scroll nanotubes.

PubMed

Khadiev, Azat; Khalitov, Zufar

2018-05-01

A quantitative theory of Fraunhofer diffraction by right- and left-handed multiwalled cylindrical scroll nanotubes is developed on the basis of the kinematical approach. The proposed theory is mainly dedicated to structural studies of individual nanotubes by the selected-area electron diffraction technique. Strong and diffuse reflections of the scroll nanotube were studied and explicit formulas that govern relations between the direct and reciprocal lattice of the scroll nanotube are achieved.

From quantum to classical interactions between a free electron and a surface

NASA Astrophysics Data System (ADS)

Beierle, Peter James

Quantum theory is often cited as being one of the most empirically validated theories in terms of its predictive power and precision. These attributes have led to numerous scientific discoveries and technological advancements. However, the precise relationship between quantum and classical physics remains obscure. The prevailing description is known as decoherence theory, where classical physics emerges from a more general quantum theory through environmental interaction. Sometimes referred to as the decoherence program, it does not solve the quantum measurement problem. We believe experiments performed between the microscopic and macroscopic world may help finish the program. The following considers a free electron that interacts with a surface (the environment), providing a controlled decoherence mechanism. There are non-decohering interactions to be examined and quantified before the weaker decohering effects are filtered out. In the first experiment, an electron beam passes over a surface that's illuminated by low-power laser light. This induces a surface charge redistribution causing the electron deflection. This phenomenon's parameters are investigated. This system can be well understood in terms of classical electrodynamics, and the technological applications of this electron beam switch are considered. Such phenomena may mask decoherence effects. A second experiment tests decoherence theory by introducing a nanofabricated diffraction grating before the surface. The electron undergoes diffraction through the grating, but as the electron passes over the surface it's predicted by various physical models that the electron will lose its wave interference property. Image charge based models, which predict a larger loss of contrast than what is observed, are falsified (despite experiencing an image charge force). A theoretical study demonstrates how a loss of contrast may not be due to the irreversible process decoherence, but dephasing (a reversible process due to randomization of the wavefunction's phase). To resolve this ambiguity, a correlation function on an ensemble of diffraction patterns is analyzed after an electron undergoes either process in a path integral calculation. The diffraction pattern is successfully recovered for dephasing, but not for decoherence, thus verifying it as a potential tool in experimental studies to determine the nature of the observed process.

High-speed classification of coherent X-ray diffraction patterns on the K computer for high-resolution single biomolecule imaging.

PubMed

Tokuhisa, Atsushi; Arai, Junya; Joti, Yasumasa; Ohno, Yoshiyuki; Kameyama, Toyohisa; Yamamoto, Keiji; Hatanaka, Masayuki; Gerofi, Balazs; Shimada, Akio; Kurokawa, Motoyoshi; Shoji, Fumiyoshi; Okada, Kensuke; Sugimoto, Takashi; Yamaga, Mitsuhiro; Tanaka, Ryotaro; Yokokawa, Mitsuo; Hori, Atsushi; Ishikawa, Yutaka; Hatsui, Takaki; Go, Nobuhiro

2013-11-01

Single-particle coherent X-ray diffraction imaging using an X-ray free-electron laser has the potential to reveal the three-dimensional structure of a biological supra-molecule at sub-nanometer resolution. In order to realise this method, it is necessary to analyze as many as 1 × 10(6) noisy X-ray diffraction patterns, each for an unknown random target orientation. To cope with the severe quantum noise, patterns need to be classified according to their similarities and average similar patterns to improve the signal-to-noise ratio. A high-speed scalable scheme has been developed to carry out classification on the K computer, a 10PFLOPS supercomputer at RIKEN Advanced Institute for Computational Science. It is designed to work on the real-time basis with the experimental diffraction pattern collection at the X-ray free-electron laser facility SACLA so that the result of classification can be feedback for optimizing experimental parameters during the experiment. The present status of our effort developing the system and also a result of application to a set of simulated diffraction patterns is reported. About 1 × 10(6) diffraction patterns were successfully classificatied by running 255 separate 1 h jobs in 385-node mode.

High-speed classification of coherent X-ray diffraction patterns on the K computer for high-resolution single biomolecule imaging

PubMed Central

Tokuhisa, Atsushi; Arai, Junya; Joti, Yasumasa; Ohno, Yoshiyuki; Kameyama, Toyohisa; Yamamoto, Keiji; Hatanaka, Masayuki; Gerofi, Balazs; Shimada, Akio; Kurokawa, Motoyoshi; Shoji, Fumiyoshi; Okada, Kensuke; Sugimoto, Takashi; Yamaga, Mitsuhiro; Tanaka, Ryotaro; Yokokawa, Mitsuo; Hori, Atsushi; Ishikawa, Yutaka; Hatsui, Takaki; Go, Nobuhiro

2013-01-01

Single-particle coherent X-ray diffraction imaging using an X-ray free-electron laser has the potential to reveal the three-dimensional structure of a biological supra-molecule at sub-nanometer resolution. In order to realise this method, it is necessary to analyze as many as 1 × 106 noisy X-ray diffraction patterns, each for an unknown random target orientation. To cope with the severe quantum noise, patterns need to be classified according to their similarities and average similar patterns to improve the signal-to-noise ratio. A high-speed scalable scheme has been developed to carry out classification on the K computer, a 10PFLOPS supercomputer at RIKEN Advanced Institute for Computational Science. It is designed to work on the real-time basis with the experimental diffraction pattern collection at the X-ray free-electron laser facility SACLA so that the result of classification can be feedback for optimizing experimental parameters during the experiment. The present status of our effort developing the system and also a result of application to a set of simulated diffraction patterns is reported. About 1 × 106 diffraction patterns were successfully classificatied by running 255 separate 1 h jobs in 385-node mode. PMID:24121336

Experimental and theoretical calculation studies on the structure elucidation and absolute configuration of calyxins from Alpinia katsumadai.

PubMed

Wang, Xiao-Bing; Yang, Chang-Shui; Luo, Jian-Guang; Zhang, Chao; Luo, Jun; Yang, Ming-Hua; Kong, Ling-Yi

2017-06-01

Six novel calyxins, named calyxin T-W, ent-calyxin T and ent-calyxin U were isolated from the seeds of Alpinia katsumadai Hayata. Their relative configurations were elucidated by means of detailed UV, IR, NMR and MS spectroscopic data. Their absolute configurations were assigned by collaborative studies on single crystal X-ray diffraction analysis, Mosher's method, electronic circular dichroism (ECD), optical rotation and theoretical calculations. These compounds are Friedel-Cranft alkylation adducts composed of coexisted diarylheptanoids and flavanone from the seeds of Alpinia katsumadai. The antiproliferative activity of the six compounds against NCI-H460, HeLa, SMMC-7721 and HCT-116 cell lines was also reported, and most of them showed moderate to strong activities. Copyright © 2017. Published by Elsevier B.V.

Diffraction of electrons at intermediate energies

NASA Astrophysics Data System (ADS)

Ascolani, H.; Barrachina, R. O.; Guraya, M. M.; Zampieri, G.

1992-08-01

We present a theory of the elastic scattering of electrons from crystalline surfaces that contains both low-energy-electron-diffraction (LEED) effects at low energies and x-ray-photoelectron- and Auger-electron-diffraction (XPD/AED) effects at intermediate energies. The theory is based on a cluster-type approach to the scattering problem and includes temperature effects. The transition from one regime to the other may be explained as follows: At low energies all the scattered waves add coherently, and the intensity is dominated by LEED effects. At intermediate energies the thermal vibration of the atoms destroys the long-range coherency responsible for the LEED peaks, but affects little the interference of those waves that share parts of their paths inside the solid. Thus, the interference of these waves comes to dominate the intensity, giving rise to structures similar to those observed in XPD/AED experiments. We perform a calculation of the elastic reflection of electrons from Cu(001) that is in good agreement with the experiment in the range 200-1500 eV. At low energies the intensity is dominated by LEED peaks; at 400 eV LEED peaks and XPD/AED structures coexist; and above this energy the intensity is dominated by the latter. We analyze the contributions to the intensity at intermediate energies of the interferences in the incoming and outgoing parts of the electron path.

Non-destructive Quantitative Phase Analysis and Microstructural Characterization of Zirconium Coated U-10Mo Fuel Foils via Neutron Diffraction

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

Cummins, Dustin Ray; Vogel, Sven C.; Hollis, Kendall Jon

2016-10-18

This report uses neutron diffraction to investigate the crystal phase composition of uranium-molybdenum alloy foils (U-10Mo) for the CONVERT MP-1 Reactor Conversion Project, and determines the effect on alpha-uranium contamination following the deposition of a Zr metal diffusion layer by various methods: plasma spray deposition of Zr powders at LANL and hot co-rolling with Zr foils at BWXT. In summary, there is minimal decomposition of the gamma phase U-10Mo foil to alpha phase contamination following both plasma spraying and hot co-rolling. The average unit cell volume, i.e. lattice spacing, of the Zr layer can be mathematically extracted from the diffractionmore » data; co-rolled Zr matches well with literature values of bulk Zr, while plasma sprayed Zr shows a slight increase in the lattice spacing, indicative of interstitial oxygen in the lattice. Neutron diffraction is a beneficial alternative to conventional methods of phase composition, i.e. x ray diffraction (XRD) and destructive metallography. XRD has minimal penetration depth in high atomic number materials, particularly uranium, and can only probe the first few microns of the fuel plate; neutrons pass completely through the foil, allowing for bulk analysis of the foil composition and no issues with addition of cladding layers, as in the final, aluminum-clad reactor fuel plates. Destructive metallography requires skilled technicians, cutting of the foil into small sections, hazardous etching conditions, long polishing and microscopy times, etc.; the neutron diffraction system has an automated sample loader and can fit larger foils, so there is minimal analysis preparation; the total spectrum acquisition time is ~ 1 hour per sample. The neutron diffraction results are limited by spectra refinement/calculation times and the availability of the neutron beam source. In the case of LANSCE at Los Alamos, the beam operates ~50% of the year. Following the lessons learned from these preliminary results, optimizations to the process and analysis can be made, and neutron diffraction can become a viable and efficient technique for gamma/alpha phase composition determination for nuclear fuels.« less

Diffractive imaging of a rotational wavepacket in nitrogen molecules with femtosecond megaelectronvolt electron pulses

DOE PAGES

Yang, Jie; Guehr, Markus; Vecchione, Theodore; ...

2016-04-05

Imaging changes in molecular geometries on their natural femtosecond timescale with sub-Angström spatial precision is one of the critical challenges in the chemical sciences, as the nuclear geometry changes determine the molecular reactivity. For photoexcited molecules, the nuclear dynamics determine the photoenergy conversion path and efficiency. Here we report a gas-phase electron diffraction experiment using megaelectronvolt (MeV) electrons, where we captured the rotational wavepacket dynamics of nonadiabatically laser-aligned nitrogen molecules. We achieved a combination of 100 fs root-mean-squared temporal resolution and sub-Angstrom (0.76 Å) spatial resolution that makes it possible to resolve the position of the nuclei within the molecule.more » In addition, the diffraction patterns reveal the angular distribution of the molecules, which changes from prolate (aligned) to oblate (anti-aligned) in 300 fs. Lastly, our results demonstrate a significant and promising step towards making atomically resolved movies of molecular reactions.« less

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.

Monochromatic X-ray sources based on a mechanism of real and virtual photon diffraction in crystals

NASA Astrophysics Data System (ADS)

Wagner, A. R.; Kuznetsov, S. I.; Potylitsyn, A. P.; Razin, S. V.; Uglov, S. R.; Zabaev, V. N.

2008-09-01

A source of monochromatic X-ray radiation is wanted in industry, science, medicine and so on. Many ways of making such a source are known. The present work describes two mechanisms for the creation of a monochromatic X-ray beam, which are parametric X-ray radiation (PXR) and bremsstrahlung diffraction (DBS). Both the experiments were carried out using an electron beam at a microtron. During the first experiment, the DBS process was investigated as a scattering of the Bremsstrahlung (BS) beam on the crystallographic surfaces of tungsten and pyrolytic graphite crystals. The second experiment consisted in the registration of the PXR and DBS yield during the passage of the electrons through the same crystals as in the first experiment. The spectral and orientation radiation characteristics and simulation results obtained for the DBS and PXR processes are presented. It is shown that the usage of mosaic crystalline targets is rather useful in order to obtain a monochromatic X-ray source based on bremsstrahlung diffraction from moderately relativistic electrons.

Molecular structure and conformational preferences of gaseous 1-iodo-1-silacyclohexane

NASA Astrophysics Data System (ADS)

Belyakov, A. V.; Baskakov, A. A.; Berger, R. J. F.; Mitzel, N. W.; Oberhammer, H.; Arnason, I.; Wallevik, S. Ò.

2012-03-01

The molecular structure of the axial and equatorial conformers of 1-iodo-1-silacyclohexane, CH2(CH2CH2)2SiH-I, as well as thermodynamic equilibrium between these species were investigated by means of gas-phase electron diffraction (GED) and quantum chemical calculations up to MP2(full)/SDB-AUG-CC-pVTZ level of theory (MP2). According to electron diffraction data, the vapor of this compound comprises a mixture of conformers with chair conformation and Cs symmetry differing in the axial and equatorial position of the Si-I bond (axial = 73(7) mol%/equatorial = 27(7) mol%) at T = 352 K. This corresponds to a free energy difference of A = -0.59(22) kcal mol-1. The observed gas-phase electron diffraction parameters are in good agreement with those obtained from theory. NBO analysis revealed that axial conformer of 1-iodo-1-silacyclohexane is an example for electrostatic stabilization of a conformer which is unfavorable in terms of steric and conjugation interaction.

Auger electron diffraction study of V/Fe(100) interface formation

NASA Astrophysics Data System (ADS)

Huttel, Y.; Avila, J.; Asensio, M. C.; Bencok, P.; Richter, C.; Ilakovac, V.; Heckmann, O.; Hricovini, K.

1998-05-01

Vanadium atoms present a magnetic moment different to zero when they are part of a thin film deposited on Fe or as a bimetallic Fe-V alloy. The understanding of this phenomenon can only be achieved with a correct structural description of these types of systems. We report an Auger electron diffraction investigation of V films grown on body cubic centred (b.c.c.) Fe(100) substrates. Angular-scanned Auger electron diffraction (AED) patterns of V L 23M 23M 4 (473 eV) and Fe L 3VV (703 eV) show the formation of a well-ordered V/Fe interface even at room temperature. The AED patterns of V films in the range of vanadium submonolayer provide evidence of an isotropic Auger emission, indicating the absence of interdiffusion of V atoms into the Fe substrate and absence of cluster growth of the V film. The annealing of these films up to 400°C does not activate the substitution of the topmost Fe surface layers by V atoms.

Beyond a phenomenological description of magnetostriction

DOE PAGES

Reid, A. H.; Shen, X.; Maldonado, P.; ...

2018-01-26

Magnetostriction, the strain induced by a change in magnetization, is a universal effect in magnetic materials. Owing to the difficulty in unraveling its microscopic origin, it has been largely treated phenomenologically. Here in this paper, we show how the source of magnetostriction—the underlying magnetoelastic stress—can be separated in the time domain, opening the door for an atomistic understanding. X-ray and electron diffraction are used to separate the sub-picosecond spin and lattice responses of FePt nanoparticles. Following excitation with a 50-fs laser pulse, time-resolved X-ray diffraction demonstrates that magnetic order is lost within the nanoparticles with a time constant of 146more » fs. Ultrafast electron diffraction reveals that this demagnetization is followed by an anisotropic, three-dimensional lattice motion. Analysis of the size, speed, and symmetry of the lattice motion, together with ab initio calculations accounting for the stresses due to electrons and phonons, allow us to reveal the magnetoelastic stress generated by demagnetization.« less

Enabling X-ray free electron laser crystallography for challenging biological systems from a limited number of crystals

DOE PAGES

Uervirojnangkoorn, Monarin; Zeldin, Oliver B.; Lyubimov, Artem Y.; ...

2015-03-17

There is considerable potential for X-ray free electron lasers (XFELs) to enable determination of macromolecular crystal structures that are difficult to solve using current synchrotron sources. Prior XFEL studies often involved the collection of thousands to millions of diffraction images, in part due to limitations of data processing methods. We implemented a data processing system based on classical post-refinement techniques, adapted to specific properties of XFEL diffraction data. When applied to XFEL data from three different proteins collected using various sample delivery systems and XFEL beam parameters, our method improved the quality of the diffraction data as well as themore » resulting refined atomic models and electron density maps. Moreover, the number of observations for a reflection necessary to assemble an accurate data set could be reduced to a few observations. In conclusion, these developments will help expand the applicability of XFEL crystallography to challenging biological systems, including cases where sample is limited.« less

Enabling X-ray free electron laser crystallography for challenging biological systems from a limited number of crystals

DOE PAGES

Uervirojnangkoorn, Monarin; Zeldin, Oliver B.; Lyubimov, Artem Y.; ...

2015-03-17

There is considerable potential for X-ray free electron lasers (XFELs) to enable determination of macromolecular crystal structures that are difficult to solve using current synchrotron sources. Prior XFEL studies often involved the collection of thousands to millions of diffraction images, in part due to limitations of data processing methods. We implemented a data processing system based on classical post-refinement techniques, adapted to specific properties of XFEL diffraction data. When applied to XFEL data from three different proteins collected using various sample delivery systems and XFEL beam parameters, our method improved the quality of the diffraction data as well as themore » resulting refined atomic models and electron density maps. Moreover, the number of observations for a reflection necessary to assemble an accurate data set could be reduced to a few observations. These developments will help expand the applicability of XFEL crystallography to challenging biological systems, including cases where sample is limited.« less

Enabling X-ray free electron laser crystallography for challenging biological systems from a limited number of crystals

PubMed Central

Uervirojnangkoorn, Monarin; Zeldin, Oliver B; Lyubimov, Artem Y; Hattne, Johan; Brewster, Aaron S; Sauter, Nicholas K; Brunger, Axel T; Weis, William I

2015-01-01

There is considerable potential for X-ray free electron lasers (XFELs) to enable determination of macromolecular crystal structures that are difficult to solve using current synchrotron sources. Prior XFEL studies often involved the collection of thousands to millions of diffraction images, in part due to limitations of data processing methods. We implemented a data processing system based on classical post-refinement techniques, adapted to specific properties of XFEL diffraction data. When applied to XFEL data from three different proteins collected using various sample delivery systems and XFEL beam parameters, our method improved the quality of the diffraction data as well as the resulting refined atomic models and electron density maps. Moreover, the number of observations for a reflection necessary to assemble an accurate data set could be reduced to a few observations. These developments will help expand the applicability of XFEL crystallography to challenging biological systems, including cases where sample is limited. DOI: http://dx.doi.org/10.7554/eLife.05421.001 PMID:25781634

Macromolecular structures probed by combining single-shot free-electron laser diffraction with synchrotron coherent X-ray imaging.

PubMed

Gallagher-Jones, Marcus; Bessho, Yoshitaka; Kim, Sunam; Park, Jaehyun; Kim, Sangsoo; Nam, Daewoong; Kim, Chan; Kim, Yoonhee; Noh, Do Young; Miyashita, Osamu; Tama, Florence; Joti, Yasumasa; Kameshima, Takashi; Hatsui, Takaki; Tono, Kensuke; Kohmura, Yoshiki; Yabashi, Makina; Hasnain, S Samar; Ishikawa, Tetsuya; Song, Changyong

2014-05-02

Nanostructures formed from biological macromolecular complexes utilizing the self-assembly properties of smaller building blocks such as DNA and RNA hold promise for many applications, including sensing and drug delivery. New tools are required for their structural characterization. Intense, femtosecond X-ray pulses from X-ray free-electron lasers enable single-shot imaging allowing for instantaneous views of nanostructures at ambient temperatures. When combined judiciously with synchrotron X-rays of a complimentary nature, suitable for observing steady-state features, it is possible to perform ab initio structural investigation. Here we demonstrate a successful combination of femtosecond X-ray single-shot diffraction with an X-ray free-electron laser and coherent diffraction imaging with synchrotron X-rays to provide an insight into the nanostructure formation of a biological macromolecular complex: RNA interference microsponges. This newly introduced multimodal analysis with coherent X-rays can be applied to unveil nano-scale structural motifs from functional nanomaterials or biological nanocomplexes, without requiring a priori knowledge.

Quantifying Morphological Features of α-U3O8 with Image Analysis for Nuclear Forensics.

PubMed

Olsen, Adam M; Richards, Bryony; Schwerdt, Ian; Heffernan, Sean; Lusk, Robert; Smith, Braxton; Jurrus, Elizabeth; Ruggiero, Christy; McDonald, Luther W

2017-03-07

Morphological changes in U 3 O 8 based on calcination temperature have been quantified enabling a morphological feature to serve as a signature of processing history in nuclear forensics. Five separate calcination temperatures were used to synthesize α-U 3 O 8 , and each sample was characterized using powder X-ray diffraction (p-XRD) and scanning electron microscopy (SEM). The p-XRD spectra were used to evaluate the purity of the synthesized U-oxide; the morphological analysis for materials (MAMA) software was utilized to quantitatively characterize the particle shape and size as indicated by the SEM images. Analysis comparing the particle attributes, such as particle area at each of the temperatures, was completed using the Kolmogorov-Smirnov two sample test (K-S test). These results illustrate a distinct statistical difference between each calcination temperature. To provide a framework for forensic analysis of an unknown sample, the sample distributions at each temperature were compared to randomly selected distributions (100, 250, 500, and 750 particles) from each synthesized temperature to determine if they were statistically different. It was found that 750 particles were required to differentiate between all of the synthesized temperatures with a confidence interval of 99.0%. Results from this study provide the first quantitative morphological study of U-oxides, and reveals the potential strength of morphological particle analysis in nuclear forensics by providing a framework for a more rapid characterization of interdicted uranium oxide samples.

Directional Auger Electron Spectroscopy — Physical Foundations and Applications

NASA Astrophysics Data System (ADS)

Mróz, S.

Experimental data about the dependence of the Auger signal from crystalline samples on the primary beam direction are presented and discussed. It is shown that, for Auger electrons and elastically and inelastically backscattered electrons, maxima of the signal in its dependence on the polar and azimuth angles of the primary beam (in polar and azimuth profiles, respectively) appear when the primary beam is parallel either to one of the close-packed rows of atoms or to one of the densely packed atomic planes in the sample. This indicates that the diffraction of the primary electron beam is responsible for the dependence mentioned above. Mechanisms proposed for simple explanation of this dependence (channeling and forward focusing of primary electrons) are presented and results of their application are discussed. It is shown that both those mechanisms play an important role in the creation of the Auger signal contrast. The possibilities and limitations of the application of polar and azimuth Auger emission profiles in the determination of the surface layer crystalline structure (directional Auger electron spectroscopy — DAES) are presented and discussed. It is shown that the thickness of the investigated surface layer can be decreased up to a few monolayers. Results obtained with DAES are similar to those provided by X-ray photoelectron diffraction (XPD) and Auger electron diffraction (AED), but the DAES experimental equipment is simple and inexpensive and measurements are fast. Finally, experimental systems for DAES are described and examples of DAES applications are presented.

Processing of U-2.5Zr-7.5Nb and U-3Zr-9Nb alloys by sintering process

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

Dos Santos, A. M. M.; Ferraz, W. B.; Lameiras, F. S.

2012-07-01

To minimize the risk of nuclear proliferation, there is worldwide interest in reducing fuel enrichment of research and test reactors. To achieve this objective while still guaranteeing criticality and cycle length requirements, there is need of developing high density uranium metallic fuels. Alloying elements such as Zr, Nb and Mo are added to uranium to improve fuel performance in reactors. In this context, the Centro de Desenvolvimento da Tecnologia Nuclear (CDTN) is developing the U-2.5Zr-7.5Nb and U-3Zr-9Nb (weight %) alloys by the innovative process of sintering that utilizes raw materials in the form of powders. The powders were pressed atmore » 400 MPa and then sintered under a vacuum of about 1x10{sup -4} Torr at temperatures ranging from 1050 deg. to 1500 deg.C. The densities of the alloys were measured geometrically and by hydrostatic method and the phases identified by X ray diffraction (XRD). The microstructures of the pellets were observed by scanning electron microscopy (SEM) and the alloying elements were analyzed by energy dispersive X-ray spectroscopy (EDS). The results obtained showed the fuel density to slightly increase with the sintering temperature. The highest density achieved was approximately 80% of theoretical density. It was observed in the pellets a superficial oxide layer formed during the sintering process. (authors)« less

Ultrafast electron crystallography: Transient structures of molecules, surfaces, and phase transitions

PubMed Central

Ruan, Chong-Yu; Vigliotti, Franco; Lobastov, Vladimir A.; Chen, Songye; Zewail, Ahmed H.

2004-01-01

The static structure of macromolecular assemblies can be mapped out with atomic-scale resolution by using electron diffraction and microscopy of crystals. For transient nonequilibrium structures, which are critical to the understanding of dynamics and mechanisms, both spatial and temporal resolutions are required; the shortest scales of length (0.1–1 nm) and time (10–13 to 10–12 s) represent the quantum limit, the nonstatistical regime of rates. Here, we report the development of ultrafast electron crystallography for direct determination of structures with submonolayer sensitivity. In these experiments, we use crystalline silicon as a template for different adsorbates: hydrogen, chlorine, and trifluoroiodomethane. We observe the coherent restructuring of the surface layers with subangstrom displacement of atoms after the ultrafast heat impulse. This nonequilibrium dynamics, which is monitored in steps of 2 ps (total change ≤10 ps), contrasts that of the nanometer substrate. The effect of adsorbates and the phase transition at higher fluences were also studied through the evolution of streaks of interferences, Bragg spots (and their rocking curves), and rings in the diffraction patterns. We compare these results with kinematical theory and those of x-ray diffraction developed to study bulk behaviors. The sensitivity achieved here, with the 6 orders of magnitude larger cross section than x-ray diffraction, and with the capabilities of combined spatial (≈0.01 Å) and temporal (300–600 fs) resolutions, promise diverse applications for this ultrafast electron crystallography tabletop methodology. PMID:14745037

Ab initio structure determination and quantitative disorder analysis on nanoparticles by electron diffraction tomography.

PubMed

Krysiak, Yaşar; Barton, Bastian; Marler, Bernd; Neder, Reinhard B; Kolb, Ute

2018-03-01

Nanoscaled porous materials such as zeolites have attracted substantial attention in industry due to their catalytic activity, and their performance in sorption and separation processes. In order to understand the properties of such materials, current research focuses increasingly on the determination of structural features beyond the averaged crystal structure. Small particle sizes, various types of disorder and intergrown structures render the description of structures at atomic level by standard crystallographic methods difficult. This paper reports the characterization of a strongly disordered zeolite structure, using a combination of electron exit-wave reconstruction, automated diffraction tomography (ADT), crystal disorder modelling and electron diffraction simulations. Zeolite beta was chosen for a proof-of-principle study of the techniques, because it consists of two different intergrown polymorphs that are built from identical layer types but with different stacking sequences. Imaging of the projected inner Coulomb potential of zeolite beta crystals shows the intergrowth of the polymorphs BEA and BEB. The structures of BEA as well as BEB could be extracted from one single ADT data set using direct methods. A ratio for BEA/BEB = 48:52 was determined by comparison of the reconstructed reciprocal space based on ADT data with simulated electron diffraction data for virtual nanocrystals, built with different ratios of BEA/BEB. In this way, it is demonstrated that this smart interplay of the above-mentioned techniques allows the elaboration of the real structures of functional materials in detail - even if they possess a severely disordered structure.

3-dimensional indexation of the icosahedral diffraction pattern using the techniques of electron microscopy

NASA Astrophysics Data System (ADS)

Bourdillon, Antony

2012-11-01

The following facts about icosahedra need wider attention. 1) The golden section τ is as fundamental to the icosahedral structure (length /edge) as π is to the sphere (circumference /diameter). 2) The diffraction series are in restricted Fibonacci order because the ratio of adjacent terms fn/fn-1 does not vary, but is the constant τ. The series is therefore geometric. 3) Because of the tetragonal subgroup in the icosahedral point group symmetry, many axes in the icosahedral structure have identical orientation to axes in the face centered cubic matrix of Al6Mn [1] (e.g. [100] and [111]). On these bases, a three dimensional stereographic projection will be presented. 4) A quasi-Bragg law is derived that correctly represents the diffraction series in powers of τ [2]. Furthermore, by employing the normal conventions of electron microscopy, all diffraction patterns are completely indexed in three dimensions. These are the topic of this presentation. Significant consequences will be presented elsewhere: 1) The diffraction pattern intensities near all main axes are correctly simulated, and all atoms are located on a specimen image. 2) The quasi-Bragg law has a special metric. Atomic locations are consistently calculated for the first time. 3) Whereas the Bragg law transforms a crystal lattice in real space into a reciprocal lattice in diffraction space, the quasi-Bragg law transforms a geometric diffraction pattern into a hierarchic structure. 4) Hyperspatial indexation [3] is superceded. [1] Shechtman, D.; Blech, I.; Gratias, D.; Cahn, J.W., Metallic phase with long-range orientational order and no translational symmetry, Phys. Rev. Lett., 1984, 53, 1951-3. [2] Bourdillon, A. J., Nearly free electron band structures in a logarithmically periodic solid, Sol. State Comm. 2009, 149, 1221-1225. [3] Duneau, M., and Katz, A., Phys Rev Lett 54, 2688-2691

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

PubMed

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

2006-07-13

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

The effect of Sr and Bi on the Si(100) surface oxidation - Auger electron spectroscopy, low energy electron diffraction, and X-ray photoelectron spectroscopy study

NASA Technical Reports Server (NTRS)

Fan, W. C.; Mesarwi, A.; Ignatiev, A.

1990-01-01

The effect of Sr and Bi on the oxidation of the Si(100) surface has been studied by Auger electron spectroscopy, low electron diffraction, and X-ray photoelectron spectroscopy. A dramatic enhancement, by a factor of 10, of the Si oxidation has been observed for Si(100) with a Sr overlayer. The SR-enhanced Si oxidation has been studied as a function of O2 exposure and Sr coverage. In contrast to the oxidation promotion of Sr on Si, it has been also observed that a Bi overlayer on Si(100) reduced Si oxidation significantly. Sr adsorption on the Si(100) with a Bi overlayer enhances Si oxidation only at Sr coverage of greater than 0.3 ML.

Surface structure of Bi2Sr2CaCu2O(8+delta) high-temperature superconductors studied using low-energy electron diffraction

NASA Astrophysics Data System (ADS)

Lindberg, P. A. P.; Shen, Z.-X.; Wells, B. O.; Mitzi, D. B.; Lindau, I.

1988-12-01

The surface structure of Bi2Sr2CaCu2O(8+delta) has been studied using low-energy electron diffraction (LEED). Sharp diffraction spots indicative of a well-ordered surface are observed. The LEED patterns unequivocally show that this type of material preferentially cleaves along the a-b planes of the nearly tetragonal unit cell. A superstructure extending along one of the axes in the a-b plane (b) is found to have a periodicity of 27 + or - 0.5 A, in good agreement with earlier studies of the three-dimensional crystal structure. The superstructure at the surface is nonlocal in character and reflects the long-range superlattice of the bulk along the b axis. Intensity modulations of the diffraction spots oriented along the b axis are also reported and discussed in terms of the cell dimension of the unit cell along the b axis.

Flow-aligned, single-shot fiber diffraction using a femtosecond X-ray free-electron laser

DOE PAGES

Popp, David; Loh, N. Duane; Zorgati, Habiba; ...

2017-06-02

A major goal for X-ray free-electron laser (XFEL) based science is to elucidate structures of biological molecules without the need for crystals. Filament systems may provide some of the first single macromolecular structures elucidated by XFEL radiation, since they contain one-dimensional translational symmetry and thereby occupy the diffraction intensity region between the extremes of crystals and single molecules. Here, we demonstrate flow alignment of as few as 100 filaments ( Escherichia coli pili, F-actin, and amyloid fibrils), which when intersected by femtosecond X-ray pulses result in diffraction patterns similar to those obtained from classical fiber diffraction studies. We also determinemore » that F-actin can be flow-aligned to a disorientation of approximately 5 degrees. Using this XFEL-based technique, we determine that gelsolin amyloids are comprised of stacked β-strands running perpendicular to the filament axis, and that a range of order from fibrillar to crystalline is discernable for individual α-synuclein amyloids.« less

Flow-aligned, single-shot fiber diffraction using a femtosecond X-ray free-electron laser

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

Popp, David; Loh, N. Duane; Zorgati, Habiba

A major goal for X-ray free-electron laser (XFEL) based science is to elucidate structures of biological molecules without the need for crystals. Filament systems may provide some of the first single macromolecular structures elucidated by XFEL radiation, since they contain one-dimensional translational symmetry and thereby occupy the diffraction intensity region between the extremes of crystals and single molecules. Here, we demonstrate flow alignment of as few as 100 filaments ( Escherichia coli pili, F-actin, and amyloid fibrils), which when intersected by femtosecond X-ray pulses result in diffraction patterns similar to those obtained from classical fiber diffraction studies. We also determinemore » that F-actin can be flow-aligned to a disorientation of approximately 5 degrees. Using this XFEL-based technique, we determine that gelsolin amyloids are comprised of stacked β-strands running perpendicular to the filament axis, and that a range of order from fibrillar to crystalline is discernable for individual α-synuclein amyloids.« less

Characterization of individual stacking faults in a wurtzite GaAs nanowire by nanobeam X-ray diffraction.

PubMed

Davtyan, Arman; Lehmann, Sebastian; Kriegner, Dominik; Zamani, Reza R; Dick, Kimberly A; Bahrami, Danial; Al-Hassan, Ali; Leake, Steven J; Pietsch, Ullrich; Holý, Václav

2017-09-01

Coherent X-ray diffraction was used to measure the type, quantity and the relative distances between stacking faults along the growth direction of two individual wurtzite GaAs nanowires grown by metalorganic vapour epitaxy. The presented approach is based on the general property of the Patterson function, which is the autocorrelation of the electron density as well as the Fourier transformation of the diffracted intensity distribution of an object. Partial Patterson functions were extracted from the diffracted intensity measured along the [000\\bar{1}] direction in the vicinity of the wurtzite 00\\bar{1}\\bar{5} Bragg peak. The maxima of the Patterson function encode both the distances between the fault planes and the type of the fault planes with the sensitivity of a single atomic bilayer. The positions of the fault planes are deduced from the positions and shapes of the maxima of the Patterson function and they are in excellent agreement with the positions found with transmission electron microscopy of the same nanowire.

Characterization of individual stacking faults in a wurtzite GaAs nanowire by nanobeam X-ray diffraction

PubMed Central

Davtyan, Arman; Lehmann, Sebastian; Zamani, Reza R.; Dick, Kimberly A.; Bahrami, Danial; Al-Hassan, Ali; Leake, Steven J.; Pietsch, Ullrich; Holý, Václav

2017-01-01

Coherent X-ray diffraction was used to measure the type, quantity and the relative distances between stacking faults along the growth direction of two individual wurtzite GaAs nanowires grown by metalorganic vapour epitaxy. The presented approach is based on the general property of the Patterson function, which is the autocorrelation of the electron density as well as the Fourier transformation of the diffracted intensity distribution of an object. Partial Patterson functions were extracted from the diffracted intensity measured along the direction in the vicinity of the wurtzite Bragg peak. The maxima of the Patterson function encode both the distances between the fault planes and the type of the fault planes with the sensitivity of a single atomic bilayer. The positions of the fault planes are deduced from the positions and shapes of the maxima of the Patterson function and they are in excellent agreement with the positions found with transmission electron microscopy of the same nanowire. PMID:28862620

Protein crystal structure obtained at 2.9 Å resolution from injecting bacterial cells into an X-ray free-electron laser beam

PubMed Central

Sawaya, Michael R.; Cascio, Duilio; Gingery, Mari; Rodriguez, Jose; Goldschmidt, Lukasz; Colletier, Jacques-Philippe; Messerschmidt, Marc M.; Boutet, Sébastien; Koglin, Jason E.; Williams, Garth J.; Brewster, Aaron S.; Nass, Karol; Hattne, Johan; Botha, Sabine; Doak, R. Bruce; Shoeman, Robert L.; DePonte, Daniel P.; Park, Hyun-Woo; Federici, Brian A.; Sauter, Nicholas K.; Schlichting, Ilme; Eisenberg, David S.

2014-01-01

It has long been known that toxins produced by Bacillus thuringiensis (Bt) are stored in the bacterial cells in crystalline form. Here we describe the structure determination of the Cry3A toxin found naturally crystallized within Bt cells. When whole Bt cells were streamed into an X-ray free-electron laser beam we found that scattering from other cell components did not obscure diffraction from the crystals. The resolution limits of the best diffraction images collected from cells were the same as from isolated crystals. The integrity of the cells at the moment of diffraction is unclear; however, given the short time (∼5 µs) between exiting the injector to intersecting with the X-ray beam, our result is a 2.9-Å-resolution structure of a crystalline protein as it exists in a living cell. The study suggests that authentic in vivo diffraction studies can produce atomic-level structural information. PMID:25136092

X-ray topography using the forward transmitted beam under multiple-beam diffraction conditions

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

Tsusaka, Y., E-mail: tsusaka@sci.u-hyogo.ac.jp; Takano, H.; Takeda, S.

2016-02-15

X-ray topographs are taken for a sapphire wafer with the [0001] surface normal, as an example, by forward transmitted synchrotron x-ray beams combined with two-dimensional electronic arrays in the x-ray detector having a spatial resolution of 1 μm. They exhibit no shape deformation and no position shift of the dislocation lines on the topographs. Since the topography is performed under multiple-beam diffraction conditions, the topographic images of a single diffraction (two-wave approximation condition) or plural diffractions (six-wave approximation condition) can be recorded without large specimen position changes. As usual Lang topographs, it is possible to determine the Burgers vector ofmore » each dislocation line. Because of high parallelism of the incoming x-rays and linear sensitivity of the electronic arrays to the incident x-rays, the present technique can be used to visualize individual dislocations in single crystals of the dislocation density as high as 1 × 10{sup 5} cm{sup −2}.« less

Resolution limits of ultrafast ultrasound localization microscopy

NASA Astrophysics Data System (ADS)

Desailly, Yann; Pierre, Juliette; Couture, Olivier; Tanter, Mickael

2015-11-01

As in other imaging methods based on waves, the resolution of ultrasound imaging is limited by the wavelength. However, the diffraction-limit can be overcome by super-localizing single events from isolated sources. In recent years, we developed plane-wave ultrasound allowing frame rates up to 20 000 fps. Ultrafast processes such as rapid movement or disruption of ultrasound contrast agents (UCA) can thus be monitored, providing us with distinct punctual sources that could be localized beyond the diffraction limit. We previously showed experimentally that resolutions beyond λ/10 can be reached in ultrafast ultrasound localization microscopy (uULM) using a 128 transducer matrix in reception. Higher resolutions are theoretically achievable and the aim of this study is to predict the maximum resolution in uULM with respect to acquisition parameters (frequency, transducer geometry, sampling electronics). The accuracy of uULM is the error on the localization of a bubble, considered a point-source in a homogeneous medium. The proposed model consists in two steps: determining the timing accuracy of the microbubble echo in radiofrequency data, then transferring this time accuracy into spatial accuracy. The simplified model predicts a maximum resolution of 40 μm for a 1.75 MHz transducer matrix composed of two rows of 64 elements. Experimental confirmation of the model was performed by flowing microbubbles within a 60 μm microfluidic channel and localizing their blinking under ultrafast imaging (500 Hz frame rate). The experimental resolution, determined as the standard deviation in the positioning of the microbubbles, was predicted within 6 μm (13%) of the theoretical values and followed the analytical relationship with respect to the number of elements and depth. Understanding the underlying physical principles determining the resolution of superlocalization will allow the optimization of the imaging setup for each organ. Ultimately, accuracies better than the size of capillaries are achievable at several centimeter depths.

On the Presentation of Wave Phenomena of Electrons with the Young-Feynman Experiment

ERIC Educational Resources Information Center

Matteucci, Giorgio

2011-01-01

The Young-Feynman two-hole interferometer is widely used to present electron wave-particle duality and, in particular, the buildup of interference fringes with single electrons. The teaching approach consists of two steps: (i) electrons come through only one hole but diffraction effects are disregarded and (ii) electrons come through both holes…

Nano-scale Characterization of Basalt - Quenched Lava and Reheated Products

NASA Astrophysics Data System (ADS)

Burkhard, D. J.; Wirth, R.

2001-12-01

In order to trace the mechanism of crystallization in basalt we investigated basalt lava from active Pu'u O'o, Kilauea, Hawaii with TEM. We considered (1) quenched melt (glass, obtained by dipping a hammer into the lava (April 1996) and subsequent quenching in air), and (2) that glass after reheating for 48 hr at 850° C, and (3) after reheating for 48 hr at 930° C. Previous investigations had illustrated interface-controlled growth of pyroxene and Fe-Ti oxides at 850° C and volumetric growth of these phases in addition to plagioclase above 920° C [1]. In general, (1) is a perfect glass to the nano-scale. Occasional inhomogeneities are identified as plagioclase. With a size of no more than approximately 100 unit cells, these "crystals" might be considered as nuclei. Dendrites of pyroxene, identified on the micron scale with back scattered electrons [1], occur as a sequence of slightly displaced plates with equal orientation on the nano-scale. HREM, diffraction pattern and EDS confirm that this is augite, in agreement with investigations on the micron-scale [1]. Fe-Ti oxides occur isolated in the matrix with a diameter less than 100 nm, in contrast to the micron-scale, where Fe-Ti oxides appear at the apices of augite. In (3) we find in addition plagioclase with thin lamellae, indicating twinning. In (3),augite contains lamellae parallel to (001), and they are identified as pigeonite by HREM and electron diffraction. Pigeonite lamellae occur also in (2), however, less developed. Electron diffraction suggests that reflections of augite correspond to the space group C 2/c, and of exsolved pigeonite to P 21/c, which is a low pigeonite. These exsolution phenomena are undistiguishable from what is usually observed in relation to high cooling rates [e.g. 2]. The stability of pigeonite at these temperatures suggests a Fe/Fe+Mg ratio above 0.6 for pyroxene in the quadilateral [3]. Microprobe analyses [1] suggest ratios of 0.4 to 0.5. [1] Burkhard D.J.M. (2001) J. Petrol. 42, 507-527; [2] Philpotts A.R. (1990) Principles of Igneous and Metamorphic Petrology, Prentice; [3] Lindsley A.(1983) Am. Mineral. 68, 477-493.

Near Edge X-Ray Absorption and X-Ray Photoelectron Diffraction Studies of the Structural Environment of Ge-Si Systems

NASA Astrophysics Data System (ADS)

Castrucci, P.; Gunnella, R.; Pinto, N.; Bernardini, R.; de Crescenzi, M.; Sacchi, M.

Near edge X-ray absorption spectroscopy (XAS), X-ray photoelectron diffraction (XPD) and Auger electron diffraction (AED) are powerful techniques for the qualitative study of the structural and electronic properties of several systems. The recent development of a multiple scattering approach to simulating experimental spectra opened a friendly way to the study of structural environments of solids and surfaces. This article reviews recent X-ray absorption experiments using synchrotron radiation which were performed at Ge L edges and core level electron diffraction measurements obtained using a traditional X-ray source from Ge core levels for ultrathin Ge films deposited on silicon substrates. Thermodynamics and surface reconstruction have been found to play a crucial role in the first stages of Ge growth on Si(001) and Si(111) surfaces. Both techniques show the occurrence of intermixing processes even for room-temperature-grown Ge/Si(001) samples and give a straightforward measurement of the overlayer tetragonal distortion. The effects of Sb as a surfactant on the Ge/Si(001) interface have also been investigated. In this case, evidence of layer-by-layer growth of the fully strained Ge overlayer with a reduced intermixing is obtained when one monolayer of Sb is predeposited on the surface.

Charge disproportionation and the pressure-induced insulator–metal transition in cubic perovskite PbCrO3

PubMed Central

Cheng, Jinguang; Kweon, K. E.; Larregola, S. A.; Ding, Yang; Shirako, Y.; Marshall, L. G.; Li, Z.-Y.; Li, X.; dos Santos, António M.; Suchomel, M. R.; Matsubayashi, K.; Uwatoko, Y.; Hwang, G. S.; Goodenough, John B.; Zhou, J.-S.

2015-01-01

The perovskite PbCrO3 is an antiferromagnetic insulator. However, the fundamental interactions leading to the insulating state in this single-valent perovskite are unclear. Moreover, the origin of the unprecedented volume drop observed at a modest pressure of P = 1.6 GPa remains an outstanding problem. We report a variety of in situ pressure measurements including electron transport properties, X-ray absorption spectrum, and crystal structure study by X-ray and neutron diffraction. These studies reveal key information leading to the elucidation of the physics behind the insulating state and the pressure-induced transition. We argue that a charge disproportionation 3Cr4+ → 2Cr3+ + Cr6+ in association with the 6s-p hybridization on the Pb2+ is responsible for the insulating ground state of PbCrO3 at ambient pressure and the charge disproportionation phase is suppressed under pressure to give rise to a metallic phase at high pressure. The model is well supported by density function theory plus the correlation energy U (DFT+U) calculations. PMID:25624483

Charge disproportionation and the pressure-induced insulator–metal transition in cubic perovskite PbCrO 3

DOE PAGES

Cheng, Jinguang; Kweon, K. E.; Larregola, S. A.; ...

2015-01-26

The perovskite PbCrO 3 is an antiferromagnetic insulator. But, the fundamental interactions leading to the insulating state in this single-valent perovskite are unclear. Moreover, the origin of the unprecedented volume drop observed at a modest pressure of P = 1.6 GPa remains an outstanding problem. Our report shows a variety of in situ pressure measurements including electron transport properties, X-ray absorption spectrum, and crystal structure study by X-ray and neutron diffraction. These studies reveal key information leading to the elucidation of the physics behind the insulating state and the pressure-induced transition. Furthermore, we argue that a charge disproportionation 3Cr 4+more » → 2Cr 3+ + Cr 6+ in association with the 6s-p hybridization on the Pb 2+ is responsible for the insulating ground state of PbCrO 3 at ambient pressure and the charge disproportionation phase is suppressed under pressure to give rise to a metallic phase at high pressure. The model is well supported by density function theory plus the correlation energy U (DFT + U) calculations.« less

Electron-lattice energy relaxation in laser-excited thin-film Au-insulator heterostructures studied by ultrafast MeV electron diffraction.

PubMed

Sokolowski-Tinten, K; Shen, X; Zheng, Q; Chase, T; Coffee, R; Jerman, M; Li, R K; Ligges, M; Makasyuk, I; Mo, M; Reid, A H; Rethfeld, B; Vecchione, T; Weathersby, S P; Dürr, H A; Wang, X J

2017-09-01

We apply time-resolved MeV electron diffraction to study the electron-lattice energy relaxation in thin film Au-insulator heterostructures. Through precise measurements of the transient Debye-Waller-factor, the mean-square atomic displacement is directly determined, which allows to quantitatively follow the temporal evolution of the lattice temperature after short pulse laser excitation. Data obtained over an extended range of laser fluences reveal an increased relaxation rate when the film thickness is reduced or the Au-film is capped with an additional insulator top-layer. This behavior is attributed to a cross-interfacial coupling of excited electrons in the Au film to phonons in the adjacent insulator layer(s). Analysis of the data using the two-temperature-model taking explicitly into account the additional energy loss at the interface(s) allows to deduce the relative strength of the two relaxation channels.

Electron-lattice energy relaxation in laser-excited thin-film Au-insulator heterostructures studied by ultrafast MeV electron diffraction

PubMed Central

Sokolowski-Tinten, K.; Shen, X.; Zheng, Q.; Chase, T.; Coffee, R.; Jerman, M.; Li, R. K.; Ligges, M.; Makasyuk, I.; Mo, M.; Reid, A. H.; Rethfeld, B.; Vecchione, T.; Weathersby, S. P.; Dürr, H. A.; Wang, X. J.

2017-01-01

We apply time-resolved MeV electron diffraction to study the electron-lattice energy relaxation in thin film Au-insulator heterostructures. Through precise measurements of the transient Debye-Waller-factor, the mean-square atomic displacement is directly determined, which allows to quantitatively follow the temporal evolution of the lattice temperature after short pulse laser excitation. Data obtained over an extended range of laser fluences reveal an increased relaxation rate when the film thickness is reduced or the Au-film is capped with an additional insulator top-layer. This behavior is attributed to a cross-interfacial coupling of excited electrons in the Au film to phonons in the adjacent insulator layer(s). Analysis of the data using the two-temperature-model taking explicitly into account the additional energy loss at the interface(s) allows to deduce the relative strength of the two relaxation channels. PMID:28795080

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

A general method for baseline-removal in ultrafast electron powder diffraction data using the dual-tree complex wavelet transform.

PubMed

René de Cotret, Laurent P; Siwick, Bradley J

2017-07-01

The general problem of background subtraction in ultrafast electron powder diffraction (UEPD) is presented with a focus on the diffraction patterns obtained from materials of moderately complex structure which contain many overlapping peaks and effectively no scattering vector regions that can be considered exclusively background. We compare the performance of background subtraction algorithms based on discrete and dual-tree complex (DTCWT) wavelet transforms when applied to simulated UEPD data on the M1-R phase transition in VO 2 with a time-varying background. We find that the DTCWT approach is capable of extracting intensities that are accurate to better than 2% across the whole range of scattering vector simulated, effectively independent of delay time. A Python package is available.

Structural and electronic evolution of Cr[subscript 2]O[subscript 3] on compression to 55 GPa

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

Dera, Przemyslaw; Lavina, Barbara; Meng, Yue

2016-08-15

Synchrotron single-crystal x-ray diffraction experiments have been performed on corundum-type Cr{sub 2}O{sub 3} up to a pressure of 55 GPa in Ne and He pressure transmitting media. Diffraction experiments were complemented by measurements of optical absorption spectra with single crystal samples up to 60 GPa. Results of the diffraction data analysis rule out the earlier reported monoclinic distortion at 15-30 GPa, but indicate evidence of two discontinuous transitions of electronic or magnetic nature, most likely associated with a change in magnetic ordering and charge transfer. The compression mechanism established from single crystal refinements indicates much smaller distortion of the Cr{supmore » 3+} coordination environment than was previously assumed.« less

Electron-beam lithography for micro and nano-optical applications

NASA Technical Reports Server (NTRS)

Wilson, Daniel W.; Muller, Richard E.; Echternach, Pierre M.

2005-01-01

Direct-write electron-beam lithography has proven to be a powerful technique for fabricating a variety of micro- and nano-optical devices. Binary E-beam lithography is the workhorse technique for fabricating optical devices that require complicated precision nano-scale features. We describe a bi-layer resist system and virtual-mark height measurement for improving the reliability of fabricating binary patterns. Analog E-beam lithography is a newer technique that has found significant application in the fabrication of diffractive optical elements. We describe our techniques for fabricating analog surface-relief profiles in E-beam resist, including some discussion regarding overcoming the problems of resist heating and charging. We also describe a multiple-field-size exposure scheme for suppression of field-stitch induced ghost diffraction orders produced by blazed diffraction gratings on non-flat substrates.

In situ synthesis of semiconducting single-walled carbon nanotubes by modified arc discharging method

NASA Astrophysics Data System (ADS)

Zhao, Tingkai; Ji, Xianglin; Jin, Wenbo; Yang, Wenbo; Zhao, Xing; Dang, Alei; Li, Hao; Li, Tiehu

2017-02-01

Semiconducting single-walled carbon nanotubes (s-SWCNTs) were in situ synthesized by a temperature-controlled arc discharging furnace with DC electric field using Co-Ni alloy powder as catalyst in helium gas. The microstructures of s-SWCNTs were characterized using high-resolution transmission electron microscopy, electron diffraction, and Raman spectrometry apparatus. The experimental results indicated that the best voltage value in DC electric field is 54 V, and the environmental temperature of the reaction chamber is 600 °C. The mean diameter of s-SWCNTs was estimated about 1.3 nm. The chiral vector ( n, m) of s-SWCNTs was calculated to be (10, 10) type according to the electron diffraction patterns.

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.

Photon-assisted electron energy loss spectroscopy and ultrafast imaging.

PubMed

Howie, Archie

2009-08-01

A variety of ways is described in which photons can be used not only for ultrafast electron microscopy but also to enormously widen the energy range of spatially-resolved electron spectroscopy. Periodic chains of femtosecond laser pulses are a particularly important and accurately timed source for single-shot imaging and diffraction as well as for several forms of pump-probe microscopy at even higher spatial resolution and sub-picosecond timing. Many exciting new fields are opened up for study by these developments. Ultrafast, single shot diffraction with intense pulses of X-rays supplemented by phase retrieval techniques may eventually offer a challenging alternative and purely photon-based route to dynamic imaging at high spatial resolution.

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

Zhang, Jie; He, Yunteng; Kong, Wei, E-mail: wei.kong@oregonstate.edu

We report electron diffraction of ferrocene doped in superfluid helium droplets. By taking advantage of the velocity slip in our pulsed droplet beam using a pulsed electron gun, and by doping with a high concentration of ferrocene delivered via a pulsed valve, we can obtain high quality diffraction images from singly doped droplets. Under the optimal doping conditions, 80% of the droplets sampled in the electron beam are doped with just one ferrocene molecule. Extension of this size selection method to dopant clusters has also been demonstrated. However, incomplete separation of dopant clusters might require deconvolution and modeling of themore » doping process. This method can be used for studies of nucleation processes in superfluid helium droplets.« less

Start-to-end simulation of single-particle imaging using ultra-short pulses at the European X-ray Free-Electron Laser

PubMed Central

Buzmakov, Alexey; Jurek, Zoltan; Loh, Ne-Te Duane; Samoylova, Liubov; Santra, Robin; Schneidmiller, Evgeny A.; Tschentscher, Thomas; Yakubov, Sergey; Yoon, Chun Hong; Yurkov, Michael V.; Ziaja-Motyka, Beata; Mancuso, Adrian P.

2017-01-01

Single-particle imaging with X-ray free-electron lasers (XFELs) has the potential to provide structural information at atomic resolution for non-crystalline biomolecules. This potential exists because ultra-short intense pulses can produce interpretable diffraction data notwithstanding radiation damage. This paper explores the impact of pulse duration on the interpretability of diffraction data using comprehensive and realistic simulations of an imaging experiment at the European X-ray Free-Electron Laser. It is found that the optimal pulse duration for molecules with a few thousand atoms at 5 keV lies between 3 and 9 fs. PMID:28989713

Ultrashort electron bunch length measurement with diffraction radiation deflector

NASA Astrophysics Data System (ADS)

Xiang, Dao; Huang, Wen-Hui

2007-01-01

In this paper, we propose a novel method to measure electron bunch length with a diffraction radiation (DR) deflector which is composed of a DR radiator and three beam position monitors (BPMs). When an electron beam passes through a metallic aperture which is tilted by 45 degrees with respect to its trajectory, backward DR that propagates perpendicular to the beam’s trajectory is generated which adds a transverse deflection to the beam as a result of momentum conservation. The deflection is found to be largely dependent on the bunch length and could be easily observed with a downstream BPM. Detailed investigations show that this method has wide applicability, high temporal resolution, and great simplicity.

One step synthesis of porous graphene by laser ablation: A new and facile approach

NASA Astrophysics Data System (ADS)

Kazemizadeh, Fatemeh; Malekfar, Rasoul

2018-02-01

Porous graphene (PG) was obtained using one step laser process. Synthesis was carried out by laser ablation of nickel-graphite target under ultra-high flow of argon gas. The field emission scanning electron microscopy (FE-SEM) results showed the formation of a porous structure and the transmission electron microscopy (TEM) revealed that the porosity of PGs increase under intense laser irradiation. Structural characterization study using Raman spectroscopy, X-ray powder diffraction (XRD) and selected area electron diffraction (SAED) technique showed that the obtained PGs display high crystalline structure in the form of few layer rhombohedral graphitic arrangement that can be interpreted as the phase prior to the formation of other carbon nanostructures.

Improved crystal orientation and physical properties from single-shot XFEL stills

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

Sauter, Nicholas K., E-mail: nksauter@lbl.gov; Hattne, Johan; Brewster, Aaron S.

X-ray free-electron laser crystallography relies on the collection of still-shot diffraction patterns. New methods are developed for optimal modeling of the crystals’ orientations and mosaic block properties. X-ray diffraction patterns from still crystals are inherently difficult to process because the crystal orientation is not uniquely determined by measuring the Bragg spot positions. Only one of the three rotational degrees of freedom is directly coupled to spot positions; the other two rotations move Bragg spots in and out of the reflecting condition but do not change the direction of the diffracted rays. This hinders the ability to recover accurate structure factorsmore » from experiments that are dependent on single-shot exposures, such as femtosecond diffract-and-destroy protocols at X-ray free-electron lasers (XFELs). Here, additional methods are introduced to optimally model the diffraction. The best orientation is obtained by requiring, for the brightest observed spots, that each reciprocal-lattice point be placed into the exact reflecting condition implied by Bragg’s law with a minimal rotation. This approach reduces the experimental uncertainties in noisy XFEL data, improving the crystallographic R factors and sharpening anomalous differences that are near the level of the noise.« less

Variable microstructural response of baddeleyite to shock metamorphism in young basaltic shergottite NWA 5298 and improved U-Pb dating of Solar System events

NASA Astrophysics Data System (ADS)

Darling, James R.; Moser, Desmond E.; Barker, Ivan R.; Tait, Kim T.; Chamberlain, Kevin R.; Schmitt, Axel K.; Hyde, Brendt C.

2016-06-01

The accurate dating of igneous and impact events is vital for the understanding of Solar System evolution, but has been hampered by limited knowledge of how shock metamorphism affects mineral and whole-rock isotopic systems used for geochronology. Baddeleyite (monoclinic ZrO2) is a refractory mineral chronometer of great potential to date these processes due to its widespread occurrence in achondrites and robust U-Pb isotopic systematics, but there is little understanding of shock-effects on this phase. Here we present new nano-structural measurements of baddeleyite grains in a thin-section of the highly-shocked basaltic shergottite Northwest Africa (NWA) 5298, using high-resolution electron backscattered diffraction (EBSD) and scanning transmission electron microscopy (STEM) techniques, to investigate shock-effects and their linkage with U-Pb isotopic disturbance that has previously been documented by in-situ U-Pb isotopic analyses. The shock-altered state of originally igneous baddeleyite grains is highly variable across the thin-section and often within single grains. Analyzed grains range from those that preserve primary (magmatic) twinning and trace-element zonation (baddeleyite shock Group 1), to quasi-amorphous ZrO2 (Group 2) and to recrystallized micro-granular domains of baddeleyite (Group 3). These groups correlate closely with measured U-Pb isotope compositions. Primary igneous features in Group 1 baddeleyites (n = 5) are retained in high shock impedance grain environments, and an average of these grains yields a revised late-Amazonian magmatic crystallization age of 175 ± 30 Ma for this shergottite. The youngest U-Pb dates occur from Group 3 recrystallized nano- to micro-granular baddeleyite grains, indicating that it is post-shock heating and new mineral growth that drives much of the isotopic disturbance, rather than just shock deformation and phase transitions. Our data demonstrate that a systematic multi-stage microstructural evolution in baddeleyite results from a single cycle of shock-loading, heating and cooling during transit to space, and that this leads to variable disturbance of the U-Pb isotope system. Furthermore, by linking in-situ U-Pb isotopic measurements with detailed micro- to nano-structural analyses, it is possible to resolve the timing of both endogenic crustal processes and impact events in highly-shocked planetary materials using baddeleyite. This opens up new opportunities to refine the timing of major events across the Solar System.

Optical Simulation of Debye-Scherrer Crystal Diffraction

ERIC Educational Resources Information Center

Logiurato, F.; Gratton, L. M.; Oss, S.

2008-01-01

In this paper we describe and discuss simple, inexpensive optical experiments used to simulate x-ray and electron diffraction according to the Debye-Scherrer theory. The experiment can be used to address, at the high school level, important subjects related to fundamental quantum and solid-state physics.

Competing retention pathways of uranium upon reaction with Fe(II)

NASA Astrophysics Data System (ADS)

Massey, Michael S.; Lezama-Pacheco, Juan S.; Jones, Morris E.; Ilton, Eugene S.; Cerrato, José M.; Bargar, John R.; Fendorf, Scott

2014-10-01

Biogeochemical retention processes, including adsorption, reductive precipitation, and incorporation into host minerals, are important in contaminant transport, remediation, and geologic deposition of uranium. Recent work has shown that U can become incorporated into iron (hydr)oxide minerals, with a key pathway arising from Fe(II)-induced transformation of ferrihydrite, (Fe(OH)3·nH2O) to goethite (α-FeO(OH)); this is a possible U retention mechanism in soils and sediments. Several key questions, however, remain unanswered regarding U incorporation into iron (hydr)oxides and this pathway's contribution to U retention, including: (i) the competitiveness of U incorporation versus reduction to U(IV) and subsequent precipitation of UO2; (ii) the oxidation state of incorporated U; (iii) the effects of uranyl aqueous speciation on U incorporation; and, (iv) the mechanism of U incorporation. Here we use a series of batch reactions conducted at pH ∼7, [U(VI)] from 1 to 170 μM, [Fe(II)] from 0 to 3 mM, and [Ca] at 0 or 4 mM coupled with spectroscopic examination of reaction products of Fe(II)-induced ferrihydrite transformation to address these outstanding questions. Uranium retention pathways were identified and quantified using extended X-ray absorption fine structure (EXAFS) spectroscopy, X-ray powder diffraction, X-ray photoelectron spectroscopy, and transmission electron microscopy. Analysis of EXAFS spectra showed that 14-89% of total U was incorporated into goethite, upon reaction with Fe(II) and ferrihydrite. Uranium incorporation was a particularly dominant retention pathway at U concentrations ⩽50 μM when either uranyl-carbonato or calcium-uranyl-carbonato complexes were dominant, accounting for 64-89% of total U. With increasing U(VI) and Fe(II) concentrations, U(VI) reduction to U(IV) became more prevalent, but U incorporation remained a functioning retention pathway. These findings highlight the potential importance of U(V) incorporation within iron oxides as a retention process of U across a wide range of biogeochemical environments and the sensitivity of uranium retention processes to operative (bio)geochemical conditions.

Competing retention pathways of uranium upon reaction with Fe(II)

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

Massey, Michael S.; Lezama Pacheco, Juan S.; Jones, Morris

Biogeochemical retention processes, including adsorption, reductive precipitation, and incorporation into host minerals, are important in contaminant transport, remediation, and geologic deposition of uranium. Recent work has shown that U can become incorporated into iron (hydr)oxide minerals, with a key pathway arising from Fe(II)-induced transformation of ferrihydrite, (Fe(OH)3•nH2O) to goethite (α-FeO(OH)); this is a possible U retention mechanism in soils and sediments. Several key questions, however, remain unanswered regarding U incorporation into iron (hydr)oxides and this pathway’s contribution to U retention, including: (i) the competitiveness of U incorporation versus reduction to U(IV) and subsequent precipitation of UO2; (ii) the oxidation statemore » of incorporated U; (iii) the effects of uranyl aqueous speciation on U incorporation; and, (iv) the mechanism of U incorporation. Here we use a series of batch reactions conducted at pH ~7, [U(VI)] from 1 to 170 μM, [Fe(II)] from 0 to 3 mM, and [Ca] at 0 or 4 mM) coupled with spectroscopic examination of reaction products of Fe(II)-induced ferrihydrite transformation to address these outstanding questions. Uranium retention pathways were identified and quantified using extended x-ray absorption fine structure (EXAFS) spectroscopy, x-ray powder diffraction, x-ray photoelectron spectroscopy, and transmission electron microscopy. Analysis of EXAFS spectra showed that 14 to 89% of total U was incorporated into goethite, upon reaction with Fe(II) and ferrihydrite. Uranium incorporation was a particularly dominant retention pathway at U concentrations ≤ 50 μM when either uranyl-carbonato or calcium-uranyl-carbonato complexes were dominant, accounting for 64 to 89% of total U. With increasing U(VI) and Fe(II) concentrations, U(VI) reduction to U(IV) became more prevalent, but U incorporation remained a functioning retention pathway. These findings highlight the potential importance of U(V) incorporation within iron oxides as a retention process of U across a wide range of biogeochemical environments and the sensitivity of uranium retention processes to operative (bio)geochemical conditions.« less

High-Resolution Mineralogical Characterization and Biogeochemical Modeling of Uranium Reduction Pathways at the NABIR Field-Research Center

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

David R. Veblen; Chen Zhu; Lee Krumholz

The effectiveness and feasibility of bioremediation at the field scale cannot be fully assessed until the mechanisms of immobilization and U speciation in the solid matrix are resolved. However, characterization of the immobilized U and its valence states is extremely difficult, because microbially mediated mineral precipitates are generally nanometer (nm)-sized, poorly crystalline, or amorphous. We are developing combined field emission gun--scanning electron microscopy (FEG-SEM, at Indiana University) and FEG transmission electron microscopy (TEM, at Hopkins) to detect and isolate uranium containing phases; (1) method developments for TEM sample preparations and parallel electron energy loss spectroscopy (EELS) determination of uranium valence;more » and (2) to determine the speciation, fate, reactivity, valence states of immobilized uranium, using the state-of-the-art 300-kV, FEG-TEM. We have obtained preliminary results on contaminated sediments from Area 3 at the Oak Ridge Field Research Center (FRC). TEM results show that the sediments contain numerous minerals, including quartz, mica/clay (muscovite and/or illite), rutile, ilmenite, zircon, and an Al-Sr-Ce-Ca phosphate mineral, none of which contain uranium above the EDS detection limit. Substantial U (up to {approx}2 wt.%) is, however, clearly associated with two materials: (1) the Fe oxyhydroxide and (2) clots of a chemically complex material that is likely a mixture of several nm-scale phases. The Fe oxyhydroxide was identified as goethite from its polycrystalline SAED pattern and EDS analysis showing it to be very Fe-rich; the aggregate also displays one of several morphologies that are common for goethite. U is strongly sorbed to goethite in the FRC sediment, and the ubiquitous association with phosphorous suggests that complexes containing both U and P may play an important role in that sorption. Results from bulk analysis and SEM had previously demonstrated the association of U with Fe and thus suggested that U may be sorbed by Fe oxide or oxyhydroxide (Dr. Roh, image presented by David Watson). However, rigorous identification of the host minerals for U requires TEM results such as these involving imaging, electron diffraction, and spectroscopic analysis. An even higher concentration of U occurs in the chemically complex material noted above. These ''clots'' are high in Fe but also contain C, O, Mg, Al, Si, P, S, Cl, K, Ca, Mn, and U. This chemical complexity strongly suggests that they consist of aggregates of carbonate, silicate, phosphate, and sulfate phases, and TEM images also suggest that they may be intergrowths of numerous exceedingly small nanoparticles. EELS and EFTEM studies should be able to resolve these various components and identify precisely where the uranium is in these complex materials. From the results, it is clear that the FEG-SEM and FEG-TEM can readily detect uranium in the FRC samples. The FEG-SEM allows a wide field of view of the samples and can detect U-rich aggregates as small as 20-30 nm. The FEG-TEM can then focus on these aggregates and use SAED, EDS, EFTEM, and PEELS techniques to determine the valence states, structures, and compositional data for these aggregates. This research will provide a crucial component for a complete understanding of the efficacy of uranium bioremediation.« less

System design and verification of the precession electron diffraction technique

NASA Astrophysics Data System (ADS)

Own, Christopher Su-Yan

2005-07-01

Bulk structural crystallography is generally a two-part process wherein a rough starting structure model is first derived, then later refined to give an accurate model of the structure. The critical step is the determination of the initial model. As materials problems decrease in length scale, the electron microscope has proven to be a versatile and effective tool for studying many problems. However, study of complex bulk structures by electron diffraction has been hindered by the problem of dynamical diffraction. This phenomenon makes bulk electron diffraction very sensitive to specimen thickness, and expensive equipment such as aberration-corrected scanning transmission microscopes or elaborate methodology such as high resolution imaging combined with diffraction and simulation are often required to generate good starting structures. The precession electron diffraction technique (PED), which has the ability to significantly reduce dynamical effects in diffraction patterns, has shown promise as being a "philosopher's stone" for bulk electron diffraction. However, a comprehensive understanding of its abilities and limitations is necessary before it can be put into widespread use as a standalone technique. This thesis aims to bridge the gaps in understanding and utilizing precession so that practical application might be realized. Two new PED systems have been built, and optimal operating parameters have been elucidated. The role of lens aberrations is described in detail, and an alignment procedure is given that shows how to circumvent aberration in order to obtain high-quality patterns. Multislice simulation is used for investigating the errors inherent in precession, and is also used as a reference for comparison to simple models and to experimental PED data. General trends over a large sampling of parameter space are determined. In particular, we show that the primary reflection intensity errors occur near the transmitted beam and decay with increasing angle and decreasing specimen thickness. These errors, occurring at the lowest spatial frequencies, fortuitously coincide with reflections for which phases are easiest to determine via imaging methods. A general two-beam dynamical model based upon an existing approximate model is found to be fairly accurate across most experimental conditions, particularly where it is needed for providing a correction to distorted data. Finally, the practical structure solution procedure using PED is demonstrated for several model material systems. Of the experiment parameters investigated, the cone semi-angle is found to be the most important (it should be as large as possible), followed closely by specimen thickness (thinner is better). Assuming good structure projection characteristics in the specimen, the thickness tractable by PED is extended to 40-50 nm without correction, demonstrated for complex oxides. With a forward calculation based upon the two-beam dynamical model (using known structure factors), usable specimen thickness can be extended past 150 nm. For a priori correction, using the squared amplitudes approximates the two-beam model for most thicknesses if the scattering from the structure adheres to psuedo-kinematical behavior. Practically, crystals up to 60 nm in thickness can now be processed by the precession methods developed in this thesis.

Simulations of the temporal and spatial resolution for a compact time-resolved electron diffractometer

NASA Astrophysics Data System (ADS)

Robinson, Matthew S.; Lane, Paul D.; Wann, Derek A.

2016-02-01

A novel compact electron gun for use in time-resolved gas electron diffraction experiments has recently been designed and commissioned. In this paper we present and discuss the extensive simulations that were performed to underpin the design in terms of the spatial and temporal qualities of the pulsed electron beam created by the ionisation of a gold photocathode using a femtosecond laser. The response of the electron pulses to a solenoid lens used to focus the electron beam has also been studied. The simulated results show that focussing the electron beam affects the overall spatial and temporal resolution of the experiment in a variety of ways, and that factors that improve the resolution of one parameter can often have a negative effect on the other. A balance must, therefore, be achieved between spatial and temporal resolution. The optimal experimental time resolution for the apparatus is predicted to be 416 fs for studies of gas-phase species, while the predicted spatial resolution of better than 2 nm-1 compares well with traditional time-averaged electron diffraction set-ups.

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.

Precession technique and electron diffractometry as new tools for crystal structure analysis and chemical bonding determination.

PubMed

Avilov, A; Kuligin, K; Nicolopoulos, S; Nickolskiy, M; Boulahya, K; Portillo, J; Lepeshov, G; Sobolev, B; Collette, J P; Martin, N; Robins, A C; Fischione, P

2007-01-01

We have developed a new fast electron diffractometer working with high dynamic range and linearity for crystal structure determinations. Electron diffraction (ED) patterns can be scanned serially in front of a Faraday cage detector; the total measurement time for several hundred ED reflections can be tens of seconds having high statistical accuracy for all measured intensities (1-2%). This new tool can be installed to any type of TEM without any column modification and is linked to a specially developed electron beam precession "Spinning Star" system. Precession of the electron beam (Vincent-Midgley technique) reduces dynamical effects allowing also use of accurate intensities for crystal structure analysis. We describe the technical characteristics of this new tool together with the first experimental results. Accurate measurement of electron diffraction intensities by electron diffractometer opens new possibilities not only for revealing unknown structures, but also for electrostatic potential determination and chemical bonding investigation. As an example, we present detailed atomic bonding information of CaF(2) as revealed for the first time by precise electron diffractometry.

Three-dimensional reconstruction of the giant mimivirus particle with an x-ray free-electron laser.

PubMed

Ekeberg, Tomas; Svenda, Martin; Abergel, Chantal; Maia, Filipe R N C; Seltzer, Virginie; Claverie, Jean-Michel; Hantke, Max; Jönsson, Olof; Nettelblad, Carl; van der Schot, Gijs; Liang, Mengning; DePonte, Daniel P; Barty, Anton; Seibert, M Marvin; Iwan, Bianca; Andersson, Inger; Loh, N Duane; Martin, Andrew V; Chapman, Henry; Bostedt, Christoph; Bozek, John D; Ferguson, Ken R; Krzywinski, Jacek; Epp, Sascha W; Rolles, Daniel; Rudenko, Artem; Hartmann, Robert; Kimmel, Nils; Hajdu, Janos

2015-03-06

We present a proof-of-concept three-dimensional reconstruction of the giant mimivirus particle from experimentally measured diffraction patterns from an x-ray free-electron laser. Three-dimensional imaging requires the assembly of many two-dimensional patterns into an internally consistent Fourier volume. Since each particle is randomly oriented when exposed to the x-ray pulse, relative orientations have to be retrieved from the diffraction data alone. We achieve this with a modified version of the expand, maximize and compress algorithm and validate our result using new methods.

Resolution enhancement in coherent x-ray diffraction imaging by overcoming instrumental noise.

PubMed

Kim, Chan; Kim, Yoonhee; Song, Changyong; Kim, Sang Soo; Kim, Sunam; Kang, Hyon Chol; Hwu, Yeukuang; Tsuei, Ku-Ding; Liang, Keng San; Noh, Do Young

2014-11-17

We report that reference objects, strong scatterers neighboring weak phase objects, enhance the phase retrieval and spatial resolution in coherent x-ray diffraction imaging (CDI). A CDI experiment with Au nano-particles exhibited that the reference objects amplified the signal-to-noise ratio in the diffraction intensity at large diffraction angles, which significantly enhanced the image resolution. The interference between the diffracted x-ray from reference objects and a specimen also improved the retrieval of the phase of the diffraction signal. The enhancement was applied to image NiO nano-particles and a mitochondrion and confirmed in a simulation with a bacteria phantom. We expect that the proposed method will be of great help in imaging weakly scattering soft matters using coherent x-ray sources including x-ray free electron lasers.

Coherent diffraction imaging: consistency of the assembled three-dimensional distribution.

PubMed

Tegze, Miklós; Bortel, Gábor

2016-07-01

The short pulses of X-ray free-electron lasers can produce diffraction patterns with structural information before radiation damage destroys the particle. From the recorded diffraction patterns the structure of particles or molecules can be determined on the nano- or even atomic scale. In a coherent diffraction imaging experiment thousands of diffraction patterns of identical particles are recorded and assembled into a three-dimensional distribution which is subsequently used to solve the structure of the particle. It is essential to know, but not always obvious, that the assembled three-dimensional reciprocal-space intensity distribution is really consistent with the measured diffraction patterns. This paper shows that, with the use of correlation maps and a single parameter calculated from them, the consistency of the three-dimensional distribution can be reliably validated.

Remediation of soils contaminated with particulate depleted uranium by multi stage chemical extraction.

PubMed

Crean, Daniel E; Livens, Francis R; Sajih, Mustafa; Stennett, Martin C; Grolimund, Daniel; Borca, Camelia N; Hyatt, Neil C

2013-12-15

Contamination of soils with depleted uranium (DU) from munitions firing occurs in conflict zones and at test firing sites. This study reports the development of a chemical extraction methodology for remediation of soils contaminated with particulate DU. Uranium phases in soils from two sites at a UK firing range, MOD Eskmeals, were characterised by electron microscopy and sequential extraction. Uranium rich particles with characteristic spherical morphologies were observed in soils, consistent with other instances of DU munitions contamination. Batch extraction efficiencies for aqueous ammonium bicarbonate (42-50% total DU extracted), citric acid (30-42% total DU) and sulphuric acid (13-19% total DU) were evaluated. Characterisation of residues from bicarbonate-treated soils by synchrotron microfocus X-ray diffraction and X-ray absorption spectroscopy revealed partially leached U(IV)-oxide particles and some secondary uranyl-carbonate phases. Based on these data, a multi-stage extraction scheme was developed utilising leaching in ammonium bicarbonate followed by citric acid to dissolve secondary carbonate species. Site specific U extraction was improved to 68-87% total U by the application of this methodology, potentially providing a route to efficient DU decontamination using low cost, environmentally compatible reagents. Copyright © 2013 The Authors. Published by Elsevier B.V. All rights reserved.

GAPD: a GPU-accelerated atom-based polychromatic diffraction simulation code.

PubMed

E, J C; Wang, L; Chen, S; Zhang, Y Y; Luo, S N

2018-03-01

GAPD, a graphics-processing-unit (GPU)-accelerated atom-based polychromatic diffraction simulation code for direct, kinematics-based, simulations of X-ray/electron diffraction of large-scale atomic systems with mono-/polychromatic beams and arbitrary plane detector geometries, is presented. This code implements GPU parallel computation via both real- and reciprocal-space decompositions. With GAPD, direct simulations are performed of the reciprocal lattice node of ultralarge systems (∼5 billion atoms) and diffraction patterns of single-crystal and polycrystalline configurations with mono- and polychromatic X-ray beams (including synchrotron undulator sources), and validation, benchmark and application cases are presented.

Impurity precipitation in atomized particles evidenced by nano x-ray diffraction computed tomography

NASA Astrophysics Data System (ADS)

Bonnin, Anne; Wright, Jonathan P.; Tucoulou, Rémi; Palancher, Hervé

2014-08-01

Performances and physical properties of high technology materials are influenced or even determined by their initial microstructure and by the behavior of impurity phases. Characterizing these impurities and their relations with the surrounding matrix is therefore of primary importance but it unfortunately often requires a destructive approach, with the risk of misinterpreting the observations. The improvement we have done in high resolution X-ray diffraction computed tomography combined with the use of an X-ray nanoprobe allows non-destructive crystallographic description of materials with microscopic heterogeneous microstructure (with a grain size between 10 nm and 10 μm). In this study, the grain localization in a 2D slice of a 20 μm solidified atomized γU-Mo particle is shown and a minority U(C,O) phase (1 wt. %) with sub-micrometer sized grains was characterized inside. Evidence is presented showing that the onset of U(C,O) grain crystallization can be described by a precipitation mechanism since one single U-Mo grain has direct orientation relationship with more than one surrounding U(C,O) grains.

Electron density studies of methyl cellobioside

USDA-ARS?s Scientific Manuscript database

Experimental X-ray diffraction crystallography determines the variations in electron density that result from the periodic array of atoms in a crystal. Normally, the positions and type of atom are determined from the electron density based on an approximation that the atoms are spherical. However, t...

Electronic and geometric structure of thin CoO(100) films studied by angle-resolved photoemission spectroscopy and Auger electron diffraction

NASA Astrophysics Data System (ADS)

Heiler, M.; Chassé, A.; Schindler, K.-M.; Hollering, M.; Neddermeyer, H.

2000-05-01

We have prepared ordered thin films of CoO by evaporating cobalt in an O 2 atmosphere on to a heated (500 K) Ag(100) substrate. The geometric and electronic structure of the films was characterized by means of Auger electron diffraction (AED) and angle-resolved photoemission spectroscopy (ARUPS), respectively. The experimental AED results were compared with simulated data, which showed that the film grows in (100) orientation on the Ag(100) substrate. Synchrotron-radiation-induced photoemission investigations were performed in the photon energy range from 25 eV to 67 eV. The dispersion of the transitions was found to be similar to that of previous results on a single-crystal CoO(100) surface. The resonance behaviour of the photoemission lines in the valence-band region was investigated by constant-initial-state (CIS) spectroscopy. The implications of this behaviour for assignment of the photoemission lines to specific electronic transitions is discussed and compared with published theoretical models of the electronic structure.

Path-separated electron interferometry in a scanning transmission electron microscope

NASA Astrophysics Data System (ADS)

Yasin, Fehmi S.; Harvey, Tyler R.; Chess, Jordan J.; Pierce, Jordan S.; McMorran, Benjamin J.

2018-05-01

We report a path-separated electron interferometer within a scanning transmission electron microscope. In this setup, we use a nanofabricated grating as an amplitude-division beamsplitter to prepare multiple spatially separated, coherent electron probe beams. We achieve path separations of 30 nm. We pass the  +1 diffraction order probe through amorphous carbon while passing the 0th and  ‑1 orders through vacuum. The probes are then made to interfere via imaging optics, and we observe an interference pattern at the CCD detector with up to 39.7% fringe visibility. We show preliminary experimental results in which the interference pattern was recorded during a 1D scan of the diffracted probes across a test phase object. These results qualitatively agree with a modeled interference predicted by an independent measurement of the specimen thickness. This experimental design can potentially be applied to phase contrast imaging and fundamental physics experiments, such as an exploration of electron wave packet coherence length.

Theory and Application of Auger and Photoelectron Diffraction and Holography

NASA Astrophysics Data System (ADS)

Chen, Xiang

This dissertation addresses the theories and applications of three important surface analysis techniques: Auger electron diffraction (AED), x-ray photoelectron diffraction (XPD), and Auger and photoelectron holography. A full multiple-scattering scheme for the calculations of XPD, AED, and Kikuchi electron diffraction pattern from a surface cluster is described. It is used to simulate 64 eV M_{2,3}VV and 913 eV L_3VV AED patterns from Cu(001) surfaces, in order to test assertions in the literature that they are explicable by a classical "blocking" and channeling model. We find that this contention is not valid, and that only a quantum mechanical multiple-scattering calculation is able to simulate these patterns well. The same multiple scattering simulation scheme is also used to investigate the anomalous phenomena of peak shifts off the forward-scattering directions in photo -electron diffraction patterns of Mg KLL (1180 eV) and O 1s (955 eV) from MgO(001) surfaces. These shifts are explained by calculations assuming a short electron mean free path. Similar simulations of XPD from a CoSi_2(111) surface for Co-3p and Si-2p normal emission agree well with experimental diffraction patterns. A filtering process aimed at eliminating the self -interference effect in photoelectron holography is developed. A better reconstructed image from Si-2p XPD from a Si(001) (2 times 1) surface is seen at atomic resolution. A reconstruction algorithm which corrects for the anisotropic emitter waves as well as the anisotropic atomic scattering factors is used for holographic reconstruction from a Co-3p XPD pattern from a CoSi_2 surface. This new algorithm considerably improves the reconstructed image. Finally, a new reconstruction algorithm called "atomic position recovery by iterative optimization of reconstructed intensities" (APRIORI), which takes account of the self-interference terms omitted by the other holographic algorithms, is developed. Tests on a Ni-C-O chain and Si(111)(sqrt{3} times sqrt{3})B surface suggest that this new method may overcome the twin image problem in the traditional holographic methods, reduce the artifacts in real space, and even separately identify the chemical species of the scatterers.

Curcumin Encapsulated into Methoxy Poly(Ethylene Glycol) Poly(ε-Caprolactone) Nanoparticles Increases Cellular Uptake and Neuroprotective Effect in Glioma Cells.

PubMed

Marslin, Gregory; Sarmento, Bruno Filipe Carmelino Cardoso; Franklin, Gregory; Martins, José Alberto Ribeiro; Silva, Carlos Jorge Ribeiro; Gomes, Andreia Ferreira Castro; Sárria, Marisa Passos; Coutinho, Olga Maria Fernandes Pereira; Dias, Alberto Carlos Pires

2017-03-01

Curcumin is a natural polyphenolic compound isolated from turmeric ( Curcuma longa ) with well-demonstrated neuroprotective and anticancer activities. Although curcumin is safe even at high doses in humans, it exhibits poor bioavailability, mainly due to poor absorption, fast metabolism, and rapid systemic elimination. To overcome these issues, several approaches, such as nanoparticle-mediated targeted delivery, have been undertaken with different degrees of success. The present study was conducted to compare the neuroprotective effect of curcumin encapsulated in poly( ε -caprolactone) and methoxy poly(ethylene glycol) poly( ε -caprolactone) nanoparticles in U251 glioblastoma cells. Prepared nanoparticles were physically characterized by laser doppler anemometry, transmission electron microscopy, and X-ray diffraction. The results from laser doppler anemometry confirmed that the size of poly( ε -caprolactone) and poly(ethylene glycol) poly( ε -caprolactone) nanoparticles ranged between 200-240 nm for poly( ε -caprolactone) nanoparticles and 30-70 nm for poly(ethylene glycol) poly( ε -caprolactone) nanoparticles, and transmission electron microscopy images revealed their spherical shape. Treatment of U251 glioma cells and zebrafish embryos with poly( ε -caprolactone) and poly(ethylene glycol) poly( ε -caprolactone) nanoparticles loaded with curcumin revealed efficient cellular uptake. The cellular uptake of poly(ethylene glycol) poly( ε -caprolactone) nanoparticles was higher in comparison to poly( ε -caprolactone) nanoparticles. Moreover, poly(ethylene glycol) poly( ε -caprolactone) di-block copolymer-loaded curcumin nanoparticles were able to protect the glioma cells against tBHP induced-oxidative damage better than free curcumin. Together, our results show that curcumin-loaded poly(ethylene glycol) poly( ε -caprolactone) di-block copolymer nanoparticles possess significantly stronger neuroprotective effect in U251 human glioma cells compared to free curcumin and curcumin-loaded poly( ε -caprolactone) nanoparticles. Georg Thieme Verlag KG Stuttgart · New York.

Neutron diffraction measurement of residual stresses, dislocation density and texture in Zr-bonded U-10Mo “mini” fuel foils and plates

DOE PAGES

Brown, Donald William; Okuniewski, Maria A.; Sisneros, Thomas A.; ...

2016-12-01

Here, Al clad U-10Mo fuel plates are being considered for conversion of several research reactors from high-enriched to low-enriched U fuel. Neutron diffraction measurements of the textures, residual phase stresses, and dislocation densities in the individual phases of the mini-foils throughout several processing steps and following hot-isostatic pressing to the Al cladding, have been completed. Recovery and recrystallization of the bare U-10Mo fuel foil, as indicated by the dislocation density and texture, are observed depending on the state of the material prior to annealing and the duration and temperature of the annealing process. In general, the cladding procedure significantly reducesmore » the dislocation density, but the final state of the clad plate, both texture and dislocation density, depends strongly on the final processing step of the fuel foil. In contrast, the residual stress state of the final plate is dominated by the thermal expansion mismatch of the constituent materials.« less

Neutron diffraction measurement of residual stresses, dislocation density and texture in Zr-bonded U-10Mo “mini” fuel foils and plates

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

Brown, Donald William; Okuniewski, Maria A.; Sisneros, Thomas A.

Here, Al clad U-10Mo fuel plates are being considered for conversion of several research reactors from high-enriched to low-enriched U fuel. Neutron diffraction measurements of the textures, residual phase stresses, and dislocation densities in the individual phases of the mini-foils throughout several processing steps and following hot-isostatic pressing to the Al cladding, have been completed. Recovery and recrystallization of the bare U-10Mo fuel foil, as indicated by the dislocation density and texture, are observed depending on the state of the material prior to annealing and the duration and temperature of the annealing process. In general, the cladding procedure significantly reducesmore » the dislocation density, but the final state of the clad plate, both texture and dislocation density, depends strongly on the final processing step of the fuel foil. In contrast, the residual stress state of the final plate is dominated by the thermal expansion mismatch of the constituent materials.« less

Diffraction-assisted micropatterning of silicon surfaces by ns-laser irradiation

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

Haro-Poniatowski, E., E-mail: haro@xanum.uam.mx; Acosta-Zepeda, C.; Mecalco, G.

2014-06-14

Single-pulse (532 nm, 8 ns) micropatterning of silicon with nanometric surface modulation is demonstrated by irradiating through a diffracting pinhole. The irradiation results obtained at fluences above the melting threshold are characterized by scanning electron and scanning force microscopy and reveal a good agreement with Fresnel diffraction theory. The physical mechanism is identified and discussed on basis of both thermocapillary and chemicapillary induced material transport during the molten state of the surface.

Room Temperature Elastic Moduli and Vickers Hardness of Hot-Pressed LLZO Cubic Garnet

DTIC Science & Technology

2012-01-01

polishing compounds, Leco, St. Joseph, MI). X - ray diffraction and scanning electron microscopy (SEM) The microstructure of the hot-pressed specimens...was examined on uncoated fracture surfaces by SEM with an accelerating voltage of 1 and 3 kV. Phase purity was evaluated from X - ray diffraction data...the micro- structure appeared to be homogenous for the two hot- pressed LLZO specimens included in this study (Fig. 1). X - ray diffraction confirmed that

Scattering electrons in Budapest (and elsewhere)

NASA Astrophysics Data System (ADS)

Hargittai, István

1983-07-01

Some of the recent research of the Budapest Electron Diffraction Group is described in anecdotal—historical perspective (as suggested by the Editor of the Journal of Molecular Structure). The importance of international cooperation is emphasized.

Ultrafast Electron Diffraction: How It Works

ScienceCinema

None

2018-01-16

A new technology at SLAC uses high-energy electrons to unravel motions in materials that are faster than a tenth of a trillionth of a second, opening up new research opportunities in ultrafast science.

Ultrafast Electron Diffraction: How It Works

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

None

2015-08-05

A new technology at SLAC uses high-energy electrons to unravel motions in materials that are faster than a tenth of a trillionth of a second, opening up new research opportunities in ultrafast science.

Characterisation of phases in nanostructured, multilayered titanium alloys by analytical and high-resolution electron microscopy.

PubMed

Czyrska-Filemonowicz, A; Buffat, P A

2009-01-01

Surface processing of a Ti-6Al-4V alloy led to a complex multilayered microstructure containing several phases of the Ni-Ti-P-Al-O system, which improves the mechanical and tribological surface properties. The microstructure, chemical and phase compositions of the hard layer formed on the surface were investigated by LM, XRD, SEM as well as analytical/high-resolution TEM, STEM, EDS, electron diffraction and FIB. Phase identification based on electron diffraction, HRTEM and EDS microanalysis revealed the presence of several binary and ternary phases in the system Ti-Ni-P, sometimes with partial substitution of Ti by Al. However some phases, mainly nanoparticles, still remain not identified satisfactorily. Electron microscopy techniques used for identification of phases present in surface multilayers and some practical limits to their routine application are reminded here.

Synthesis of zirconia (ZrO2) nanowires via chemical vapor deposition

NASA Astrophysics Data System (ADS)

Baek, M. K.; Park, S. J.; Choi, D. J.

2017-02-01

Monoclinic zirconia nanowires were synthesized by chemical vapor deposition using ZrCl4 powder as a starting material at 1200 °C and 760 Torr. Graphite was employed as a substrate, and an Au thin film was pre-deposited on the graphite as a catalyst. The zirconia nanostructure morphology was observed through scanning electron microscopy and transmission electron microscopy. Based on X-ray diffraction, selected area electron diffraction, and Raman spectroscopy data, the resulting crystal structure was found to be single crystalline monoclinic zirconia. The homogeneous distributions of Zr, O and Au were studied by scanning transmission electron microscopy with energy dispersive X-ray spectroscopy mapping, and there was no metal droplet at the nanowire tips despite the use of an Au metal catalyst. This result is apart from that of conventional metal catalyzed nanowires.

Ferromagnetism in sphalerite and wurtzite CdS nanostructures

PubMed Central

2013-01-01

Room-temperature ferromagnetism is observed in undoped sphalerite and wurtzite CdS nanostructures which are synthesized by hydrothermal methods. Scanning electron microscopy and transmission electron microscopy results indicate that the sphalerite CdS samples show a spherical-like shape and the wurtzite CdS ones show a flower-like shape, both of which are aggregated by lots of smaller particles. The impurity of the samples has been ruled out by the results of X-ray diffraction, selected-area electron diffraction, and X-ray photoelectron spectroscopy. Magnetization measurements indicate that all the samples exhibit room-temperature ferromagnetism and the saturation magnetization decreases with the increased crystal sizes, revealing that the observed ferromagnetism is defect-related, which is also confirmed by the post-annealing processes. This finding in CdS should be the focus of future electronic and spintronic devices. PMID:23294671

Online in situ x-ray diffraction setup for structural modification studies during swift heavy ion irradiation

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

Grygiel, C.; Lebius, H.; Bouffard, S.

2012-01-15

The high energy density of electronic excitations due to the impact of swift heavy ions can induce structural modifications in materials. We present an x-ray diffractometer called ALIX (''Analyse en Ligne sur IRRSUD par diffraction de rayons X''), which has been set up at the low-energy beamline (IRRadiation SUD - IRRSUD) of the Grand Accelerateur National d'Ions Lourds facility, to allow the study of structural modification kinetics as a function of the ion fluence. The x-ray setup has been modified and optimized to enable irradiation by swift heavy ions simultaneously to x-ray pattern recording. We present the capability of ALIXmore » to perform simultaneous irradiation-diffraction by using energy discrimination between x-rays from diffraction and from ion-target interaction. To illustrate its potential, results of sequential or simultaneous irradiation-diffraction are presented in this article to show radiation effects on the structural properties of ceramics. Phase transition kinetics have been studied during xenon ion irradiation of polycrystalline MgO and SrTiO{sub 3}. We have observed that MgO oxide is radiation-resistant to high electronic excitations, contrary to the high sensitivity of SrTiO{sub 3}, which exhibits transition from the crystalline to the amorphous state during irradiation. By interpreting the amorphization kinetics of SrTiO{sub 3}, defect overlapping models are discussed as well as latent track characteristics. Together with a transmission electron microscopy study, we conclude that a single impact model describes the phase transition mechanism.« less