Structural characterization of nano-oxide layers in PtMn based specular spin valves

NASA Astrophysics Data System (ADS)

Zhou, Min; Chen, Lifan; Diao, Zhitao; Park, Chang-Man; Huai, Yiming

2005-05-01

A systematic structure characterization of nano-oxide layers (NOLs) and specular spin valves using x-ray diffraction and high-resolution transmission electron microscopy (HRTEM) has been studied. High-angle x-ray diffraction data show almost identical fcc textures for both natural and plasma NOL spin-valves. Low-angle x-ray reflectivity spectrum shows more deteriorated Kiessig fringes at high incident angles for natural oxide sample, indicating rougher interfaces in natural oxidation than in plasma oxidation. Oxygen exposure plays an important role in NOLs process. Fabricating NOLs without any crystal structure degradation is critical to obtain high MR ratio. HRTEM reveals that oxide clusters mixing with insufficiently oxidized CoFe layers prevailed in natural NOL, and the natural oxidation was inhomogeneous. In contrast, plasma NOL has a thinner, more homogeneously oxidized CoFe layers with sharp interfaces. In plasma NOLs, the structures still maintain CoFe crystal structure. The structures and magnetic correlation of the NOL specular spin valves are discussed.

Photoluminescence studies on Cd(1-x)Zn(x)S:Mn2+ nanocrystals.

PubMed

Sethi, Ruchi; Kumar, Lokendra; Pandey, A C

2009-09-01

Highly monodispersed, undoped and doped with Mn2+, binary and ternary (CdS, ZnS, Cd(1-x)Zn(x)S) compound semiconductor nanocrystals have been synthesized by co-precipitation method using citric acid as a stabilizer. As prepared sample are characterized by X-ray diffraction, Small angle X-ray scattering, Transmission electron microscope, Optical absorption and Photoluminescence spectroscopy, for their optical and structural properties. X-ray diffraction, Small angle X-ray scattering and Transmission electron microscope results confirm the preparation of monodispersed nanocrystals. Photoluminescence studies show a significant blue shift in the wavelength with an increasing concentration of Zn in alloy nanocrystals.

Yes, one can obtain better quality structures from routine X-ray data collection.

PubMed

Sanjuan-Szklarz, W Fabiola; Hoser, Anna A; Gutmann, Matthias; Madsen, Anders Østergaard; Woźniak, Krzysztof

2016-01-01

Single-crystal X-ray diffraction structural results for benzidine dihydrochloride, hydrated and protonated N,N,N,N-peri(dimethylamino)naphthalene chloride, triptycene, dichlorodimethyltriptycene and decamethylferrocene have been analysed. A critical discussion of the dependence of structural and thermal parameters on resolution for these compounds is presented. Results of refinements against X-ray data, cut off to different resolutions from the high-resolution data files, are compared to structural models derived from neutron diffraction experiments. The Independent Atom Model (IAM) and the Transferable Aspherical Atom Model (TAAM) are tested. The average differences between the X-ray and neutron structural parameters (with the exception of valence angles defined by H atoms) decrease with the increasing 2θmax angle. The scale of differences between X-ray and neutron geometrical parameters can be significantly reduced when data are collected to the higher, than commonly used, 2θmax diffraction angles (for Mo Kα 2θmax > 65°). The final structural and thermal parameters obtained for the studied compounds using TAAM refinement are in better agreement with the neutron values than the IAM results for all resolutions and all compounds. By using TAAM, it is still possible to obtain accurate results even from low-resolution X-ray data. This is particularly important as TAAM is easy to apply and can routinely be used to improve the quality of structural investigations [Dominiak (2015 ▸). LSDB from UBDB. University of Buffalo, USA]. We can recommend that, in order to obtain more adequate (more accurate and precise) structural and displacement parameters during the IAM model refinement, data should be collected up to the larger diffraction angles, at least, for Mo Kα radiation to 2θmax = 65° (sin θmax/λ < 0.75 Å(-1)). The TAAM approach is a very good option to obtain more adequate results even using data collected to the lower 2θmax angles. Also the results of translation-libration-screw (TLS) analysis and vibrational entropy values are more reliable for 2θmax > 65°.

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.

Characterization of low thermal conductivity PAN-based carbon fibers

NASA Technical Reports Server (NTRS)

Katzman, Howard A.; Adams, P. M.; Le, T. D.; Hemminger, Carl S.

1992-01-01

The microstructure and surface chemistry of eight low thermal conductivity (LTC) PAN-based carbon fibers were determined and compared with PAN-based fibers heat treated to higher temperatures. Based on wide-angle x ray diffraction, the LTC PAN fibers all appear to have a similar turbostratic structure with large 002 d-spacings, small crystallite sizes, and moderate preferred orientation. Limited small-angle x ray scattering (SAXS) results indicate that, with the exception of LTC fibers made by BASF, the LTC fibers do not have well developed pores. Transmission electron microscopy shows that the texture of the two LTC PAN-based fibers studied (Amoco T350/23X and /25X) consists of multiple sets of parallel, wavy, bent layers that interweave with each other forming a complex three dimensional network oriented randomly around the fiber axis. X ray photoelectron spectroscopy (XPS) analysis finds correlations between heat treated temperatures and the surface composition chemistry of the carbon fiber samples.

[Study on bamboo treated with gamma rays by X-ray diffraction].

PubMed

Sun, Feng-Bo; Fei, Ben-Hua; Jiang, Ze-Hui; Yu, Zi-Xuan; Tian, Gen-Lin; Yang, Quan-Wen

2011-06-01

The microfibril angle and crystallinity of bamboo treated with gamma rays were tested by X-ray diffraction (XRD). The result indicated that crystallinity in bamboo increased when irradiation dose was less than 100 kGy, while the irradiation dose was raised to about 100 kGy, crystallinity in bamboo reduced. But during the whole irradiation process, the influence on microfibril angle was not obvious, so it was not the dominant factors on variation in physical-mechanical properties of bamboo during the process of irradiation.

X-ray diffraction analysis of residual stresses in textured ZnO thin films

NASA Astrophysics Data System (ADS)

Dobročka, E.; Novák, P.; Búc, D.; Harmatha, L.; Murín, J.

2017-02-01

Residual stresses are commonly generated in thin films during the deposition process and can influence the film properties. Among a number of techniques developed for stress analysis, X-ray diffraction methods, especially the grazing incidence set-up, are of special importance due to their capability to analyze the stresses in very thin layers as well as to investigate the depth variation of the stresses. In this contribution a method combining multiple {hkl} and multiple χ modes of X-ray diffraction stress analysis in grazing incidence set-up is used for the measurement of residual stress in strongly textured ZnO thin films. The method improves the precision of the stress evaluation in textured samples. Because the measurements are performed at very low incidence angles, the effect of refraction of X-rays on the measured stress is analyzed in details for the general case of non-coplanar geometry. It is shown that this effect cannot be neglected if the angle of incidence approaches the critical angle. The X-ray stress factors are calculated for hexagonal fiber-textured ZnO for the Reuss model of grain-interaction and the effect of texture on the stress factors is analyzed. The texture in the layer is modelled by Gaussian distribution function. Numerical results indicate that in the process of stress evaluation the Reuss model can be replaced by much simpler crystallite group method if the standard deviation of Gaussian describing the texture is less than 6°. The results can be adapted for fiber-textured films of various hexagonal materials.

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.

Development of variable-magnification X-ray Bragg optics.

PubMed

Hirano, Keiichi; Yamashita, Yoshiki; Takahashi, Yumiko; Sugiyama, Hiroshi

2015-07-01

A novel X-ray Bragg optics is proposed for variable-magnification of an X-ray beam. This X-ray Bragg optics is composed of two magnifiers in a crossed arrangement, and the magnification factor, M, is controlled through the azimuth angle of each magnifier. The basic properties of the X-ray optics such as the magnification factor, image transformation matrix and intrinsic acceptance angle are described based on the dynamical theory of X-ray diffraction. The feasibility of the variable-magnification X-ray Bragg optics was verified at the vertical-wiggler beamline BL-14B of the Photon Factory. For X-ray Bragg magnifiers, Si(220) crystals with an asymmetric angle of 14° were used. The magnification factor was calculated to be tunable between 0.1 and 10.0 at a wavelength of 0.112 nm. At various magnification factors (M ≥ 1.0), X-ray images of a nylon mesh were observed with an air-cooled X-ray CCD camera. Image deformation caused by the optics could be corrected by using a 2 × 2 transformation matrix and bilinear interpolation method. Not only absorption-contrast but also edge-contrast due to Fresnel diffraction was observed in the magnified images.

Infrastructure development for radioactive materials at the NSLS-II

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

Sprouster, D. J.; Weidner, R.; Ghose, S. K.

2018-02-01

The X-ray Powder Diffraction (XPD) Beamline at the National Synchrotron Light Source-II is a multipurpose instrument designed for high-resolution, high-energy X-ray scattering techniques. In this article, the capabilities, opportunities and recent developments in the characterization of radioactive materials at XPD are described. The overarching goal of this work is to provide researchers access to advanced synchrotron techniques suited to the structural characterization of materials for advanced nuclear energy systems. XPD is a new beamline providing high photon flux for X-ray Diffraction, Pair Distribution Function analysis and Small Angle X-ray Scattering. The infrastructure and software described here extend the existing capabilitiesmore » at XPD to accommodate radioactive materials. Such techniques will contribute crucial information to the characterization and quantification of advanced materials for nuclear energy applications. We describe the automated radioactive sample collection capabilities and recent X-ray Diffraction and Small Angle X-ray Scattering results from neutron irradiated reactor pressure vessel steels and oxide dispersion strengthened steels.« less

Infrastructure development for radioactive materials at the NSLS-II

DOE PAGES

Sprouster, David J.; Weidner, R.; Ghose, S. K.; ...

2017-11-04

The X-ray Powder Diffraction (XPD) Beamline at the National Synchrotron Light Source-II is a multipurpose instrument designed for high-resolution, high-energy X-ray scattering techniques. In this paper, the capabilities, opportunities and recent developments in the characterization of radioactive materials at XPD are described. The overarching goal of this work is to provide researchers access to advanced synchrotron techniques suited to the structural characterization of materials for advanced nuclear energy systems. XPD is a new beamline providing high photon flux for X-ray Diffraction, Pair Distribution Function analysis and Small Angle X-ray Scattering. The infrastructure and software described here extend the existing capabilitiesmore » at XPD to accommodate radioactive materials. Such techniques will contribute crucial information to the characterization and quantification of advanced materials for nuclear energy applications. Finally, we describe the automated radioactive sample collection capabilities and recent X-ray Diffraction and Small Angle X-ray Scattering results from neutron irradiated reactor pressure vessel steels and oxide dispersion strengthened steels.« less

Near-surface density profiling of Fe ion irradiated Si (100) using extremely asymmetric x-ray diffraction by variation of the wavelength

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

Khanbabaee, B., E-mail: khanbabaee@physik.uni-siegen.de; Pietsch, U.; Facsko, S.

2014-10-20

In this work, we report on correlations between surface density variations and ion parameters during ion beam-induced surface patterning process. The near-surface density variations of irradiated Si(100) surfaces were investigated after off-normal irradiation with 5 keV Fe ions at different fluences. In order to reduce the x-ray probing depth to a thickness below 5 nm, the extremely asymmetrical x-ray diffraction by variation of wavelength was applied, exploiting x-ray refraction at the air-sample interface. Depth profiling was achieved by measuring x-ray rocking curves as function of varying wavelengths providing incidence angles down to 0°. The density variation was extracted from the deviationsmore » from kinematical Bragg angle at grazing incidence angles due to refraction of the x-ray beam at the air-sample interface. The simulations based on the dynamical theory of x-ray diffraction revealed that while a net near-surface density decreases with increasing ion fluence which is accompanied by surface patterning, there is a certain threshold of ion fluence to surface density modulation. Our finding suggests that the surface density variation can be relevant with the mechanism of pattern formation.« less

Resonance energy shifts during nuclear Bragg diffraction of x rays

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

Arthur, J.; Brown, G.S.; Brown, D.E.

1989-10-09

We have observed dramatic changes in the time distribution of synchrotron x rays resonantly scattered from {sup 57}Fe nuclei in a crystal of yttrium iron garnet, which depend on the deviation angle of the incident radiation from the Bragg angle. These changes are caused by small shifts in the effective energies of the hyperfine-split nuclear resonances, an effect of dynamical diffraction for the coherently excited nuclei in the crystal. The very high brightness of the synchro- tron x-ray source allows this effect to be observed in a 15-min measurement.

Observation of the strain field near the Si(111) 7 x 7 surface with a new X-ray diffraction technique.

PubMed

Emoto, T; Akimoto, K; Ichimiya, A

1998-05-01

A new X-ray diffraction technique has been developed in order to measure the strain field near a solid surface under ultrahigh vacuum (UHV) conditions. The X-ray optics use an extremely asymmetric Bragg-case bulk reflection. The glancing angle of the X-rays can be set near the critical angle of total reflection by tuning the X-ray energy. Using this technique, rocking curves for Si surfaces with different surface structures, i.e. a native oxide surface, a slightly oxide surface and an Si(111) 7 x 7 surface, were measured. It was found that the widths of the rocking curves depend on the surface structures. This technique is efficient in distinguishing the strain field corresponding to each surface structure.

Diffraction effects on angular response of X-ray collimators

NASA Technical Reports Server (NTRS)

Blake, R. L.; Barrus, D. M.; Fenimore, E.

1976-01-01

Angular responses have been measured for X-ray collimators with half-widths ranging from minutes of arc down to 10 arcsec. In the seconds-of-arc range, diffraction peaks at off-axis angles can masquerade as side lobes of the collimator angular response. Measurements and qualitative physical arguments lead to a rule of thumb for collimator design; namely, the angle of first minimum in the Fraunhofer single-slit diffraction pattern should be less than one-fourth of the collimator geometrical full-width at half-maximum intensity.

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

Diamond-anvil cell for radial x-ray diffraction.

PubMed

Chesnut, G N; Schiferl, D; Streetman, B D; Anderson, W W

2006-06-28

We have designed a new diamond-anvil cell capable of radial x-ray diffraction to pressures of a few hundred GPa. The diffraction geometry allows access to multiple angles of Ψ, which is the angle between each reciprocal lattice vector g(hkl) and the compression axis of the cell. At the 'magic angle', Ψ≈54.7°, the effects of deviatoric stresses on the interplanar spacings, d(hkl), are significantly reduced. Because the systematic errors, which are different for each d(hkl), are significantly reduced, the crystal structures and the derived equations of state can be determined reliably. At other values of Ψ, the effects of deviatoric stresses on the diffraction pattern could eventually be used to determine elastic constants.

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.

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.

A Compact X-Ray System for Support of High Throughput Crystallography

NASA Technical Reports Server (NTRS)

Ciszak, Ewa; Gubarev, Mikhail; Gibson, Walter M.; Joy, Marshall K.; Whitaker, Ann F. (Technical Monitor)

2001-01-01

Standard x-ray systems for crystallography rely on massive generators coupled with optics that guide X-ray beams onto the crystal sample. Optics for single-crystal diffractometry include total reflection mirrors, polycapillary optics or graded multilayer monochromators. The benefit of using polycapillary optic is that it can collect x-rays over tile greatest solid angle, and thus most efficiently, utilize the greatest portion of X-rays emitted from the Source, The x-ray generator has to have a small anode spot, and thus its size and power requirements can be substantially reduced We present the design and results from the first high flux x-ray system for crystallography that combine's a microfocus X-ray generator (40microns FWHM Spot size at a power of 45 W) and a collimating, polycapillary optic. Diffraction data collected from small test crystals with cell dimensions up to 160A (lysozyme and thaumatin) are of high quality. For example, diffraction data collected from a lysozyme crystal at RT yielded R=5.0% for data extending to 1.70A. We compare these results with measurements taken from standard crystallographic systems. Our current microfocus X-ray diffraction system is attractive for supporting crystal growth research in the standard crystallography laboratory as well as in remote, automated crystal growth laboratory. Its small volume, light-weight, and low power requirements are sufficient to have it installed in unique environments, i.e.. on-board International Space Station.

Multiple film plane diagnostic for shocked lattice measurements (invited)

NASA Astrophysics Data System (ADS)

Kalantar, Daniel H.; Bringa, E.; Caturla, M.; Colvin, J.; Lorenz, K. T.; Kumar, M.; Stölken, J.; Allen, A. M.; Rosolankova, K.; Wark, J. S.; Meyers, M. A.; Schneider, M.; Boehly, T. R.

2003-03-01

Laser-based shock experiments have been conducted in thin Si and Cu crystals at pressures above the Hugoniot elastic limit. In these experiments, static film and x-ray streak cameras recorded x rays diffracted from lattice planes both parallel and perpendicular to the shock direction. These data showed uniaxial compression of Si(100) along the shock direction and three-dimensional compression of Cu(100). In the case of the Si diffraction, there was a multiple wave structure observed, which may be due to a one-dimensional phase transition or a time variation in the shock pressure. A new film-based detector has been developed for these in situ dynamic diffraction experiments. This large-angle detector consists of three film cassettes that are positioned to record x rays diffracted from a shocked crystal anywhere within a full π steradian. It records x rays that are diffracted from multiple lattice planes both parallel and at oblique angles with respect to the shock direction. It is a time-integrating measurement, but time-resolved data may be recorded using a short duration laser pulse to create the diffraction source x rays. This new instrument has been fielded at the OMEGA and Janus lasers to study single-crystal materials shock compressed by direct laser irradiation. In these experiments, a multiple wave structure was observed on many different lattice planes in Si. These data provide information on the structure under compression.

Development of an x-ray prism for analyzer based imaging systems

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

Bewer, Brian; Chapman, Dean

Analyzer crystal based imaging techniques such as diffraction enhanced imaging (DEI) and multiple imaging radiography (MIR) utilize the Bragg peak of perfect crystal diffraction to convert angular changes into intensity changes. These x-ray techniques extend the capability of conventional radiography, which derives image contrast from absorption, by providing large intensity changes for small angle changes introduced from the x-ray beam traversing the sample. Objects that have very little absorption contrast may have considerable refraction and ultrasmall angle x-ray scattering contrast improving visualization and extending the utility of x-ray imaging. To improve on the current DEI technique an x-ray prism (XRP)more » was designed and included in the imaging system. The XRP allows the analyzer crystal to be aligned anywhere on the rocking curve without physically moving the analyzer from the Bragg angle. By using the XRP to set the rocking curve alignment rather than moving the analyzer crystal physically the needed angle sensitivity is changed from submicroradians for direct mechanical movement of the analyzer crystal to tens of milliradians for movement of the XRP angle. However, this improvement in angle positioning comes at the cost of absorption loss in the XRP and depends on the x-ray energy. In addition to using an XRP for crystal alignment it has the potential for scanning quickly through the entire rocking curve. This has the benefit of collecting all the required data for image reconstruction in a single measurement thereby removing some problems with motion artifacts which remain a concern in current DEI/MIR systems especially for living animals.« less

Development of an x-ray prism for analyzer based imaging systems

NASA Astrophysics Data System (ADS)

Bewer, Brian; Chapman, Dean

2010-08-01

Analyzer crystal based imaging techniques such as diffraction enhanced imaging (DEI) and multiple imaging radiography (MIR) utilize the Bragg peak of perfect crystal diffraction to convert angular changes into intensity changes. These x-ray techniques extend the capability of conventional radiography, which derives image contrast from absorption, by providing large intensity changes for small angle changes introduced from the x-ray beam traversing the sample. Objects that have very little absorption contrast may have considerable refraction and ultrasmall angle x-ray scattering contrast improving visualization and extending the utility of x-ray imaging. To improve on the current DEI technique an x-ray prism (XRP) was designed and included in the imaging system. The XRP allows the analyzer crystal to be aligned anywhere on the rocking curve without physically moving the analyzer from the Bragg angle. By using the XRP to set the rocking curve alignment rather than moving the analyzer crystal physically the needed angle sensitivity is changed from submicroradians for direct mechanical movement of the analyzer crystal to tens of milliradians for movement of the XRP angle. However, this improvement in angle positioning comes at the cost of absorption loss in the XRP and depends on the x-ray energy. In addition to using an XRP for crystal alignment it has the potential for scanning quickly through the entire rocking curve. This has the benefit of collecting all the required data for image reconstruction in a single measurement thereby removing some problems with motion artifacts which remain a concern in current DEI/MIR systems especially for living animals.

Development of an x-ray prism for analyzer based imaging systems.

PubMed

Bewer, Brian; Chapman, Dean

2010-08-01

Analyzer crystal based imaging techniques such as diffraction enhanced imaging (DEI) and multiple imaging radiography (MIR) utilize the Bragg peak of perfect crystal diffraction to convert angular changes into intensity changes. These x-ray techniques extend the capability of conventional radiography, which derives image contrast from absorption, by providing large intensity changes for small angle changes introduced from the x-ray beam traversing the sample. Objects that have very little absorption contrast may have considerable refraction and ultrasmall angle x-ray scattering contrast improving visualization and extending the utility of x-ray imaging. To improve on the current DEI technique an x-ray prism (XRP) was designed and included in the imaging system. The XRP allows the analyzer crystal to be aligned anywhere on the rocking curve without physically moving the analyzer from the Bragg angle. By using the XRP to set the rocking curve alignment rather than moving the analyzer crystal physically the needed angle sensitivity is changed from submicroradians for direct mechanical movement of the analyzer crystal to tens of milliradians for movement of the XRP angle. However, this improvement in angle positioning comes at the cost of absorption loss in the XRP and depends on the x-ray energy. In addition to using an XRP for crystal alignment it has the potential for scanning quickly through the entire rocking curve. This has the benefit of collecting all the required data for image reconstruction in a single measurement thereby removing some problems with motion artifacts which remain a concern in current DEI/MIR systems especially for living animals.

Note: application of a pixel-array area detector to simultaneous single crystal X-ray diffraction and X-ray absorption spectroscopy measurements.

PubMed

Sun, Cheng-Jun; Zhang, Bangmin; Brewe, Dale L; Chen, Jing-Sheng; Chow, G M; Venkatesan, T; Heald, Steve M

2014-04-01

X-ray diffraction (XRD) and X-ray absorption spectroscopy (XAS) are two main x-ray techniques in synchrotron radiation facilities. In this Note, we present an experimental setup capable of performing simultaneous XRD and XAS measurements by the application of a pixel-array area detector. For XRD, the momentum transfer in specular diffraction was measured by scanning the X-ray energy with fixed incoming and outgoing x-ray angles. By selecting a small fixed region of the detector to collect the XRD signal, the rest of the area was available for collecting the x-ray fluorescence for XAS measurements. The simultaneous measurement of XRD and X-ray absorption near edge structure for Pr0.67Sr0.33MnO3 film was demonstrated as a proof of principle for future time-resolved pump-probe measurements. A static sample makes it easy to maintain an accurate overlap of the X-ray spot and laser pump beam.

Diffraction based method to reconstruct the spectrum of the Thomson scattering x-ray source

NASA Astrophysics Data System (ADS)

Chi, Zhijun; Yan, Lixin; Zhang, Zhen; Zhou, Zheng; Zheng, Lianmin; Wang, Dong; Tian, Qili; Wang, Wei; Nie, Zan; Zhang, Jie; Du, Yingchao; Hua, Jianfei; Shi, Jiaru; Pai, Chihao; Lu, Wei; Huang, Wenhui; Chen, Huaibi; Tang, Chuanxiang

2017-04-01

As Thomson scattering x-ray sources based on the collision of intense laser and relativistic electrons have drawn much attention in various scientific fields, there is an increasing demand for the effective methods to reconstruct the spectrum information of the ultra-short and high-intensity x-ray pulses. In this paper, a precise spectrum measurement method for the Thomson scattering x-ray sources was proposed with the diffraction of a Highly Oriented Pyrolytic Graphite (HOPG) crystal and was demonstrated at the Tsinghua Thomson scattering X-ray source. The x-ray pulse is diffracted by a 15 mm (L) ×15 mm (H)× 1 mm (D) HOPG crystal with 1° mosaic spread. By analyzing the diffraction pattern, both x-ray peak energies and energy spectral bandwidths at different polar angles can be reconstructed, which agree well with the theoretical value and simulation. The higher integral reflectivity of the HOPG crystal makes this method possible for single-shot measurement.

Diffraction based method to reconstruct the spectrum of the Thomson scattering x-ray source.

PubMed

Chi, Zhijun; Yan, Lixin; Zhang, Zhen; Zhou, Zheng; Zheng, Lianmin; Wang, Dong; Tian, Qili; Wang, Wei; Nie, Zan; Zhang, Jie; Du, Yingchao; Hua, Jianfei; Shi, Jiaru; Pai, Chihao; Lu, Wei; Huang, Wenhui; Chen, Huaibi; Tang, Chuanxiang

2017-04-01

As Thomson scattering x-ray sources based on the collision of intense laser and relativistic electrons have drawn much attention in various scientific fields, there is an increasing demand for the effective methods to reconstruct the spectrum information of the ultra-short and high-intensity x-ray pulses. In this paper, a precise spectrum measurement method for the Thomson scattering x-ray sources was proposed with the diffraction of a Highly Oriented Pyrolytic Graphite (HOPG) crystal and was demonstrated at the Tsinghua Thomson scattering X-ray source. The x-ray pulse is diffracted by a 15 mm (L) ×15 mm (H)× 1 mm (D) HOPG crystal with 1° mosaic spread. By analyzing the diffraction pattern, both x-ray peak energies and energy spectral bandwidths at different polar angles can be reconstructed, which agree well with the theoretical value and simulation. The higher integral reflectivity of the HOPG crystal makes this method possible for single-shot measurement.

Influence of gamma ray irradiation on stoichiometry of hydrothermally synthesized bismuth telluride nanoparticles

NASA Astrophysics Data System (ADS)

Abishek, N. S.; Naik, K. Gopalakrishna

2018-05-01

Bismuth telluride (Bi2Te3) nanoparticles were synthesized by the hydrothermal method at 200 °C for 24 h. The synthesized Bi2Te3 nanoparticles were irradiated with gamma rays at doses of 50 kGy and 100 kGy. The structural characterization of the pre-irradiated and post-irradiated samples was carried out by X-ray diffraction technique and was found to have rhombohedral phase having R3 ¯m (166) space group. The X-ray diffraction peaks were found to shift towards lower diffraction angle with gamma ray irradiation. The morphologies and compositions of the grown Bi2Te3 nanoparticles were studied using Field Emission Scanning Electron Microscope and X-ray energy dispersive analysis, respectively. The possible cause for the shift in the X-ray diffraction peaks with gamma ray irradiation has been discussed in the present work.

An Optimized Table-Top Small-Angle X-ray Scattering Set-up for the Nanoscale Structural Analysis of Soft Matter

NASA Astrophysics Data System (ADS)

Sibillano, T.; de Caro, L.; Altamura, D.; Siliqi, D.; Ramella, M.; Boccafoschi, F.; Ciasca, G.; Campi, G.; Tirinato, L.; di Fabrizio, E.; Giannini, C.

2014-11-01

The paper shows how a table top superbright microfocus laboratory X-ray source and an innovative restoring-data algorithm, used in combination, allow to analyze the super molecular structure of soft matter by means of Small Angle X-ray Scattering ex-situ experiments. The proposed theoretical approach is aimed to restore diffraction features from SAXS profiles collected from low scattering biomaterials or soft tissues, and therefore to deal with extremely noisy diffraction SAXS profiles/maps. As biological test cases we inspected: i) residues of exosomes' drops from healthy epithelial colon cell line and colorectal cancer cells; ii) collagen/human elastin artificial scaffolds developed for vascular tissue engineering applications; iii) apoferritin protein in solution. Our results show how this combination can provide morphological/structural nanoscale information to characterize new artificial biomaterials and/or to get insight into the transition between healthy and pathological tissues during the progression of a disease, or to morphologically characterize nanoscale proteins, based on SAXS data collected in a room-sized laboratory.

A split-beam probe-pump-probe scheme for femtosecond time resolved protein X-ray crystallography

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

van Thor, Jasper J.; Madsen, Anders

In order to exploit the femtosecond pulse duration of X-ray Free-Electron Lasers (XFEL) operating in the hard X-ray regime for ultrafast time-resolved protein crystallography experiments, critical parameters that determine the crystallographic signal-to-noise (I/σI) must be addressed. For single-crystal studies under low absorbed dose conditions, it has been shown that the intrinsic pulse intensity stability as well as mode structure and jitter of this structure, significantly affect the crystallographic signal-to-noise. Here, geometrical parameters are theoretically explored for a three-beam scheme: X-ray probe, optical pump, X-ray probe (or “probe-pump-probe”) which will allow experimental determination of the photo-induced structure factor amplitude differences, ΔF,more » in a ratiometric manner, thereby internally referencing the intensity noise of the XFEL source. In addition to a non-collinear split-beam geometry which separates un-pumped and pumped diffraction patterns on an area detector, applying an additional convergence angle to both beams by focusing leads to integration over mosaic blocks in the case of well-ordered stationary protein crystals. Ray-tracing X-ray diffraction simulations are performed for an example using photoactive yellow protein crystals in order to explore the geometrical design parameters which would be needed. The specifications for an X-ray split and delay instrument that implements both an offset angle and focused beams are discussed, for implementation of a probe-pump-probe scheme at the European XFEL. We discuss possible extension of single crystal studies to serial femtosecond crystallography, particularly in view of the expected X-ray damage and ablation due to the first probe pulse.« less

A split-beam probe-pump-probe scheme for femtosecond time resolved protein X-ray crystallography

DOE PAGES

van Thor, Jasper J.; Madsen, Anders

2015-01-01

In order to exploit the femtosecond pulse duration of X-ray Free-Electron Lasers (XFEL) operating in the hard X-ray regime for ultrafast time-resolved protein crystallography experiments, critical parameters that determine the crystallographic signal-to-noise (I/σI) must be addressed. For single-crystal studies under low absorbed dose conditions, it has been shown that the intrinsic pulse intensity stability as well as mode structure and jitter of this structure, significantly affect the crystallographic signal-to-noise. Here, geometrical parameters are theoretically explored for a three-beam scheme: X-ray probe, optical pump, X-ray probe (or “probe-pump-probe”) which will allow experimental determination of the photo-induced structure factor amplitude differences, ΔF,more » in a ratiometric manner, thereby internally referencing the intensity noise of the XFEL source. In addition to a non-collinear split-beam geometry which separates un-pumped and pumped diffraction patterns on an area detector, applying an additional convergence angle to both beams by focusing leads to integration over mosaic blocks in the case of well-ordered stationary protein crystals. Ray-tracing X-ray diffraction simulations are performed for an example using photoactive yellow protein crystals in order to explore the geometrical design parameters which would be needed. The specifications for an X-ray split and delay instrument that implements both an offset angle and focused beams are discussed, for implementation of a probe-pump-probe scheme at the European XFEL. We discuss possible extension of single crystal studies to serial femtosecond crystallography, particularly in view of the expected X-ray damage and ablation due to the first probe pulse.« less

A split-beam probe-pump-probe scheme for femtosecond time resolved protein X-ray crystallography

PubMed Central

van Thor, Jasper J.; Madsen, Anders

2015-01-01

In order to exploit the femtosecond pulse duration of X-ray Free-Electron Lasers (XFEL) operating in the hard X-ray regime for ultrafast time-resolved protein crystallography experiments, critical parameters that determine the crystallographic signal-to-noise (I/σI) must be addressed. For single-crystal studies under low absorbed dose conditions, it has been shown that the intrinsic pulse intensity stability as well as mode structure and jitter of this structure, significantly affect the crystallographic signal-to-noise. Here, geometrical parameters are theoretically explored for a three-beam scheme: X-ray probe, optical pump, X-ray probe (or “probe-pump-probe”) which will allow experimental determination of the photo-induced structure factor amplitude differences, ΔF, in a ratiometric manner, thereby internally referencing the intensity noise of the XFEL source. In addition to a non-collinear split-beam geometry which separates un-pumped and pumped diffraction patterns on an area detector, applying an additional convergence angle to both beams by focusing leads to integration over mosaic blocks in the case of well-ordered stationary protein crystals. Ray-tracing X-ray diffraction simulations are performed for an example using photoactive yellow protein crystals in order to explore the geometrical design parameters which would be needed. The specifications for an X-ray split and delay instrument that implements both an offset angle and focused beams are discussed, for implementation of a probe-pump-probe scheme at the European XFEL. We discuss possible extension of single crystal studies to serial femtosecond crystallography, particularly in view of the expected X-ray damage and ablation due to the first probe pulse. PMID:26798786

Development of an X-ray prism for a combined diffraction enhanced imaging and fluorescence imaging system

NASA Astrophysics Data System (ADS)

Bewer, Brian E.

Analyzer crystal based imaging techniques such as diffraction enhanced imaging (DEI) and multiple imaging radiography (MIR) utilize the Bragg peak of perfect crystal diffraction to convert angular changes into intensity changes. These X-ray techniques extend the capability of conventional radiography, which derives image contrast from absorption, by providing a large change in intensity for a small angle change introduced by the X-ray beam traversing the sample. Objects that have very little absorption contrast may have considerable refraction and ultra small angle X-ray scattering (USAXS) contrast thus improving visualization and extending the utility of X-ray imaging. To improve on the current DEI technique this body of work describes the design of an X-ray prism (XRP) included in the imaging system which allows the analyzer crystal to be aligned anywhere on the rocking curve without moving the analyzer from the Bragg angle. By using the XRP to set the rocking curve alignment rather than moving the analyzer crystal physically the needed angle sensitivity is changed from muradians for direct mechanical movement of the analyzer crystal to milliradian control for movement the XRP angle. In addition to using an XRP for the traditional DEI acquisition method of two scans on opposite sides of the rocking curve preliminary tests will be presented showing the potential of using an XRP to scan quickly through the entire rocking curve. This has the benefit of collecting all the required data for image reconstruction in a single fast measurement thus removing the occurrence of motion artifacts for each point or line used during a scan. The XRP design is also intended to be compatible with combined imaging systems where more than one technique is used to investigate a sample. Candidates for complimentary techniques are investigated and measurements from a combined X-ray imaging system are presented.

Cryogenic x-ray diffraction microscopy utilizing high-pressure cryopreservation

NASA Astrophysics Data System (ADS)

Lima, Enju; Chushkin, Yuriy; van der Linden, Peter; Kim, Chae Un; Zontone, Federico; Carpentier, Philippe; Gruner, Sol M.; Pernot, Petra

2014-10-01

We present cryo x-ray diffraction microscopy of high-pressure-cryofixed bacteria and report high-convergence imaging with multiple image reconstructions. Hydrated D. radiodurans cells were cryofixed at 200 MPa pressure into ˜10-μm-thick water layers and their unstained, hydrated cellular environments were imaged by phasing diffraction patterns, reaching sub-30-nm resolutions with hard x-rays. Comparisons were made with conventional ambient-pressure-cryofixed samples, with respect to both coherent small-angle x-ray scattering and the image reconstruction. The results show a correlation between the level of background ice signal and phasing convergence, suggesting that phasing difficulties with frozen-hydrated specimens may be caused by high-background ice scattering.

Nanofiber-Based Bulk-Heterojunction Organic Solar Cells Using Coaxial Electrospinning

DTIC Science & Technology

2012-01-01

chains are likely oriented with the [010] direction, perpendicular to the substrate, in the fi lm device. Glancing incidence X - ray diffraction (GIXD...Electron and X - ray diffraction measurements were per- formed in order to study the structural order in annealed fi bers and devices. For reference... angle X - ray scattering (SAXS/WAXS) beamline 7.3.3 of the Advanced Light Source at Lawrence Berkeley National Laboratory at 10 keV (1.24 Å) from a bend

Peculiarities of section topograms for the multiple diffraction of X rays

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

Kohn, V. G., E-mail: kohnvict@yandex.ru; Smirnova, I. A.

The distortion of interference fringes on the section topograms of single crystal due to the multiple diffraction of X rays has been investigated. The cases of the 220 and 400 reflections in a silicon crystal in the form of a plate with a surface oriented normally to the [001] direction are considered both theoretically and experimentally. The same section topogram exhibits five cases of multiple diffraction at small azimuthal angles for the 400 reflection and MoK{sub α} radiation, while the topogram for the 220 reflection demonstrates two cases of multiple diffraction. All these cases correspond to different combinations of reciprocalmore » lattice vectors. Exact theoretical calculations of section topograms for the aforementioned cases of multiple diffraction have been performed for the first time. The section topograms exhibit two different distortion regions. The distortions in the central region of the structure are fairly complex and depend strongly on the azimuthal angle. In the tails of the multiple diffraction region, there is a shift of two-beam interference fringes, which can be observed even with a laboratory X-ray source.« less

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

Amaya, Andrew J.; Pathak, Harshad; Modak, Viraj P.

Using an X-ray laser, we investigated the crystal structure of ice formed by homogeneous ice nucleation in deeply supercooled water nanodrops (r ≈ 10 nm) at ~225 K. The nanodrops were formed by condensation of vapor in a supersonic nozzle, and the ice was probed within 100 μs of freezing using femtosecond wide-angle X-ray scattering at the Linac Coherent Light Source free-electron X-ray laser. The X-ray diffraction spectra indicate that this ice has a metastable, predominantly cubic structure; the shape of the first ice diffraction peak suggests stacking-disordered ice with a cubicity value, χ, in the range of 0.78 ±more » 0.05. The cubicity value determined here is higher than those determined in experiments with micron-sized drops but comparable to those found in molecular dynamics simulations. Lastly, the high cubicity is most likely caused by the extremely low freezing temperatures and by the rapid freezing, which occurs on a ~1 μs time scale in single nanodroplets.« less

How Cubic Can Ice Be?

DOE PAGES

Amaya, Andrew J.; Pathak, Harshad; Modak, Viraj P.; ...

2017-06-28

Using an X-ray laser, we investigated the crystal structure of ice formed by homogeneous ice nucleation in deeply supercooled water nanodrops (r ≈ 10 nm) at ~225 K. The nanodrops were formed by condensation of vapor in a supersonic nozzle, and the ice was probed within 100 μs of freezing using femtosecond wide-angle X-ray scattering at the Linac Coherent Light Source free-electron X-ray laser. The X-ray diffraction spectra indicate that this ice has a metastable, predominantly cubic structure; the shape of the first ice diffraction peak suggests stacking-disordered ice with a cubicity value, χ, in the range of 0.78 ±more » 0.05. The cubicity value determined here is higher than those determined in experiments with micron-sized drops but comparable to those found in molecular dynamics simulations. Lastly, the high cubicity is most likely caused by the extremely low freezing temperatures and by the rapid freezing, which occurs on a ~1 μs time scale in single nanodroplets.« less

High-resolution ab initio three-dimensional x-ray diffraction microscopy

DOE PAGES

Chapman, Henry N.; Barty, Anton; Marchesini, Stefano; ...

2006-01-01

Coherent x-ray diffraction microscopy is a method of imaging nonperiodic isolated objects at resolutions limited, in principle, by only the wavelength and largest scattering angles recorded. We demonstrate x-ray diffraction imaging with high resolution in all three dimensions, as determined by a quantitative analysis of the reconstructed volume images. These images are retrieved from the three-dimensional diffraction data using no a priori knowledge about the shape or composition of the object, which has never before been demonstrated on a nonperiodic object. We also construct two-dimensional images of thick objects with greatly increased depth of focus (without loss of transverse spatialmore » resolution). These methods can be used to image biological and materials science samples at high resolution with x-ray undulator radiation and establishes the techniques to be used in atomic-resolution ultrafast imaging at x-ray free-electron laser sources.« less

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.

Nanoscale femtosecond imaging of transient hot solid density plasmas with elemental and charge state sensitivity using resonant coherent diffraction

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

Kluge, T., E-mail: t.kluge@hzdr.de; Bussmann, M.; Huang, L. G., E-mail: lingen.huang@hzdr.de

Here, we propose to exploit the low energy bandwidth, small wavelength, and penetration power of ultrashort pulses from XFELs for resonant Small Angle Scattering (SAXS) on plasma structures in laser excited plasmas. Small angle scattering allows to detect nanoscale density fluctuations in forward scattering direction. Typically, the SAXS signal from laser excited plasmas is expected to be dominated by the free electron distribution. We propose that the ionic scattering signal becomes visible when the X-ray energy is in resonance with an electron transition between two bound states (resonant coherent X-ray diffraction). In this case, the scattering cross-section dramatically increases somore » that the signal of X-ray scattering from ions silhouettes against the free electron scattering background which allows to measure the opacity and derived quantities with high spatial and temporal resolution, being fundamentally limited only by the X-ray wavelength and timing. Deriving quantities such as ion spatial distribution, charge state distribution, and plasma temperature with such high spatial and temporal resolution will make a vast number of processes in shortpulse laser-solid interaction accessible for direct experimental observation, e.g., hole-boring and shock propagation, filamentation and instability dynamics, electron transport, heating, and ultrafast ionization dynamics.« less

Time-resolved coherent X-ray diffraction imaging of surface acoustic waves

PubMed Central

Nicolas, Jan-David; Reusch, Tobias; Osterhoff, Markus; Sprung, Michael; Schülein, Florian J. R.; Krenner, Hubert J.; Wixforth, Achim; Salditt, Tim

2014-01-01

Time-resolved coherent X-ray diffraction experiments of standing surface acoustic waves, illuminated under grazing incidence by a nanofocused synchrotron beam, are reported. The data have been recorded in stroboscopic mode at controlled and varied phase between the acoustic frequency generator and the synchrotron bunch train. At each time delay (phase angle), the coherent far-field diffraction pattern in the small-angle regime is inverted by an iterative algorithm to yield the local instantaneous surface height profile along the optical axis. The results show that periodic nanoscale dynamics can be imaged at high temporal resolution in the range of 50 ps (pulse length). PMID:25294979

Time-resolved coherent X-ray diffraction imaging of surface acoustic waves.

PubMed

Nicolas, Jan-David; Reusch, Tobias; Osterhoff, Markus; Sprung, Michael; Schülein, Florian J R; Krenner, Hubert J; Wixforth, Achim; Salditt, Tim

2014-10-01

Time-resolved coherent X-ray diffraction experiments of standing surface acoustic waves, illuminated under grazing incidence by a nanofocused synchrotron beam, are reported. The data have been recorded in stroboscopic mode at controlled and varied phase between the acoustic frequency generator and the synchrotron bunch train. At each time delay (phase angle), the coherent far-field diffraction pattern in the small-angle regime is inverted by an iterative algorithm to yield the local instantaneous surface height profile along the optical axis. The results show that periodic nanoscale dynamics can be imaged at high temporal resolution in the range of 50 ps (pulse length).

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.

Risk and benefit of diffraction in Energy Dispersive X-ray fluorescence mapping

NASA Astrophysics Data System (ADS)

Nikonow, Wilhelm; Rammlmair, Dieter

2016-11-01

Energy dispersive X-ray fluorescence mapping (μ-EDXRF) is a fast and non-destructive method for chemical quantification and therefore used in many scientific fields. The combination of spatial and chemical information is highly valuable for understanding geological processes. Problems occur with crystalline samples due to diffraction, which appears according to Bragg's law, depending on the energy of the X-ray beam, the incident angle and the crystal parameters. In the spectra these peaks can overlap with element peaks suggesting higher element concentrations. The aim of this study is to investigate the effect of diffraction, the possibility of diffraction removal and potential geoscientific applications for X-ray mapping. In this work the μ-EDXRF M4 Tornado from Bruker was operated with a Rh-tube and polychromatic beam with two SDD detectors mounted each at ± 90° to the tube. Due to the polychromatic beam the Bragg condition fits for several mineral lattice planes. Since diffraction depends on the angle, it is shown that a novel correction approach can be applied by measuring from two different angles and calculating the minimum spectrum of both detectors gaining a better limit of quantification for this method. Furthermore, it is possible to use the diffraction information for separation of differently oriented crystallites within a monomineralic aggregate and obtain parameters like particle size distribution for the sample, as it is done by thin section image analysis in cross-polarized light. Only with μ-EDXRF this can be made on larger samples without preparation of thin sections.

Innovative diffraction gratings for high-resolution resonant inelastic soft x-ray scattering spectroscopy

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

Voronov, D.L.; Warwick, T.; Gullikson, E. M.

2016-07-27

High-resolution Resonant Inelastic X-ray Scattering (RIXS) requires diffraction gratings with very exacting characteristics. The gratings should provide both very high dispersion and high efficiency which are conflicting requirements and extremely challenging to satisfy in the soft x-ray region for a traditional grazing incidence geometry. To achieve high dispersion one should increase the groove density of a grating; this however results in a diffraction angle beyond the critical angle range and results in drastic efficiency loss. The problem can be solved by use of multilayer coated blazed gratings (MBG). In this work we have investigated the diffraction characteristics of MBGs viamore » numerical simulations and have developed a procedure for optimization of grating design for a multiplexed high resolution imaging spectrometer for RIXS spectroscopy to be built in sector 6 at the Advanced Light Source (ALS). We found that highest diffraction efficiency can be achieved for gratings optimized for 4{sup th} or 5{sup th} order operation. Fabrication of such gratings is an extremely challenging technological problem. We present a first experimental prototype of these gratings and report its performance. High order and high line density gratings have the potential to be a revolutionary new optical element that should have great impact in the area of soft x-ray RIXS.« less

AEGIS: An Astrophysics Experiment for Grating and Imaging Spectroscopy---a Soft X-ray, High-resolution Spectrometer

NASA Astrophysics Data System (ADS)

Huenemoerder, David; Bautz, M. W.; Davis, J. E.; Heilmann, R. K.; Houck, J. C.; Marshall, H. L.; Neilsen, J.; Nicastro, F.; Nowak, M. A.; Schattenburg, M. L.; Schulz, N. S.; Smith, R. K.; Wolk, S.; AEGIS Team

2012-01-01

AEGIS is a concept for a high-resolution soft X-ray spectroscopic observatory developed in response to NASA's request for definitions of the next X-ray astronomy mission. At a small fraction of the cost of the once-planned International X-ray Observatory (IXO), AEGIS has capabilities that surpass IXO grating spectrometer requirements, and which are far superior to those of existing soft X-ray spectrometers. AEGIS incorporates innovative technology in X-ray optics, diffraction gratings and detectors. The mirror uses high area-to-mass ratio segmented glass architecture developed for IXO, but with smaller aperture and larger graze angles optimized for high-throughput grating spectroscopy with low mass and cost. The unique Critical Angle Transmission gratings combine low mass and relaxed figure and alignment tolerances of Chandra transmission gratings but with high diffraction efficiency and resolving power of blazed reflection gratings. With more than an order of magnitude better performance over Chandra and XMM grating spectrometers, AEGIS can obtain high quality spectra of bright AGN in a few hours rather than 10 days. Such high resolving power allows detailed kinematic studies of galactic outflows, hot gas in galactic haloes, and stellar accretion flows. Absorption line spectroscopy will be used to study large scale structure, cosmic feedback, and growth of black holes in thousands of sources to great distances. AEGIS will enable powerful multi-wavelength investigations, for example with Hubble/COS in the UV to characterize the intergalactic medium. AEGIS will be the first observatory with sufficient resolution below 1 keV to resolve thermally-broadened lines in hot ( 10 MK) plasmas. Here we describe key science investigations enable by Aegis, its scientific payload and mission plan. Acknowledgements: Support was provided in part by: NASA SAO contract SV3-73016 to MIT for the Chandra X-ray Center and Science Instruments; NASA grant NNX08AI62G; and the MKI Instrumentation Development Fund.

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

NASA Astrophysics Data System (ADS)

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

1999-04-01

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

THz-pump and X-ray-probe sources based on an electron linac

NASA Astrophysics Data System (ADS)

Setiniyaz, Sadiq; Park, Seong Hee; Kim, Hyun Woo; Vinokurov, Nikolay A.; Jang, Kyu-Ha; Lee, Kitae; Baek, In Hyung; Jeong, Young Uk

2017-11-01

We describe a compact THz-pump and X-ray-probe beamline, based on an electron linac, for ultrafast time-resolved diffraction applications. Two high-energy electron (γ > 50) bunches, 5 ns apart, impinge upon a single-foil or multifoil radiator and generate THz radiation and X-rays simultaneously. The THz pulse from the first bunch is synchronized to the X-ray beam of the second bunch by using an adjustable optical delay of a THz pulse. The peak power of THz radiation from the multifoil radiator is estimated to be 0.14 GW for a 200 pC well-optimized electron bunch. GEANT4 simulations show that a carbon foil with a thickness of 0.5-1.0 mm has the highest yield of 10-20 keV hard X-rays for a 25 MeV beam, which is approximately 103 photons/(keV pC-electrons) within a few degrees of the polar angle. A carbon multifoil radiator with 35 foils (25 μm thick each) can generate close to 103 hard X-rays/(keV pC-electrons) within a 2° acceptance angle. With 200 pC charge and a 100 Hz repetition rate, we can generate 107 X-rays per 1 keV energy bin per second or 105 X-rays per 1 keV energy bin per pulse. The longitudinal time profile of an X-ray pulse ranges from 400 to 600 fs depending on the acceptance angle. The broadening of the time duration of an X-ray pulse is observed owing to its diverging effect. A double-crystal monochromator will be used to select and transport the desired X-rays to the sample. The heating of the radiators by an electron beam is negligible because of the low beam current.

Towards shot-noise limited diffraction experiments with table-top femtosecond hard x-ray sources.

PubMed

Holtz, Marcel; Hauf, Christoph; Weisshaupt, Jannick; Salvador, Antonio-Andres Hernandez; Woerner, Michael; Elsaesser, Thomas

2017-09-01

Table-top laser-driven hard x-ray sources with kilohertz repetition rates are an attractive alternative to large-scale accelerator-based systems and have found widespread applications in x-ray studies of ultrafast structural dynamics. Hard x-ray pulses of 100 fs duration have been generated at the Cu K α wavelength with a photon flux of up to 10 9 photons per pulse into the full solid angle, perfectly synchronized to the sub-100-fs optical pulses from the driving laser system. Based on spontaneous x-ray emission, such sources display a particular noise behavior which impacts the sensitivity of x-ray diffraction experiments. We present a detailed analysis of the photon statistics and temporal fluctuations of the x-ray flux, together with experimental strategies to optimize the sensitivity of optical pump/x-ray probe experiments. We demonstrate measurements close to the shot-noise limit of the x-ray source.

Towards shot-noise limited diffraction experiments with table-top femtosecond hard x-ray sources

PubMed Central

Holtz, Marcel; Hauf, Christoph; Weisshaupt, Jannick; Salvador, Antonio-Andres Hernandez; Woerner, Michael; Elsaesser, Thomas

2017-01-01

Table-top laser-driven hard x-ray sources with kilohertz repetition rates are an attractive alternative to large-scale accelerator-based systems and have found widespread applications in x-ray studies of ultrafast structural dynamics. Hard x-ray pulses of 100 fs duration have been generated at the Cu Kα wavelength with a photon flux of up to 109 photons per pulse into the full solid angle, perfectly synchronized to the sub-100-fs optical pulses from the driving laser system. Based on spontaneous x-ray emission, such sources display a particular noise behavior which impacts the sensitivity of x-ray diffraction experiments. We present a detailed analysis of the photon statistics and temporal fluctuations of the x-ray flux, together with experimental strategies to optimize the sensitivity of optical pump/x-ray probe experiments. We demonstrate measurements close to the shot-noise limit of the x-ray source. PMID:28795079

X-ray diffraction-based electronic structure calculations and experimental x-ray analysis for medical and materials applications

NASA Astrophysics Data System (ADS)

Mahato, Dip Narayan

This thesis includes x-ray experiments for medical and materials applications and the use of x-ray diffraction data in a first-principles study of electronic structures and hyperfine properties of chemical and biological systems. Polycapillary focusing lenses were used to collect divergent x rays emitted from conventional x-ray tubes and redirect them to form an intense focused beam. These lenses are routinely used in microbeam x-ray fluorescence analysis. In this thesis, their potential application to powder diffraction and focused beam orthovoltage cancer therapy has been investigated. In conventional x-ray therapy, very high energy (˜ MeV) beams are used, partly to reduce the skin dose. For any divergent beam, the dose is necessarily highest at the entry point, and decays exponentially into the tissue. To reduce the skin dose, high energy beams, which have long absorption lengths, are employed, and rotated about the patient to enter from different angles. This necessitates large expensive specialized equipment. A focused beam could concentrate the dose within the patient. Since this is inherently skin dose sparing, lower energy photons could be employed. A primary concern in applying focused beams to therapy is whether the focus would be maintained despite Compton scattering within the tissue. To investigate this, transmission and focal spot sizes as a function of photon energy of two polycapillary focusing lenses were measured. The effects of tissue-equivalent phantoms of different thicknesses on the focal spot size were studied. Scatter fraction and depth dose were calculated. For powder diffraction, the polycapillary optics provide clean Gaussian peaks, which result in angular resolution that is much smaller than the peak width due to the beam convergence. Powder diffraction (also called coherent scatter) without optics can also be used to distinguish between tissue types that, because they have different nanoscale structures, scatter at different angles. Measurements were performed on the development of coherent scatter imaging to provide tissue type information in mammography. Atomic coordinates from x-ray diffraction data were used to study the nuclear quadrupole interactions and nature of molecular binding in DNA/RNA nucleobases and molecular solid BF3 systems.

A Microbeam Small-Angle X-ray Scattering Study on Enamel Crystallites in Subsurface Lesion

NASA Astrophysics Data System (ADS)

Yagi, N.; Ohta, N.; Matsuo, T.; Tanaka, T.; Terada, Y.; Kamasaka, H.; Kometani, T.

2010-10-01

The early caries lesion in bovine tooth enamel was studied by two different X-ray diffraction systems at the SPring-8 third generation synchrotron radiation facility. Both allowed us simultaneous measurement of the small and large angle regions. The beam size was 6μm at BL40XU and 50μm at BL45XU. The small-angle scattering from voids in the hydroxyapatite crystallites and the wide-angle diffraction from the hydroxyapatite crystals were observed simultaneously. At BL40XU an X-ray image intensifier was used for the small-angle and a CMOS flatpanel detector for the large-angle region. At BL45XU, a large-area CCD detector was used to cover both regions. A linear microbeam scan at BL40XU showed a detailed distribution of voids and crystals and made it possible to examine the structural details in the lesion. The two-dimensional scan at BL45XU showed distribution of voids and crystals in a wider region in the enamel. The simultaneous small- and wide-angle measurement with a microbeam is a powerful tool to elucidate the mechanisms of demineralization and remineralization in the early caries lesion.

High-pressure Irreversible Amorphization of La1/3NbO3

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

I Halevy; A Hen; A Broide

2011-12-31

The crystallographic structure of La{sub 1/3}NbO{sub 3} perovskite was studied at high pressures using a diamond-anvil cell and synchrotron radiation. High-pressure energy dispersive (EDS) x-ray diffraction and high-pressure angle dispersive (ADS) x-ray diffraction revealed an irreversible amorphization at {approx}10 GPa. A large change in the bulk modulus accompanied the high-pressure amorphization.

Two-dimensional time-resolved X-ray diffraction study of liquid/solid fraction and solid particle size in Fe-C binary system with an electrostatic levitator furnace

NASA Astrophysics Data System (ADS)

Yonemura, M.; Okada, J.; Watanabe, Y.; Ishikawa, T.; Nanao, S.; Shobu, T.; Toyokawa, H.

2013-03-01

Liquid state provides functions such as matter transport or a reaction field and plays an important role in manufacturing processes such as refining, forging or welding. However, experimental procedures are significantly difficult for an observation of solidification process of iron and iron-based alloys in order to identify rapid transformations subjected to fast temperature evolution. Therefore, in order to study the solidification in iron and iron-based alloys, we considered a combination of high energy X-ray diffraction measurements and an electrostatic levitation method (ESL). In order to analyze the liquid/solid fraction, the solidification of melted spherical specimens was measured at a time resolution of 0.1 seconds during rapid cooling using the two-dimensional time-resolved X-ray diffraction. Furthermore, the observation of particle sizes and phase identification was performed on a trial basis using X-ray small angle scattering with X-ray diffraction.

Magnetic x-ray dichroism in ultrathin epitaxial films

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

Tobin, J.G.; Goodman, K.W.; Cummins, T.R.

1997-04-01

The authors have used Magnetic X-ray Linear Dichroism (MXLD) and Magnetic X-ray Circular Dichroism (MXCD) to study the magnetic properties of epitaxial overlayers in an elementally specific fashion. Both MXLD and MXCD Photoelectron Spectroscopy were performed in a high resolution mode at the Spectromicroscopy Facility of the ALS. Circular Polarization was obtained via the utilization of a novel phase retarder (soft x-ray quarter wave plate) based upon transmission through a multilayer film. The samples were low temperature Fe overlayers, magnetic alloy films of NiFe and CoNi, and Gd grown on Y. The authors results include a direct comparison of highmore » resolution angle resolved Photoelectron Spectroscopy performed in MXLD and MXCD modes as well as structural studies with photoelectron diffraction.« less

A simple and low temperature process for super-hydrophilic rutile TiO 2 thin films growth

NASA Astrophysics Data System (ADS)

Mane, R. S.; Joo, Oh-Shim; Min, Sun-Ki; Lokhande, C. D.; Han, Sung-Hwan

2006-11-01

We investigate an environmentally friendly aqueous solution system for rutile TiO2 violet color nanocrystalline thin films growth on ITO substrate at room temperature. Film shows considerable absorption in visible region with excitonic maxima at 434 nm. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED), UV-vis, water surface contact angle and energy dispersive X-ray analysis (EDX) techniques in addition to actual photo-image that shows purely rutile phase of TiO2 with violet color, super-hydrophilic and densely packed nanometer-sized spherical grains of approximate diameter 3.15 ± 0.4 nm, characterize the films. Band gap energy of 4.61 eV for direct transition was obtained for the rutile TiO2 films. Film surface shows super-hydrophilic behavior, as exhibited water contact angle was 7°. Strong visible absorption (not due to chlorine) leaves future challenge to use these films in extremely thin absorber (ETA) solar cells.

Coherent assembly of heterostructures in ternary and quaternary carbonitrides

NASA Astrophysics Data System (ADS)

Caicedo, J. C.; Aperador, W.; Saldarriaga, W.

2018-05-01

In this study, ternary and quaternary carbonitride heterostructure systems were grown on silicon (100) substrates in order to investigate coherent assembly in TiCN/TiNbCN. The heterostructure films were grown using the reactive r. f. magnetron sputtering technique by systematically varying the bilayer period (Λ) and the bilayer number (n), while maintaining a constant total coating thickness (∼3 μm). The heterostructures were characterized by high angle X-ray diffraction (HA-XRD) and low angle X-ray diffraction, while the TiCN and TiNbCN layers were analyzed by X-ray photoelectron spectroscopy and transmission electron microscopy. The HA-XRD results indicated preferential growth in the face-centered cubic (111) crystal structure for the [TiCN/TiNbCN]n heterostructures. The maximum coherent assembly was observed with the presence of satellite peaks. Thus, ternary and quaternary carbonitride films were designed and deposited on Si (100) substrates with bilayer periods (Λ) in a broad range from nanometers to hundreds of nanometers in order to study the structural evolution and coherent assembly progress as the bilayer thickness decreased. We determined physical properties comprising the critical angle (θc) (0.362°), electronic density (ρe) (0.521 × 1033 el/m3), dispersion coefficient (δ) (0.554 el/m3), and refractive index (n) (0.999944) as functions of the number of bilayers (n).

Theoretical calculation of coherent Laue-case conversion between x-rays and ALPs for an x-ray light-shining-through-a-wall experiment

NASA Astrophysics Data System (ADS)

Yamaji, T.; Yamazaki, T.; Tamasaku, K.; Namba, T.

2017-12-01

Single crystals have high atomic electric fields as much as 1 011 V /m , which correspond to magnetic fields of ˜103 T . These fields can be utilized to convert x-rays into axionlike particles (ALPs) coherently similar to x-ray diffraction. In this paper, we perform the first theoretical calculation of the Laue-case conversion in crystals based on the Darwin dynamical theory of x-ray diffraction. The calculation shows that the Laue-case conversion has longer interaction length than the Bragg case, and that ALPs in the keV range can be resonantly converted by tuning an incident angle of x-rays. ALPs with mass up to O (10 keV ) can be searched by light-shining-through-a-wall (LSW) experiments at synchrotron x-ray facilities.

X-ray imaging crystal spectrometer for extended X-ray sources

DOEpatents

Bitter, Manfred L.; Fraenkel, Ben; Gorman, James L.; Hill, Kenneth W.; Roquemore, A. Lane; Stodiek, Wolfgang; von Goeler, Schweickhard E.

2001-01-01

Spherically or toroidally curved, double focusing crystals are used in a spectrometer for X-ray diagnostics of an extended X-ray source such as a hot plasma produced in a tokomak fusion experiment to provide spatially and temporally resolved data on plasma parameters using the imaging properties for Bragg angles near 45. For a Bragg angle of 45.degree., the spherical crystal focuses a bundle of near parallel X-rays (the cross section of which is determined by the cross section of the crystal) from the plasma to a point on a detector, with parallel rays inclined to the main plain of diffraction focused to different points on the detector. Thus, it is possible to radially image the plasma X-ray emission in different wavelengths simultaneously with a single crystal.

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

Sun, Cheng-Jun, E-mail: cjsun@aps.anl.gov; Brewe, Dale L.; Heald, Steve M.

X-ray diffraction (XRD) and X-ray absorption spectroscopy (XAS) are two main x-ray techniques in synchrotron radiation facilities. In this Note, we present an experimental setup capable of performing simultaneous XRD and XAS measurements by the application of a pixel-array area detector. For XRD, the momentum transfer in specular diffraction was measured by scanning the X-ray energy with fixed incoming and outgoing x-ray angles. By selecting a small fixed region of the detector to collect the XRD signal, the rest of the area was available for collecting the x-ray fluorescence for XAS measurements. The simultaneous measurement of XRD and X-ray absorptionmore » near edge structure for Pr{sub 0.67}Sr{sub 0.33}MnO{sub 3} film was demonstrated as a proof of principle for future time-resolved pump-probe measurements. A static sample makes it easy to maintain an accurate overlap of the X-ray spot and laser pump beam.« less

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

Sathyalakshmi, R.; Bhagavannarayana, G.; Ramasamy, P.

L-(+)-Glutamic acid hydro bromide, an isomorphic salt of L-glutamic acid hydrochloride, was synthesized and the synthesis was confirmed using Fourier transform infrared analysis. Solubility of the material in water was determined. L-Glutamic acid hydro bromide crystals were grown by low temperature solution growth using the solvent evaporation technique. Single crystal X-ray diffraction studies were carried out and the cell parameters, atomic co-ordinates, bond lengths and bond angles were reported. High-resolution X-ray diffraction studies were carried out and good crystallinity for the grown crystal was observed from the diffraction curve. The grown crystals were subjected to dielectric studies. Ultraviolet-visible-near infrared spectralmore » analysis shows good optical transmission in the visible and infrared region of the grown crystals. The second harmonic generation efficiency of L-glutamic acid hydro bromide crystal was determined using the Kurtz powder test and it was found that it had efficiency comparable with that of the potassium di-hydrogen phosphate crystal.« less

New software to model energy dispersive X-ray diffraction in polycrystalline materials

NASA Astrophysics Data System (ADS)

Ghammraoui, B.; Tabary, J.; Pouget, S.; Paulus, C.; Moulin, V.; Verger, L.; Duvauchelle, Ph.

2012-02-01

Detection of illicit materials, such as explosives or drugs, within mixed samples is a major issue, both for general security and as part of forensic analyses. In this paper, we describe a new code simulating energy dispersive X-ray diffraction patterns in polycrystalline materials. This program, SinFullscat, models diffraction of any object in any diffractometer system taking all physical phenomena, including amorphous background, into account. Many system parameters can be tuned: geometry, collimators (slit and cylindrical), sample properties, X-ray source and detector energy resolution. Good agreement between simulations and experimental data was obtained. Simulations using explosive materials indicated that parameters such as the diffraction angle or the energy resolution of the detector have a significant impact on the diffraction signature of the material inspected. This software will be a convenient tool to test many diffractometer configurations, providing information on the one that best restores the spectral diffraction signature of the materials of interest.

Time-resolved x-ray diffraction and calorimetric studies at low scan rates

PubMed Central

Yao, Haruhiko; Hatta, Ichiro; Koynova, Rumiana; Tenchov, Boris

1992-01-01

The phase transitions of dipalmitoylphosphatidylethanolamine (DPPE) in excess water have been examined by low-angle time-resolved x-ray diffraction and calorimetry at low scan rates. The lamellar subgel/lamellar liquid-crystalline (Lc → Lα), lamellar gel/lamellar liquid-crystalline (Lβ → Lα), and lamellar liquid-crystalline/lamellar gel (Lα → Lβ) phase transitions proceed via coexistence of the initial and final phases with no detectable intermediates at scan rates 0.1 and 0.5°C/min. At constant temperature within the region of the Lβ → Lα transition the ratio of the two coexisting phases was found to be stable for over 30 min. The state of stable phase coexistence was preceded by a 150-s relaxation taking place at constant temperature after termination of the heating scan in the transition region. While no intermediate structures were present in the coexistence region, a well reproducible multipeak pattern, with at least four prominent heat capacity peaks separated in temperature by 0.4-0.5°C, has been observed in the cooling transition (Lα → Lβ) by calorimetry. The multipeak pattern became distinct with an increase of incubation time in the liquid-crystalline phase. It was also clearly resolved in the x-ray diffraction intensity versus temperature plots recorded at slow cooling rates. These data suggest that the equilibrium state of the Lα phase of hydrated DPPE is represented by a mixture of domains that differ in thermal behavior, but cannot be distinguished structurally by x-ray scattering. Imagesp689-aFIGURE 9 PMID:19431820

Calculation of effective penetration depth in X-ray diffraction for pharmaceutical solids.

PubMed

Liu, Jodi; Saw, Robert E; Kiang, Y-H

2010-09-01

The use of the glancing incidence X-ray diffraction configuration to depth profile surface phase transformations is of interest to pharmaceutical scientists. The Parratt equation has been used to depth profile phase changes in pharmaceutical compacts. However, it was derived to calculate 1/e penetration at glancing incident angles slightly below the critical angle of condensed matter and is, therefore, applicable to surface studies of materials such as single crystalline nanorods and metal thin films. When the depth of interest is 50-200 microm into the surface, which is typical for pharmaceutical solids, the 1/e penetration depth, or skin depth, can be directly calculated from an exponential absorption law without utilizing the Parratt equation. In this work, we developed a more relevant method to define X-ray penetration depth based on the signal detection limits of the X-ray diffractometer. Our definition of effective penetration depth was empirically verified using bilayer compacts of varying known thicknesses of mannitol and lactose.

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.

Evaluation of the residual stresses in 95wt%Al2O3-5wt% SiC wear protection coating using X-Ray diffraction technique

NASA Astrophysics Data System (ADS)

Mahmoud, Adel K.; Hammoudi, Zaid S.; Student Samah Rasheed, M. Sc.

2018-02-01

This paper aims to measuring the residual stresses practically in wear protection coatings using the sin2ψ method according to X-ray diffraction technique. The wear protection coatings used in this study was composite coating 95wt% Al2O3-5wt% SiC, while bond coat was AlNi alloy produced by using flame spraying technique on the mild steel substrate. The diffraction angle, 2θ, is measured experimentally and then the lattice spacing is calculated from the diffraction angle, and the known X-ray wavelength using Bragg’s Law. Once the dspacing values are known, they can be plotted versus sin2ψ, (ψ is the tilt angle). In this paper, stress measurement of the samples that exhibit a linear behavior as in the case of a homogenous isotropic sample in a biaxial stress state is included. The plot of dspacing versus sin2ψ is a straight line which slope is proportional to stress. On the other hand, the second set of samples showed oscillatory dspacing versus sin2ψ behaviour. The oscillatory behaviour indicates the presence of inhomogeneous stress distribution. In this case the X-ray elastic constants must be used instead of Young’s modulus (E) and Poisson ratio (ν)values. These constants can be obtained from the literature for a given material and reflection combination. The value of the residual stresses for the present coating calculated was compressive stresses (-325.6758MPa).

Estimation of crystallinity in a model thermoplastic composite

NASA Technical Reports Server (NTRS)

Wakelyn, N. T.

1986-01-01

Crystallinities as low as 16 percent have been estimated by determination of the interplanar spacing on PET/carbonaceous filament composites with resin content of aobut 25 percent w/w using wide-angle X-ray scattering (WAXS) in the angular range 2 theta = 16-18 deg. The diffraction pattern of the carbonaceous reinforcements masks the major reflections of the resin, and the resin content and the crystallinity are kept low to make the simulation reasonable.

Large angle solid state position sensitive x-ray detector system

DOEpatents

Kurtz, David S.; Ruud, Clay O.

1998-01-01

A method and apparatus for x-ray measurement of certain properties of a solid material. In distinction to known methods and apparatus, this invention employs a specific fiber-optic bundle configuration, termed a reorganizer, itself known for other uses, for coherently transmitting visible light originating from the scintillation of diffracted x-radiation from the solid material gathered along a substantially one dimensional linear arc, to a two-dimensional photo-sensor array. The two-dimensional photodetector array, with its many closely packed light sensitive pixels, is employed to process the information contained in the diffracted radiation and present the information in the form of a conventional x-ray diffraction spectrum. By this arrangement, the angular range of the combined detector faces may be increased without loss of angular resolution. Further, the prohibitively expensive coupling together of a large number of individual linear diode photodetectors, which would be required to process signals generated by the diffracted radiation, is avoided.

X-Ray Amorphous Phases in Terrestrial Analog Volcanic Sediments: Implications for Amorphous Phases in Gale Crater, Mars

NASA Technical Reports Server (NTRS)

Smith, R. J.; Horgan, B.; Rampe, E.; Dehouck, E.; Morris, R. V.

2017-01-01

X-ray diffraction (XRD) amorphous phases have been found as major components (approx.15-60 wt%) of all rock and soil samples measured by the CheMin XRD instrument in Gale Crater, Mars. The nature of these phases is not well understood and could be any combination of primary (e.g., glass) and secondary (e.g., allophane) phases. Amorphous phases form in abundance during surface weathering on Earth. Yet, these materials are poorly characterized, and it is not certain how properties like composition and structure change with formation environment. The presence of poorly crystalline phases can be inferred from XRD patterns by the appearance of a low angle rise (< or approx.10deg 2(theta)) or broad peaks in the background at low to moderate 2(theta) angles (amorphous humps). CheMin mineral abundances combined with bulk chemical composition measurements from the Alpha Particle X-ray Spectrometer (APXS) have been used to estimate the abundance and composition of the XRD amorphous materials in soil and rock samples on Mars. Here we apply a similar approach to a diverse suite of terrestrial samples - modern soils, glacial sediments, and paleosols - in order to determine how formation environment, climate, and diagenesis affect the abundance and composition of X-ray amorphous phases.

Instrumentation on Multi-Scaled Scattering of Bio-Macromolecular Solutions

PubMed Central

Chu, Benjamin; Fang, Dufei; Mao, Yimin

2015-01-01

The design, construction and initial tests on a combined laser light scattering and synchrotron X-ray scattering instrument can cover studies of length scales from atomic sizes in Angstroms to microns and dynamics from microseconds to seconds are presented. In addition to static light scattering (SLS), dynamic light scattering (DLS), small angle X-ray scattering (SAXS) and wide angle X-ray diffraction (WAXD), the light scattering instrument is being developed to carry out studies in mildly turbid solutions, in the presence of multiple scattering. Three-dimensional photon cross correlation function (3D-PCCF) measurements have been introduced to couple with synchrotron X-ray scattering to study the structure, size and dynamics of macromolecules in solution. PMID:25946340

THz-pump and X-ray-probe sources based on an electron linac.

PubMed

Setiniyaz, Sadiq; Park, Seong Hee; Kim, Hyun Woo; Vinokurov, Nikolay A; Jang, Kyu-Ha; Lee, Kitae; Baek, In Hyung; Jeong, Young Uk

2017-11-01

We describe a compact THz-pump and X-ray-probe beamline, based on an electron linac, for ultrafast time-resolved diffraction applications. Two high-energy electron (γ > 50) bunches, 5 ns apart, impinge upon a single-foil or multifoil radiator and generate THz radiation and X-rays simultaneously. The THz pulse from the first bunch is synchronized to the X-ray beam of the second bunch by using an adjustable optical delay of a THz pulse. The peak power of THz radiation from the multifoil radiator is estimated to be 0.14 GW for a 200 pC well-optimized electron bunch. GEANT4 simulations show that a carbon foil with a thickness of 0.5-1.0 mm has the highest yield of 10-20 keV hard X-rays for a 25 MeV beam, which is approximately 10 3 photons/(keV pC-electrons) within a few degrees of the polar angle. A carbon multifoil radiator with 35 foils (25 μm thick each) can generate close to 10 3 hard X-rays/(keV pC-electrons) within a 2° acceptance angle. With 200 pC charge and a 100 Hz repetition rate, we can generate 10 7 X-rays per 1 keV energy bin per second or 10 5 X-rays per 1 keV energy bin per pulse. The longitudinal time profile of an X-ray pulse ranges from 400 to 600 fs depending on the acceptance angle. The broadening of the time duration of an X-ray pulse is observed owing to its diverging effect. A double-crystal monochromator will be used to select and transport the desired X-rays to the sample. The heating of the radiators by an electron beam is negligible because of the low beam current.

Coherent convergent-beam time-resolved X-ray diffraction

PubMed Central

Spence, John C. H.; Zatsepin, Nadia A.; Li, Chufeng

2014-01-01

The use of coherent X-ray lasers for structural biology allows the use of nanometre diameter X-ray beams with large beam divergence. Their application to the structure analysis of protein nanocrystals and single particles raises new challenges and opportunities. We discuss the form of these coherent convergent-beam (CCB) hard X-ray diffraction patterns and their potential use for time-resolved crystallography, normally achieved by Laue (polychromatic) diffraction, for which the monochromatic laser radiation of a free-electron X-ray laser is unsuitable. We discuss the possibility of obtaining single-shot, angle-integrated rocking curves from CCB patterns, and the dependence of the resulting patterns on the focused beam coordinate when the beam diameter is larger or smaller than a nanocrystal, or smaller than one unit cell. We show how structure factor phase information is provided at overlapping interfering orders and how a common phase origin between different shots may be obtained. Their use in refinement of the phase-sensitive intensity between overlapping orders is suggested. PMID:24914153

Hydrothermal formation of tobermorite studied by in situ X-ray diffraction under autoclave condition.

PubMed

Kikuma, Jun; Tsunashima, Masamichi; Ishikawa, Tetsuji; Matsuno, Shin-ya; Ogawa, Akihiro; Matsui, Kunio; Sato, Masugu

2009-09-01

Hydrothermal formation of tobermorite from a pre-cured cake has been investigated by transmission X-ray diffraction (XRD) using high-energy X-rays from a synchrotron radiation source in combination with a newly designed autoclave cell. The autoclave cell has a large and thin beryllium window for wide-angle X-ray diffraction; nevertheless, it withstands a steam pressure of more than 1.2 MPa, which enables in situ XRD measurements in a temperature range of 373 to 463 K under a saturated steam pressure. Formation and/or decomposition of several components has been successfully observed during 7.5 h of reaction time. From the intensity changes of the intermediate materials, namely non-crystalline C-S-H and hydroxylellestadite, two pathways for tobermorite formation have been confirmed. Thus, the newly developed autoclave cell can be used for the analyses of reaction mechanisms under specific atmospheres and temperatures.

X-Ray Diffraction Study of the Internal Structure of Supercooled Water

NASA Technical Reports Server (NTRS)

Dorsch, Robert G.; Boyd, Bemrose

1951-01-01

A Bragg X-ray spectrometer equipped with a volume-sensitive Geiger counter and Soller slits and employing filtered molybdenum Ka radiation was used to obtain a set of diffracted intensity curves as a Punction of angle for supercooled water. Diffracted intensity curves in the temperature region of 21 to -16 C were obtained. The minimum between the two main diffraction peaks deepened continuously with lowering temperature, indicating a gradual change in the internal structure of the water. No discontinuity in this trend was noted at the melting point. The internal structure of supercooled water was concluded to become progressively more ice-like as the temperature is lowered.

Crystallographic Determination of Molecular Parameters for K2SiF6: A Physical Chemistry Laboratory Experiment.

ERIC Educational Resources Information Center

Loehlin, James H.; Norton, Alexandra P.

1988-01-01

Describes a crystallography experiment using both diffraction-angle and diffraction-intensity information to determine the lattice constant and a lattice independent molecular parameter, while still employing standard X-ray powder diffraction techniques. Details the method, experimental details, and analysis for this activity. (CW)

Fluorescence X-ray absorption spectroscopy using a Ge pixel array detector: application to high-temperature superconducting thin-film single crystals.

PubMed

Oyanagi, H; Tsukada, A; Naito, M; Saini, N L; Lampert, M O; Gutknecht, D; Dressler, P; Ogawa, S; Kasai, K; Mohamed, S; Fukano, A

2006-07-01

A Ge pixel array detector with 100 segments was applied to fluorescence X-ray absorption spectroscopy, probing the local structure of high-temperature superconducting thin-film single crystals (100 nm in thickness). Independent monitoring of pixel signals allows real-time inspection of artifacts owing to substrate diffractions. By optimizing the grazing-incidence angle theta and adjusting the azimuthal angle phi, smooth extended X-ray absorption fine structure (EXAFS) oscillations were obtained for strained (La,Sr)2CuO4 thin-film single crystals grown by molecular beam epitaxy. The results of EXAFS data analysis show that the local structure (CuO6 octahedron) in (La,Sr)2CuO4 thin films grown on LaSrAlO4 and SrTiO3 substrates is uniaxially distorted changing the tetragonality by approximately 5 x 10(-3) in accordance with the crystallographic lattice mismatch. It is demonstrated that the local structure of thin-film single crystals can be probed with high accuracy at low temperature without interference from substrates.

The structural properties of flower-like ZnO nanostructures on porous silicon

NASA Astrophysics Data System (ADS)

Eswar, Kevin Alvin; Suhaimi, Mohd Husairi Fadzillah; Guliling, Muliyadi; Mohamad, Maryam; Khusaimi, Zuraida; Rusop, M.; Abdullah, Saifollah

2018-05-01

The flower-like zinc oxide (ZnO) were successfully synthesized on porous silicon (PSi) via hydrothermal method. The characteristic of ZnO nanostructures was investigated using field emission scanning microscopy (FESEM) and X-ray diffraction (X-Ray). The FESEM images show the flower-like ZnO nanostructures composed ZnO nanoparticles. The X-ray diffraction shows that strong intensity of (100), (002) and (101) peaks. The structural analysis revealed that the peaks angles were shifted due to the stress or imperfection of the crystalline of ZnO nanostructures. The crystalline sizes in range of 42.60 to 54.09 nm were produced.

Serial femtosecond X-ray diffraction of enveloped virus microcrystals

DOE PAGES

Lawrence, Robert M.; Conrad, Chelsie E.; Zatsepin, Nadia A.; ...

2015-08-20

Serial femtosecond crystallography (SFX) using X-ray free-electron lasers has produced high-resolution, room temperature, time-resolved protein structures. We report preliminary SFX of Sindbis virus, an enveloped icosahedral RNA virus with ~700 Å diameter. Microcrystals delivered in viscous agarose medium diffracted to ~40 Å resolution. Small-angle diffuse X-ray scattering overlaid Bragg peaks and analysis suggests this results from molecular transforms of individual particles. Viral proteins undergo structural changes during entry and infection, which could, in principle, be studied with SFX. This is a pertinent step toward determining room temperature structures from virus microcrystals that may enable time-resolved studies of enveloped viruses.

Remote analysis of planetary soils: X-ray diffractometer development

NASA Technical Reports Server (NTRS)

Gregory, J. C.

1973-01-01

A system is described suitable for remote low power mineralogical analysis of lunar, planetary, or asteroid soils. It includes an X-ray diffractometer, fluorescence spectrometer, and sample preparation system. A one Curie Fe-55 source provides a monochromatic X-ray beam of 5.9 keV. Seeman-Bohlin or focusing geometry is employed in the camera, allowing peak detection to proceed simultaneously at all angles and obviating the need for moving parts. The detector system is an array of 500-600 proportional counters with a wire-spacing of 1 mm. An electronics unit comprising preamplifier, postamplifier, window discriminators, and storage flipflops requiring only 3.5 milliwatts was designed and tested. Total instrument power is less than 5 watts. Powder diffraction patterns using a flat breadboard multiwire counter were recorded.

Unified structure theory of icosahedral quasicrystals: Evidence from neutron powder diffraction patterns that AlCrFeMnSi, AlCuLiMg, and TiNiFeSi icosahedral quasicrystals are twins of cubic crystals containing about 820 or 1012 atoms in a primitive unit cube

PubMed Central

Pauling, Linus

1988-01-01

A unified structure theory of icosahedral quasicrystals, combining the twinned-cubic-crystal theory and the Penrose-tiling-six-dimensional-projection theory, is described. Values of the primitive-cubic lattice constant for several quasicrystals are evaluated from x-ray and neutron diffraction data. The fact that the low-angle diffraction maxima can be indexed with cubic unit cells provides additional support for the twinned-cubic-crystal theory of icosahedral quasicrystals. PMID:16593990

Borman effect in resonant diffraction of X-rays

NASA Astrophysics Data System (ADS)

Oreshko, A. P.

2013-08-01

A dynamic theory of resonant diffraction (occurring when the energy of incident radiation is close to the energy of the absorption edge of an element in the composition of a given substance) of synchronous X-rays is developed in the two-wave approximation in the coplanar Laue geometry for large grazing angles in perfect crystals. A sharp decrease in the absorption coefficient in the substance with simultaneously satisfied diffraction conditions (Borman effect) is demonstrated, and the theoretical and first experimental results are compared. The calculations reveal the possibility of applying this approach in analyzing the quadrupole-quadrupole contribution to the absorption coefficient.

A graphite crystal polarimeter for stellar X-ray astronomy.

NASA Technical Reports Server (NTRS)

Weisskopf, M. C.; Berthelsdorf, R.; Epstein, G.; Linke, R.; Mitchell, D.; Novick, R.; Wolff, R. S.

1972-01-01

The first crystal X-ray polarimeter to be used for X-ray astronomy is described. Polarization is measured by modulation of the X rays diffracted at an average 45 deg glancing angle from large, curved graphite crystal panels as these rotate about an axis parallel to the incident X-ray flux. Arrangement of the crystal panels, the design of the detector, and the signal-processing circuitry were optimized to minimize systematic effects produced by off-axis pointing of the rocket and cosmic ray induced events. The in-flight performance of the instrument in relation to the observed background signal is discussed.

[Study of selegiline and related compounds with x-ray diffraction].

PubMed

Simon, K; Böcskei, Z; Török, Z

1992-09-01

Selegiline and its parent compounds were studied by X-ray diffraction. It was established that the racemates of primary and secondary amines (p-fluoro-amphetamine, methamphetamine, p-fluoro-methamphetamine) hydrochloride do not form racemic compounds but crystalline as conglomerates, at the same time tertiary amines like selegiline and p-fluoro-selegiline hydrochlorides do. The crystalline structure of five enantiomeric hydrochlorides were determined, the CPhe-C-C-N torsion angle is anti-periplanar in all cases but in p-fluoro-amphetamine where it is gauche.

Local texture and strongly linked conduction in spray-pyrolyzed TlBa2Ca2Cu3O(8+x) deposits

NASA Astrophysics Data System (ADS)

Kroeger, D. M.; Goyal, A.; Specht, E. D.; Wang, Z. L.; Tkaczyk, J. E.; Sutliff, J. A.; Deluca, J. A.

Local texture in polycrystalline TlBa2Ca2 Cu3O(8+x) deposits has been determined from transmission electron microscopy, electron backscatter diffraction patterns and x-ray diffraction. The small-grained deposits had excellent c-axis alignment and contained colonies of grains with similar but not identical a-axis orientations. Most grain boundaries within a colony have small misorientation angles and should not be weak links. It is proposed that long range conduction utilizes a percolative network of small angle grain boundaries at colony intersections.

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

Determining and Controlling the Magnesium Composition in CdTe/CdMgTe Heterostructures

DOE PAGES

LeBlanc, E. G.; Edirisooriya, M.; Ogedengbe, O. S.; ...

2017-06-05

The relationships between Mg composition, band gap, and lattice characteristics are investigated for Cd 1-xMg xTe barrier layers using a combination of cathodoluminescence, energy dispersive x-ray spectroscopy, variable angle spectral ellipsometry, and atom probe tomography. The use of a simplified, yet accurate, variable angle spectral ellipsometry analysis is shown to be appropriate for fast determination of composition in thin Cd 1-xMg xTe layers. The validity of using high-resolution x-ray diffraction for CdTe/Cd 1-xMg xTe double heterostructures is discussed. Furthermore, the stability of CdTe/Cd 1-xMg xTe heterostructures are investigated with respect to thermal processing.

Determining and Controlling the Magnesium Composition in CdTe/CdMgTe Heterostructures

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

LeBlanc, E. G.; Edirisooriya, M.; Ogedengbe, O. S.

The relationships between Mg composition, band gap, and lattice characteristics are investigated for Cd 1-xMg xTe barrier layers using a combination of cathodoluminescence, energy dispersive x-ray spectroscopy, variable angle spectral ellipsometry, and atom probe tomography. The use of a simplified, yet accurate, variable angle spectral ellipsometry analysis is shown to be appropriate for fast determination of composition in thin Cd 1-xMg xTe layers. The validity of using high-resolution x-ray diffraction for CdTe/Cd 1-xMg xTe double heterostructures is discussed. Furthermore, the stability of CdTe/Cd 1-xMg xTe heterostructures are investigated with respect to thermal processing.

Synchrotron X-ray reciprocal-space mapping, topography and diffraction resolution studies of macromolecular crystal quality.

PubMed

Boggon, T J; Helliwell, J R; Judge, R A; Olczak, A; Siddons, D P; Snell, E H; Stojanoff, V

2000-07-01

A comprehensive study of microgravity and ground-grown chicken egg-white lysozyme crystals is presented using synchrotron X-ray reciprocal-space mapping, topography techniques and diffraction resolution. Microgravity crystals displayed reduced intrinsic mosaicities on average, but no differences in terms of strain over their ground-grown counterparts. Topographic analysis revealed that in the microgravity case the majority of the crystal was contributing to the peak of the reflection at the appropriate Bragg angle. In the ground-control case only a small volume of the crystal contributed to the intensity at the diffraction peak. The techniques prove to be highly complementary, with the reciprocal-space mapping providing a quantitative measure of the crystal mosaicity and strain (or variation in lattice spacing) and the topography providing a qualitative overall assessment of the crystal in terms of its X-ray diffraction properties. Structural data collection was also carried out at the synchrotron.

Synchrotron X-Ray Reciprocal Space Mapping, Topography and Diffraction Resolution Studies of Macromolecular Crystal Quality

NASA Technical Reports Server (NTRS)

Boggon, T. J.; Helliwell, J. R.; Judge, Russell A.; Siddons, D. P.; Snell, Edward H.; Stojanoff, V.

2000-01-01

A comprehensive study of microgravity and ground grown chicken egg white lysozyme crystals is presented using synchrotron X-ray reciprocal space mapping, topography techniques and diffraction resolution. Microgravity crystals displayed, on average, reduced intrinsic mosaicities but no differences in terms of stress over their earth grown counterparts. Topographic analysis revealed that in the microgravity case the majority of the crystal was contributing to the peak of the reflection at the appropriate Bragg angle. In the earth case at the diffraction peak only a small volume of the crystal contributed to the intensity. The techniques prove to be highly complementary with the reciprocal space mapping providing a quantitative measure of the crystal mosaicity and stress (or variation in lattice spacing) and topography providing a qualitative overall assessment of the crystal in terms of its X-ray diffraction properties. Structural data collection was also carried out both at the synchrotron and in the laboratory.

Local texture and grain boundary misorientations in high H(C) oxide superconductors

NASA Astrophysics Data System (ADS)

Kroeger, D. M.; Goyal, A.; Specht, E. D.; Tkaczyk, J. E.; Sutliff, J.; Deluca, J. A.; Wang, Z. L.; Riley, G. N., Jr.

The orientations of hundreds of contiguous grains in high J(C) TlBa2Ca2Cu3O(x) deposits and (Bi, Pb)2 Sr2Ca2Cu3O(y) powder-in-tube tapes have been determined from electron back scatter diffraction patterns (EBSP). The misorientation angles and axes of rotation (angle/axis pairs) for grain boundaries connecting these grains were calculated. For both materials the population of low angle boundaries was found to be much larger than expected from calculations based on the macroscopic texture. The TlBa2Ca2Cu3O(x) deposits exhibit pronounced local texture which has been defined by EBSP and x-ray diffraction. Locally grains show significant in-plane (a-axis) alignment even though macroscopically a-axes are random, indicating the presence of colonies of grains with similar a-axis orientations. In (Bi, Pb)2 Sr2Ca2Cu3O(x) tapes no local texture was observed. In both materials the existence of connected networks of small angle grain boundaries can be inferred. Coincident site lattice (CSL) grain boundaries are also present in higher than expected numbers. Grain boundary energy thus appears to play a significant role in enhancing the population of potentially strongly-linked boundaries. We propose that long range strongly-linked conduction occurs through a percolative network small angle (and perhaps CSL) grain boundaries.

Measurement of strain in Al-Cu interconnect lines with x-ray microdiffraction

NASA Astrophysics Data System (ADS)

Solak, H. H.; Vladimirsky, Y.; Cerrina, F.; Lai, B.; Yun, W.; Cai, Z.; Ilinski, P.; Legnini, D.; Rodrigues, W.

1999-07-01

We report measurement of strain in patterned Al-Cu interconnect lines with x-ray microdiffraction technique with a ˜1 μm spatial resolution. Monochromatized x rays from an undulator were focused on the sample using a phase fresnel zone plate and diffracted light was collected by an area detector in a symmetric, angle dispersive x-ray diffraction geometry. Measurements were made before and after the line sample was stressed for electromigration. Results show an increase in inter- and intra-grain strain variation after the testing. Differences in strain behavior of grains with (111) and (200) crystallographic planes parallel to the substrate surface were observed. A position dependent variation of strain after the testing was measured whereas no such dependence was found before the testing.

Complexation and Structure Elucidation of the Axial Conformers of Mono- and (±)-trans-1,2-Disubstituted Cyclohexanes by Enantiopure Alleno-Acetylenic Cage Receptors.

PubMed

Gropp, Cornelius; Trapp, Nils

2018-04-25

Single crystal X-ray diffraction is a powerful method to unambiguously characterize the structure of molecules with atomic resolution. Herein, we review the molecular recognition of the (di)axial conformers of Mono- and (±)-trans-1,2-disubstituted cyclohexanes by enantiopure alleno-acetylenic cage receptors in solution and in the solid state. Single crystals of the host-guest complexes suitable for X-ray diffraction allow for the first time to study the dihedral angles of a series of Mono- and (±)-trans-1,2-disubstituted cyclohexanes in their (di)axial chair conformation. Theoretical studies indicate negligible influence of the host structure on the guest conformation, suggesting that the structural information obtained from the host-guest complexes give insight into the innate structures of Mono- and (±)-trans-1,2-disubstituted cyclohexanes. Strong deviation of the dihedral angles a,a(X-C(1)-C(2)-X) from the idealized 180° are observed, accompanied by substantial flattening of the ring dihedral angles ρ(X-C(1)-C(2)-C(3)).

Large angle solid state position sensitive x-ray detector system

DOEpatents

Kurtz, D.S.; Ruud, C.O.

1998-03-03

A method and apparatus for x-ray measurement of certain properties of a solid material are disclosed. In distinction to known methods and apparatus, this invention employs a specific fiber-optic bundle configuration, termed a reorganizer, itself known for other uses, for coherently transmitting visible light originating from the scintillation of diffracted x-radiation from the solid material gathered along a substantially one dimensional linear arc, to a two-dimensional photo-sensor array. The two-dimensional photodetector array, with its many closely packed light sensitive pixels, is employed to process the information contained in the diffracted radiation and present the information in the form of a conventional x-ray diffraction spectrum. By this arrangement, the angular range of the combined detector faces may be increased without loss of angular resolution. Further, the prohibitively expensive coupling together of a large number of individual linear diode photodetectors, which would be required to process signals generated by the diffracted radiation, is avoided. 7 figs.

Large angle solid state position sensitive x-ray detector system

DOEpatents

Kurtz, D.S.; Ruud, C.O.

1998-07-21

A method and apparatus are disclosed for x-ray measurement of certain properties of a solid material. In distinction to known methods and apparatus, this invention employs a specific fiber-optic bundle configuration, termed a reorganizer, itself known for other uses, for coherently transmitting visible light originating from the scintillation of diffracted x-radiation from the solid material gathered along a substantially one dimensional linear arc, to a two-dimensional photo-sensor array. The two-dimensional photodetector array, with its many closely packed light sensitive pixels, is employed to process the information contained in the diffracted radiation and present the information in the form of a conventional x-ray diffraction spectrum. By this arrangement, the angular range of the combined detector faces may be increased without loss of angular resolution. Further, the prohibitively expensive coupling together of a large number of individual linear diode photodetectors, which would be required to process signals generated by the diffracted radiation, is avoided. 7 figs.

Grating-based holographic diffraction methods for X-rays and neutrons: phase object approximation and dynamical theory

DOE PAGES

Feng, Hao; Ashkar, Rana; Steinke, Nina; ...

2018-02-01

A method dubbed grating-based holography was recently used to determine the structure of colloidal fluids in the rectangular grooves of a diffraction grating from X-ray scattering measurements. Similar grating-based measurements have also been recently made with neutrons using a technique called spin-echo small-angle neutron scattering. The analysis of the X-ray diffraction data was done using an approximation that treats the X-ray phase change caused by the colloidal structure as a small perturbation to the overall phase pattern generated by the grating. In this paper, the adequacy of this weak phase approximation is explored for both X-ray and neutron grating holography.more » Additionally, it is found that there are several approximations hidden within the weak phase approximation that can lead to incorrect conclusions from experiments. In particular, the phase contrast for the empty grating is a critical parameter. Finally, while the approximation is found to be perfectly adequate for X-ray grating holography experiments performed to date, it cannot be applied to similar neutron experiments because the latter technique requires much deeper grating channels.« less

Effective increase in beam emittance by phase-space expansion using asymmetric Bragg diffraction.

PubMed

Chu, Chia-Hung; Tang, Mau-Tsu; Chang, Shih-Lin

2015-08-24

We propose an innovative method to extend the utilization of the phase space downstream of a synchrotron light source for X-ray transmission microscopy. Based on the dynamical theory of X-ray diffraction, asymmetrically cut perfect crystals are applied to reshape the position-angle-wavelength space of the light source, by which the usable phase space of the source can be magnified by over one hundred times, thereby "phase-space-matching" the source with the objective lens of the microscope. The method's validity is confirmed using SHADOW code simulations, and aberration through an optical lens such as a Fresnel zone plate is examined via matrix optics for nano-resolution X-ray images.

Transmission-geometry electrochemical cell for in-situ scattering and spectroscopy investigations

DOEpatents

Chupas, Peter J.; Chapman, Karena W.; Kurtz, Charles A.; Borkiewicz, Olaf J.; Wiaderek, Kamila Magdelena; Shyam, Badri

2015-05-05

The present invention relates to a test chamber that can be used to perform a variety of X-ray and neutron spectroscopy experiments including powder diffraction, small-angle scattering, X-ray absorption spectroscopy, and pair distribution functions, such chamber comprising a first electrode with an X-ray transparent window; a second electrode with an X-ray transparent window; a plurality of insulating gaskets providing a hermetic seal around the sample and preventing contact between said first and second electrodes; and an insulating housing into which the first electrode is secured.

X-ray diffraction patterns and diffracted intensity of Kα spectral lines of He-like ions

NASA Astrophysics Data System (ADS)

Goyal, Arun; Khatri, Indu; Singh, A. K.; Sharma, Rinku; Mohan, Man

2017-09-01

In the present paper, we have calculated fine-structure energy levels related to the configurations 1s2s, 1s2p, 1s3s and 1s3p by employing GRASP2K code. We have also computed radiative data for transitions from 1s2p 1 P1o, 1s2p 3 P2o, 1s2p 3 P1o and 1s2s 3S1 to the ground state 1s2. We have made comparisons of our presented energy levels and transition wavelengths with available results compiled by NIST and good agreement is achieved. We have also provided X-ray diffraction (XRD) patterns of Kα spectral lines, namely w, x, y and z of Cu XXVIII, Kr XXXV and Mo with diffraction angle and maximum diffracted intensity which is not published elsewhere in the literature. We believe that our presented results may be beneficial in determination of the order parameter, X-ray crystallography, solid-state drug analysis, forensic science, geological and medical applications.

Diffraction properties of multilayer Laue lenses with an aperture of 102 µm and WSi 2/Al bilayers

DOE PAGES

Kubec, Adam; Kujala, Naresh; Conley, Raymond; ...

2015-01-01

Here, we report on the characterization of a multilayer Laue lens (MLL) with large acceptance, made of a novel WSi2/Al bilayer system. Fabrication of multilayers with large deposition thickness is required to obtain MLL structures with sufficient apertures capable of accepting the full lateral coherence length of x-rays at typical nanofocusing beamlines. To date, the total deposition thickness has been limited by stress-buildup in the multilayer. We were able to grow WSi2/Al with low grown-in stress, and asses the degree of stress reduction. X-ray diffraction experiments were conducted at beamline 1-BM at the Advanced Photon Source. We used monochromatic x-raysmore » with a photon energy of 12 keV and a bandwidth of ΔE/E=5.4 ∙ 10 -4. The MLL was grown with parallel layer interfaces, and was designed to have a large focal length of 9.6 mm. The mounted lens was 2.7 mm in width. We found and quantified kinks and bending of sections of the MLL. Sections with bending were found to partly have a systematic progression in the interface angles. We also observed kinking in some, but not all, areas. The measurements are compared with dynamic diffraction calculations made with Coupled Wave Theory. Finally our data are plotted showing the diffraction efficiency as a function of the external tilting angle of the entire mounted lens. This way of plotting the data was found to provide an overview into the diffraction properties of the whole lens, and enabled the following layer tilt analyses.« less

X-ray Interferometry with Transmissive Beam Combiners for Ultra-High Angular Resolution Astronomy

NASA Technical Reports Server (NTRS)

Skinner, G. K.; Krismanic, John F.

2009-01-01

Abstract Interferometry provides one of the possible routes to ultra-high angular resolution for X-ray and gamma-ray astronomy. Sub-micro-arc-second angular resolution, necessary to achieve objectives such as imaging the regions around the event horizon of a super-massive black hole at the center of an active galaxy, can be achieved if beams from parts of the incoming wavefront separated by 100s of meters can be stably and accurately brought together at small angles. One way of achieving this is by using grazing incidence mirrors. We here investigate an alternative approach in which the beams are recombined by optical elements working in transmission. It is shown that the use of diffractive elements is a particularly attractive option. We report experimental results from a simple 2-beam interferometer using a low-cost commercially available profiled film as the diffractive elements. A rotationally symmetric filled (or mostly filled) aperture variant of such an interferometer, equivalent to an X-ray axicon, is shown to offer a much wider bandpass than either a Phase Fresnel Lens (PFL) or a PFL with a refractive lens in an achromatic pair. Simulations of an example system are presented.

Relations for lipid bilayers. Connection of electron density profiles to other structural quantities.

PubMed Central

Nagle, J F; Wiener, M C

1989-01-01

Three relations are derived that connect low angle diffraction/scattering results obtained from lipid bilayers to other structural quantities of interest. The first relates the area along the surface of the bilayer, the measured specific volume, and the zeroth order structure factor, F(0). The second relates the size of the trough in the center of the electron density profile, the volume of the terminal methyl groups, and the volume of the methylene groups in the fatty acid chains. The third relates the size of the headgroup electron density peak, the volume of the headgroup, and the volumes of water and hydrocarbon in the headgroup region. These relations, which are easily modified for neutron diffraction, are useful for obtaining structural quantities from electron density profiles obtained by fitting model profiles to measured low angle x-ray intensities. PMID:2713444

Analysis of energy dispersive x-ray diffraction profiles for material identification, imaging and system control

NASA Astrophysics Data System (ADS)

Cook, Emily Jane

2008-12-01

This thesis presents the analysis of low angle X-ray scatter measurements taken with an energy dispersive system for substance identification, imaging and system control. Diffraction measurements were made on illicit drugs, which have pseudo- crystalline structures and thus produce diffraction patterns comprising a se ries of sharp peaks. Though the diffraction profiles of each drug are visually characteristic, automated detection systems require a substance identification algorithm, and multivariate analysis was selected as suitable. The software was trained with measured diffraction data from 60 samples covering 7 illicit drugs and 5 common cutting agents, collected with a range of statistical qual ities and used to predict the content of 7 unknown samples. In all cases the constituents were identified correctly and the contents predicted to within 15%. Soft tissues exhibit broad peaks in their diffraction patterns. Diffraction data were collected from formalin fixed breast tissue samples and used to gen erate images. Maximum contrast between healthy and suspicious regions was achieved using momentum transfer windows 1.04-1.10 and 1.84-1.90 nm_1. The resulting images had an average contrast of 24.6% and 38.9% compared to the corresponding transmission X-ray images (18.3%). The data was used to simulate the feedback for an adaptive imaging system and the ratio of the aforementioned momentum transfer regions found to be an excellent pa rameter. Investigation into the effects of formalin fixation on human breast tissue and animal tissue equivalents indicated that fixation in standard 10% buffered formalin does not alter the diffraction profiles of tissue in the mo mentum transfer regions examined, though 100% unbuffered formalin affects the profile of porcine muscle tissue (a substitute for glandular and tumourous tissue), though fat is unaffected.

Growth, crystalline perfection, spectral, thermal and theoretical studies on imidazolium L-tartrate crystals.

PubMed

Meena, K; Muthu, K; Meenatchi, V; Rajasekar, M; Bhagavannarayana, G; Meenakshisundaram, S P

2014-04-24

Transparent optical quality single crystals of imidazolium L-tartrate (IMLT) were grown by conventional slow evaporation solution growth technique. Crystal structure of the as-grown IMLT was determined by single crystal X-ray diffraction analysis. Thermal analysis reveals the purity of the crystal and the sample is stable up to the melting point. Good transmittance in the visible region is observed and the band gap energy is estimated using diffuse reflectance data by the application of Kubelka-Munk algorithm. The powder X-ray diffraction study reveals the crystallinity of the as-grown crystal and it is compared with that of the experimental one. An additional peak in high resolution X-ray diffraction (HRXRD) indicates the presence of an internal structural low angle boundary. Second harmonic generation (SHG) activity of IMLT is significant as estimated by Kurtz and Perry powder technique. HOMO-LUMO energies and first-order molecular hyperpolarizability of IMLT have been evaluated using density functional theory (DFT) employing B3LYP functional and 6-31G(d,p) basis set. The optimized geometry closely resembles the ORTEP. The vibrational patterns present in the molecule are confirmed by FT-IR coinciding with theoretical patterns. Copyright © 2014 Elsevier B.V. All rights reserved.

Ambiguities and completeness of SAS data analysis: investigations of apoferritin by SAXS/SANS EID and SEC-SAXS methods

NASA Astrophysics Data System (ADS)

Zabelskii, D. V.; Vlasov, A. V.; Ryzhykau, Yu L.; Murugova, T. N.; Brennich, M.; Soloviov, D. V.; Ivankov, O. I.; Borshchevskiy, V. I.; Mishin, A. V.; Rogachev, A. V.; Round, A.; Dencher, N. A.; Büldt, G.; Gordeliy, V. I.; Kuklin, A. I.

2018-03-01

The method of small angle scattering (SAS) is widely used in the field of biophysical research of proteins in aqueous solutions. Obtaining low-resolution structure of proteins is still a highly valuable method despite the advances in high-resolution methods such as X-ray diffraction, cryo-EM etc. SAS offers the unique possibility to obtain structural information under conditions close to those of functional assays, i.e. in solution, without different additives, in the mg/mL concentration range. SAS method has a long history, but there are still many uncertainties related to data treatment. We compared 1D SAS profiles of apoferritin obtained by X-ray diffraction (XRD) and SAS methods. It is shown that SAS curves for X-ray diffraction crystallographic structure of apoferritin differ more significantly than it might be expected due to the resolution of the SAS instrument. Extrapolation to infinite dilution (EID) method does not sufficiently exclude dimerization and oligomerization effects and therefore could not guarantee total absence of dimers account in the final SAS curve. In this study, we show that EID SAXS, EID SANS and SEC-SAXS methods give complementary results and when they are used all together, it allows obtaining the most accurate results and high confidence from SAS data analysis of proteins.

Refraction effects in soft x-ray multilayer blazed gratings.

PubMed

Voronov, D L; Salmassi, F; Meyer-Ilse, J; Gullikson, E M; Warwick, T; Padmore, H A

2016-05-30

A 2500 lines/mm Multilayer Blazed Grating (MBG) optimized for the soft x-ray wavelength range was fabricated and tested. The grating coated with a W/B₄C multilayer demonstrated a record diffraction efficiency in the 2nd blazed diffraction order in the energy range from 500 to 1200 eV. Detailed investigation of the diffraction properties of the grating demonstrated that the diffraction efficiency of high groove density MBGs is not limited by the normal shadowing effects that limits grazing incidence x-ray grating performance. Refraction effects inherent in asymmetrical Bragg diffraction were experimentally confirmed for MBGs. The refraction affects the blazing properties of the MBGs and results in a shift of the resonance wavelength of the gratings and broadening or narrowing of the grating bandwidth depending on diffraction geometry. The true blaze angle of the MBGs is defined by both the real structure of the multilayer stack and by asymmetrical refraction effects. Refraction effects can be used as a powerful tool in providing highly efficient suppression of high order harmonics.

Effect of borax concentration on the structure of Poly(Vinyl Alcohol) gels

NASA Astrophysics Data System (ADS)

Lawrence, Mathias B.; Desa, J. A. E.; Aswal, V. K.

2012-06-01

Poly(Vinyl Alcohol) hydrogels cross-linked with varying concentrations of borax have been studied using Small-Angle Neutron Scattering and X-Ray Diffraction. The intensity of scattering increases with borax concentration from 1 mg/ml up to 2 mg/ml and falls thereafter for 4 mg/ml, increasing again for a concentration of 10 mg/ml. The mesoscopic structural changes that cause these trends in the SANS data are in keeping with the variations in the X-ray diffraction patterns pertaining to structures within the PVA chains.

The Effects of Stoichiometry on the Mechanical Properties of Icosahedral Boron Carbide Under Loading

DTIC Science & Technology

2012-11-19

ranging from 10% to 20% C using glancing incidence x - ray diffraction and similar experimental studies of structure as a function of stoichiometry were...blue) positions. it has been suggested that x - ray diffraction analysis of a series of boron-rich materials indicates a distinct change in the c lattice...Angstroms, angles in degrees, volume in cubic Angstroms). Structure Formula % C a b c α β γ Volume Experiment37 B5.6C 15.2 5.19 5.19 5.19 65.18 65.18

Purification, crystallization, small-angle X-ray scattering and preliminary X-ray diffraction analysis of the SH2 domain of the Csk-homologous kinase.

PubMed

Gunn, Natalie J; Gorman, Michael A; Dobson, Renwick C J; Parker, Michael W; Mulhern, Terrence D

2011-03-01

The C-terminal Src kinase (Csk) and Csk-homologous kinase (CHK) are endogenous inhibitors of the proto-oncogenic Src family of protein tyrosine kinases (SFKs). Phosphotyrosyl peptide binding to their Src-homology 2 (SH2) domains activates Csk and CHK, enhancing their ability to suppress SFK signalling; however, the detailed mechanistic basis of this activation event is unclear. The CHK SH2 was expressed in Escherichia coli and the purified protein was characterized as monomeric by synchrotron small-angle X-ray scattering in-line with size-exclusion chromatography. The CHK SH2 crystallized in 0.2 M sodium bromide, 0.1 M bis-Tris propane pH 6.5 and 20% polyethylene glycol 3350 and the best crystals diffracted to ∼1.6 Å resolution. The crystals belonged to space group P2, with unit-cell parameters a=25.8, b=34.6, c=63.2 Å, β=99.4°.

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.

New insights into microstructural evolution of epitaxial Ni-Mn-Ga films on MgO (1 0 0) substrate by high-resolution X-ray diffraction and orientation imaging investigations

NASA Astrophysics Data System (ADS)

Sharma, Amit; Mohan, Sangeneni; Suwas, Satyam

2018-04-01

In this work, a detailed investigation has been performed on hetero-epitaxial growth and microstructural evolution in highly oriented Ni-Mn-Ga (1 0 0) films grown on MgO (1 0 0) substrate using high-resolution X-ray diffraction and orientation imaging microscopy. Mosaicity of the films has been analysed in terms of tilt angle, twist angle, lateral and vertical coherence length and threading dislocation densities by performing rocking curve measurements and reciprocal space mapping. Density of edge dislocations is found to be an order of magnitude higher than the density of screw dislocations, irrespective of film thickness. X-ray pole figure measurements have revealed an orientation relationship of ? || (1 0 0)MgO; ? || [0 0 1]MgO between the film and substrate. Microstructure predicted by X-ray diffraction is in agreement with that obtained from electron microscopy and atomic force microscopy. The evolution of microstructure in the film with increasing thickness has been explained vis-à-vis dislocation generation and growth mechanisms. Orientation imaging microscopy observations indicate evolutionary growth of film by overgrowth mechanism. Decrease in coercivity with film thickness has been explained as an interplay between stress field developed due to crystal defects and magnetic domain pinning due to surface roughness.

Probing multi-scale mechanical damage in connective tissues using X-ray diffraction.

PubMed

Bianchi, Fabio; Hofmann, Felix; Smith, Andrew J; Thompson, Mark S

2016-11-01

The accumulation of microstructural collagen damage following repetitive loading is linked to painful and debilitating tendon injuries. As a hierarchical, semi-crystalline material, collagen mechanics can be studied using X-ray diffraction. The aim of the study was to describe multi-structural changes in tendon collagen following controlled plastic damage (5% permanent strain). We used small angle X-ray scattering (SAXS) to interrogate the spacing of collagen molecules within a fibril, and wide angle X-ray scattering (WAXS) to measure molecular strains under macroscopic loading. Simultaneous recordings of SAXS and WAXS patterns, together with whole-tissue strain in physiologically hydrated rat-tail tendons were made during increments of in situ tensile loading. Results showed that while tissue level modulus was unchanged, fibril modulus decreased significantly, and molecular modulus significantly increased. Further, analysis of higher order SAXS peaks suggested structural changes in the gap and overlap regions, possibly localising the damage to molecular cross-links. Our results provide new insight into the fundamental damage processes at work in collagenous tissues and point to new directions for their mitigation and repair. This article reports the first in situ loading synchrotron studies on mechanical damage in collagenous tissues. We provide new insight into the nano- and micro-structural mechanisms of damage processes. Pre-damaged tendons showed differential alteration of moduli at macro, micro and nano-scales as measured using X-ray scattering techniques. Detailed analysis of higher order diffraction peaks suggested damage is localised to molecular cross-links. The results are consistent with previous X-ray scattering studies of tendons and also with recent thermal stability studies on damaged material. Detailed understanding of damage mechanisms is essential in the development of new therapies promoting tissue repair. Copyright © 2016 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Shear induced weakening of the hydrogen bonding lattice of the energetic material 5,5'-Hydrazinebistetrazole at high-pressure

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

Ciezak-Jenkins, Jennifer A.; Jenkins, Timothy A.

5,5'-Hydrazinebistetrazole (HBTA) has been studied by in-situ x-ray diffraction and vibrational spectroscopy to pressures near 25 GPa at room temperature. Analysis of the x-ray diffraction pattern of HBTA collected at ambient pressure and temperature revealed a monoclinic structure consistent with that previously reported. Under compression, the x-ray diffraction reveals little evidence of a phase transition over the pressure range studied. Slight anisotropy in response to compression was noted and the β angle decreased moderately, suggesting geometry modifications occur in the hydrogen bonding lattice and between neighboring HBTA molecules as a result of compression along the c axis. Blue shifts inmore » the Infrared active N-H stretching modes were observed, implying a weakening of the hydrogen bond with compression. The weakening of the hydrogen bonding lattice with pressure may lead to an increase in the bending angle of the C-N=N-C bridge between the tetrazole rings and an increased overlap between the π-bonding orbitals. The Raman spectra showed a number of modes associated with H-N=N-H motions of the bridge become more prominent in the spectra under compression. Additionally, the possibility that the increased bend in the angle of the C-N=N-C bridge results from a shearing deformation is discussed.« less

Development of low temperature and high magnetic field X-ray diffraction facility

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

Shahee, Aga; Sharma, Shivani; Singh, K.

2015-06-24

The current progress of materials science regarding multifunctional materials (MFM) has put forward the challenges to understand the microscopic origin of their properties. Most of such MFMs have magneto-elastic correlations. To investigate the underlying mechanism it is therefore essential to investigate the structural properties in the presence of magnetic field. Keeping this in view low temperature and high magnetic field (LTHM) powder x-ray diffraction (XRD), a unique state-of-art facility in the country has been developed at CSR Indore. This setup works on symmetric Bragg Brentano geometry using a parallel incident x-ray beam from a rotating anode source working at 17more » kW. Using this one can do structural studies at non-ambient conditions i.e. at low- temperatures (2-300 K) and high magnetic field (+8 to −8 T). The available scattering angle ranges from 5° to 115° 2θ with a resolution better than 0.1°. The proper functioning of the setup has been checked using Si sample. The effect of magnetic field on the structural properties has been demonstrated on Pr{sub 0.5}Sr{sub 0.5}MnO{sub 3} sample. Clear effect of field induced phase transition has been observed. Moreover, the effect of zero field cooled and field cooled conditions is also observed.« less

X-ray and neutron diffraction studies of crystallinity in hydroxyapatite coatings.

PubMed

Girardin, E; Millet, P; Lodini, A

2000-02-01

To standardize industrial implant production and make comparisons between different experimental results, we have to be able to quantify the crystallinity of hydroxyapatite. Methods of measuring crystallinity ratio were developed for various HA samples before and after plasma spraying. The first series of methods uses X-ray diffraction. The advantage of these methods is that X-ray diffraction equipment is used widely in science and industry. In the second series, a neutron diffraction method is developed and the results recorded are similar to those obtained by the modified X-ray diffraction methods. The advantage of neutron diffraction is the ability to obtain measurements deep inside a component. It is a nondestructive method, owing to the very low absorption of neutrons in most materials. Copyright 2000 John Wiley & Sons, Inc.

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

High Rate Deposition of Thick CrN and Cr2N Coatings Using Modulated Pulse Power (MPP) Magnetron Sputtering

DTIC Science & Technology

2010-12-01

in the conventional Bragg-Bentano mode. The residual stress of the coatings was measured by glancing incident angle XRD (GIXRD) in the same X - ray ...micro-analysis (EPMA), x - ray diffraction (XRD), field-emission scanning electron microscopy (FESEM), nanoindentation, scratch test, and ball-on...the coatings was determined by XRD using a SIEMENS X - ray diffractometer (Model KRISTALLOFLEX-810) operated with K-alpha Cu radiation (30 kV and 20 mA

Magnetic field effects on ultrafast lattice compression dynamics of Si(111) crystal when excited by linearly-polarized femtosecond laser pulses

NASA Astrophysics Data System (ADS)

Hatanaka, Koji; Odaka, Hideho; Ono, Kimitoshi; Fukumura, Hiroshi

2007-03-01

Time-resolved X-ray diffraction measurements of Si (111) single crystal are performed when excited by linearly-polarized femtosecond laser pulses (780 nm, 260 fs, negatively-chirped, 1 kHz) under a magnetic field (0.47 T). Laser fluence on the sample surface is 40 mJ/cm^2, which is enough lower than the ablation threshold at 200 mJ/cm^2. Probing X-ray pulses of iron characteristic X-ray lines at 0.193604 and 0.193998 nm are generated by focusing femtosecond laser pulses onto audio-cassette tapes in air. Linearly-polarized femtosecond laser pulse irradiation onto Si(111) crystal surface induces transient lattice compression in the picosecond time range, which is confirmed by transient angle shift of X-ray diffraction to higher angles. Little difference of compression dynamics is observed when the laser polarization is changed from p to s-pol. without a magnetic field. On the other hand, under a magnetic field, the lattice compression dynamics changes when the laser is p-polarized which is vertical to the magnetic field vector. These results may be assigned to photo-carrier formation and energy-band distortion.

Achieving diffraction-limited nanometer-scale X-ray point focus with two crossed multilayer Laue lenses: alignment challenges

DOE PAGES

Yan, Hanfei; Huang, Xiaojing; Bouet, Nathalie; ...

2017-10-16

In this article, we discuss misalignment-induced aberrations in a pair of crossed multilayer Laue lenses used for achieving a nanometer-scale x-ray point focus. We thoroughly investigate the impacts of two most important contributions, the orthogonality and the separation distance between two lenses. We find that misalignment in the orthogonality results in astigmatism at 45º and other inclination angles when coupled with a separation distance error. Theoretical explanation and experimental verification are provided. We show that to achieve a diffraction-limited point focus, accurate alignment of the azimuthal angle is required to ensure orthogonality between two lenses, and the required accuracy ismore » scaled with the ratio of the focus size to the aperture size.« less

Highly exothermic and superhydrophobic Mg/fluorocarbon core/shell nanoenergetic arrays.

PubMed

Zhou, Xiang; Xu, Daguo; Yang, Guangcheng; Zhang, Qiaobao; Shen, Jinpeng; Lu, Jian; Zhang, Kaili

2014-07-09

Mg/fluorocarbon core/shell nanoenergetic arrays are prepared onto silicon substrate, with Mg nanorods as the core and fluorocarbon as the shell. Mg nanorods are deposited by the glancing angle deposition technique, and the fluorocarbon layer is then prepared as a shell to encase the Mg nanorods by the magnetron sputtering deposition process. Scanning electron microscopy and transmission electron microscopy show the core/shell structure of the Mg/fluorocarbon arrays. X-ray energy-dispersive spectroscopy, X-ray diffraction, and Fourier transform infrared spectroscopy are used to characterize the structural composition of the Mg/fluorocarbon. It is found that the as-prepared fluorocarbon layer consists of shorter molecular chains compared to that of bulk polytetrafluoroethylene, which is proven beneficial to the low onset reaction temperature of Mg/fluorocarbon. Water contact angle test demonstrates the superhydrophobicity of the Mg/fluorocarbon arrays, and a static contact angle as high as 162° is achieved. Thermal analysis shows that the Mg/fluorocarbon material exhibits a very low onset reaction temperature of about 270 °C as well as an ultrahigh heat of reaction approaching 9 kJ/g. A preliminary combustion test reveals rapid combustion wave propagation, and a convective mechanism is adopted to explain the combustion behaviors.

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.

Development of an adaptable coherent x-ray diffraction microscope with the emphasis on imaging hydrated specimens.

PubMed

Nam, Daewoong; Park, Jaehyun; Gallagher-Jones, Marcus; Shimada, Hiroki; Kim, Sangsoo; Kim, Sunam; Kohmura, Yoshiki; Ishikawa, Tetsuya; Song, Changyong

2013-11-01

This paper describes the development of a versatile coherent x-ray diffraction microscope capable of imaging biological specimens in solution. The microscope is a flexible platform accommodating various conditions, from low vacuum (10(-2) Pa) to helium gas filled ambient pressure. This flexibility greatly expands the application area, from in situ materials science to biology systems in their native state, by significantly relaxing restrictions to the sample environment. The coherent diffraction microscope has been used successfully to image a yeast cell immersed in buffer solution. We believe that the design of this coherent diffraction microscope can be directly adapted to various platforms such as table top soft x-ray laser, synchrotron x-ray sources, and x-ray free electron laser with minor relevant adjustments.

Development of an adaptable coherent x-ray diffraction microscope with the emphasis on imaging hydrated specimens

NASA Astrophysics Data System (ADS)

Nam, Daewoong; Park, Jaehyun; Gallagher-Jones, Marcus; Shimada, Hiroki; Kim, Sangsoo; Kim, Sunam; Kohmura, Yoshiki; Ishikawa, Tetsuya; Song, Changyong

2013-11-01

This paper describes the development of a versatile coherent x-ray diffraction microscope capable of imaging biological specimens in solution. The microscope is a flexible platform accommodating various conditions, from low vacuum (10-2 Pa) to helium gas filled ambient pressure. This flexibility greatly expands the application area, from in situ materials science to biology systems in their native state, by significantly relaxing restrictions to the sample environment. The coherent diffraction microscope has been used successfully to image a yeast cell immersed in buffer solution. We believe that the design of this coherent diffraction microscope can be directly adapted to various platforms such as table top soft x-ray laser, synchrotron x-ray sources, and x-ray free electron laser with minor relevant adjustments.

Fabrication update on critical-angle transmission gratings for soft x-ray grating spectrometers

NASA Astrophysics Data System (ADS)

Heilmann, Ralf K.; Bruccoleri, Alex; Mukherjee, Pran; Yam, Jonathan; Schattenburg, Mark L.

2011-09-01

Diffraction grating-based, wavelength dispersive high-resolution soft x-ray spectroscopy of celestial sources promises to reveal crucial data for the study of the Warm-Hot Intergalactic Medium, the Interstellar Medium, warm absorption and outflows in Active Galactic Nuclei, coronal emission from stars, and other areas of interest to the astrophysics community. Our recently developed critical-angle transmission (CAT) gratings combine the advantages of the Chandra high and medium energy transmission gratings (low mass, high tolerance of misalignments and figure errors, polarization insensitivity) with those of blazed reflection gratings (high broad band diffraction efficiency, high resolution through use of higher diffraction orders) such as the ones on XMM-Newton. Extensive instrument and system configuration studies have shown that a CAT grating-based spectrometer is an outstanding instrument capable of delivering resolving power on the order of 5,000 and high effective area, even with a telescope point-spread function on the order of many arc-seconds. We have fabricated freestanding, ultra-high aspect-ratio CAT grating bars from silicon-on-insulator wafers using both wet and dry etch processes. The 200 nm-period grating bars are supported by an integrated Level 1 support mesh, and a coarser external Level 2 support mesh. The resulting grating membrane is mounted to a frame, resulting in a grating facet. Many such facets comprise a grating array that provides light-weight coverage of large-area telescope apertures. Here we present fabrication results on the integration of CAT gratings and the different high-throughput support mesh levels and on membrane-frame bonding. We also summarize recent x-ray data analysis of 3 and 6 micron deep wet-etched CAT grating prototypes.

Magnetic topology of Co-based inverse opal-like structures

NASA Astrophysics Data System (ADS)

Grigoryeva, N. A.; Mistonov, A. A.; Napolskii, K. S.; Sapoletova, N. A.; Eliseev, A. A.; Bouwman, W.; Byelov, D. V.; Petukhov, A. V.; Chernyshov, D. Yu.; Eckerlebe, H.; Vasilieva, A. V.; Grigoriev, S. V.

2011-08-01

The magnetic and structural properties of a cobalt inverse opal-like crystal have been studied by a combination of complementary techniques ranging from polarized neutron scattering and superconducting quantum interference device (SQUID) magnetometry to x-ray diffraction. Microradian small-angle x-ray diffraction shows that the inverse opal-like structure (OLS) synthesized by the electrochemical method fully duplicates the three-dimensional net of voids of the template artificial opal. The inverse OLS has a face-centered cubic (fcc) structure with a lattice constant of 640±10 nm and with a clear tendency to a random hexagonal close-packed structure along the [111] axes. Wide-angle x-ray powder diffraction shows that the atomic cobalt structure is described by coexistence of 95% hexagonal close-packed and 5% fcc phases. The SQUID measurements demonstrate that the inverse OLS film possesses easy-plane magnetization geometry with a coercive field of 14.0 ± 0.5 mT at room temperature. The detailed picture of the transformation of the magnetic structure under an in-plane applied field was detected with the help of small-angle diffraction of polarized neutrons. In the demagnetized state the magnetic system consists of randomly oriented magnetic domains. A complex magnetic structure appears upon application of the magnetic field, with nonhomogeneous distribution of magnetization density within the unit element of the OLS. This distribution is determined by the combined effect of the easy-plane geometry of the film and the crystallographic geometry of the opal-like structure with respect to the applied field direction.

USAF Summer Research Program - 1993 High School Apprenticeship Program Final Reports, Volume 15, Wright Laboratory

DTIC Science & Technology

1993-12-01

of the films. One is x - ray diffraction which is used to determine the crystallographic orientation of the films. No phases other than the YBa 2Cu3O 7...x were observed in any of the films. The x - ray data for the films with high critical current densities show strong peaks of reflections indicating a...Solving for x ca = (p/2 Now, if we look at a close-up of the prism face at the input ray (FIGURE 7), we want to solve for the angle between the rays

Scanning electron microscopy, x-ray diffraction, and electron microprobe analysis of calcific deposits on intrauterine contraceptive devices

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

Khan, S.R.; Wilkinson, E.J.

Deposits found on intrauterine contraceptive devices (IUDs) were studied by scanning electron microscopy, x-ray diffraction, and energy dispersive x-ray microanalysis. All seven devices, including five plastic and two copper IUDs, were coated with a crust containing cellular, acellular, and fibrillar material. The cellular material was composed of erythrocytes, leukocytes, cells of epithelial origin, sperm, and bacteria. Some of the bacteria were filamentous, with acute-angle branching. The fibrillar material appeared to be fibrin. Most of the acellular material was amorphous; calcite was identified by x-ray diffraction, and x-ray microanalysis showed only calcium. Some of the acellular material, particularly that on themore » IUD side of the crust, was organized in spherulitic crystals and was identified as calcium phosphate by x-ray microanalysis. The crust was joined to the IUD surface by a layer of fibrillar and amorphous material. It is suggested that the initial event in the formation of calcific deposits on IUD surfaces is the deposition of an amorphous and fibrillar layer. Various types of cells present in the endometrial environment adhere to this layer and then calcify. Thus, the deposition of calcific material on the IUDs is a calcification phenomenon, not unlike the formation of plaque on teeth.« less

Multifunctional Metallosupramolecular Materials

DTIC Science & Technology

2011-02-28

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

X-ray diffraction study of nanocrystalline and amorphous structure within major and minor ampullate dragline spider silks

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

Sampath, Sujatha; Isdebski, Thomas; Jenkins, Janelle E.

Synchrotron X-ray micro-diffraction experiments were carried out on Nephila clavipes (NC) and Argiope aurantia (AA) major (MA) and minor ampullate (MiA) fibers that make up dragline spider silk. The diffraction patterns show a semi-crystalline structure with {beta}-poly(L-alanine) nanocrystallites embedded in a partially oriented amorphous matrix. A superlattice reflection 'S' diffraction ring is observed, which corresponds to a crystalline component larger in size and is poorly oriented, when compared to the {beta}-poly(L-alanine) nanocrystallites that are commonly observed in dragline spider silks. Crystallite size, crystallinity and orientation about the fiber axis have been determined from the wide-angle X-ray diffraction (WAXD) patterns. Inmore » both NC and AA, the MiA silks are found to be more highly crystalline, when compared with the corresponding MA silks. Detailed analysis on the amorphous matrix shows considerable differences in the degree of order of the oriented amorphous component between the different silks studied and may play a crucial role in determining the mechanical properties of the silks.« less

Microgravity

NASA Image and Video Library

2001-06-06

X-rays diffracted from a well-ordered protein crystal create sharp patterns of scattered light on film. A computer can use these patterns to generate a model of a protein molecule. To analyze the selected crystal, an X-ray crystallographer shines X-rays through the crystal. Unlike a single dental X-ray, which produces a shadow image of a tooth, these X-rays have to be taken many times from different angles to produce a pattern from the scattered light, a map of the intensity of the X-rays after they diffract through the crystal. The X-rays bounce off the electron clouds that form the outer structure of each atom. A flawed crystal will yield a blurry pattern; a well-ordered protein crystal yields a series of sharp diffraction patterns. From these patterns, researchers build an electron density map. With powerful computers and a lot of calculations, scientists can use the electron density patterns to determine the structure of the protein and make a computer-generated model of the structure. The models let researchers improve their understanding of how the protein functions. They also allow scientists to look for receptor sites and active areas that control a protein's function and role in the progress of diseases. From there, pharmaceutical researchers can design molecules that fit the active site, much like a key and lock, so that the protein is locked without affecting the rest of the body. This is called structure-based drug design.

Corrosion product layers on magnesium alloys AZ31 and AZ61: Surface chemistry and protective ability

NASA Astrophysics Data System (ADS)

Feliu, S.; Llorente, I.

2015-08-01

This paper studies the chemical composition of the corrosion product layers formed on magnesium alloys AZ31 and AZ61 following immersion in 0.6 M NaCl, with a view to better understanding their protective action. Relative differences in the chemical nature of the layers were quantified by X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), energy dispersive analysis of X-ray (EDX) and low-angle X-ray diffraction (XRD). Corrosion behavior was investigated by Electrochemical Impedance Spectroscopy (EIS) and hydrogen evolution measurement. An inhibitive effect from the corrosion product layers was observed from EIS, principally in the case of AZ31, as confirmed by hydrogen evolution tests. A link was found between carbonate enrichment observed by XPS in the surface of the corrosion product layer, concomitant with the increase in the protective properties observed by EIS.

Construction of horizontal stratum landform-like composite foams and their methyl orange adsorption capacity

NASA Astrophysics Data System (ADS)

Chen, Jiajia; Shi, Xiaowen; Zhan, Yingfei; Qiu, Xiaodan; Du, Yumin; Deng, Hongbing

2017-03-01

Chitosan (CS)/rectorite (REC)/carbon nanotubes (CNTs) composite foams with good mechanical properties were successfully fabricated by unidirectional freeze-casting technique. The morphology of the foam showed the well-ordered porous three-dimensional layers and horizontal stratum landform-like structure. The holes on the layers looked like the wings of butterfly. Additionally, the X-ray photoelectron spectroscopy and energy-dispersive X-ray spectroscopy results indicated the successful addition of CNTs and REC. The intercalated REC with CS chains was confirmed by small-angle X-ray diffraction. The surface structure of the foams was also analyzed by Raman spectroscopy. The adsorption experiments showed that when the mass ratio of CS to REC was 10:1 and CNTs content was 20%, the composite foam performed best in adsorbing low concentration methyl orange, and the largest adsorption capacity was 41.65 mg/g.

A multi-cone x-ray imaging Bragg crystal spectrometer

DOE PAGES

Bitter, M.; Hill, K. W.; Gao, Lan; ...

2016-08-26

This article describes a new x-ray imaging Bragg crystal spectrometer, which—in combination with a streak camera or a gated strip detector—can be used for time-resolved measurements of x-ray line spectra at the National Ignition Facility and other high power laser facilities. The main advantage of this instrument is that it produces perfect images of a point source for each wavelength in a selectable spectral range and that the detector plane can be perpendicular to the crystal surface or inclined by an arbitrary angle with respect to the crystal surface. Furthermore, these unique imaging properties are obtained by bending the x-raymore » diffracting crystal into a certain shape, which is generated by arranging multiple cones with different aperture angles on a common nodal line.« less

Materials identification using a small-scale pixellated x-ray diffraction system

NASA Astrophysics Data System (ADS)

O'Flynn, D.; Crews, C.; Drakos, I.; Christodoulou, C.; Wilson, M. D.; Veale, M. C.; Seller, P.; Speller, R. D.

2016-05-01

A transmission x-ray diffraction system has been developed using a pixellated, energy-resolving detector (HEXITEC) and a small-scale, mains operated x-ray source (Amptek Mini-X). HEXITEC enables diffraction to be measured without the requirement of incident spectrum filtration, or collimation of the scatter from the sample, preserving a large proportion of the useful signal compared with other diffraction techniques. Due to this efficiency, sufficient molecular information for material identification can be obtained within 5 s despite the relatively low x-ray source power. Diffraction data are presented from caffeine, hexamine, paracetamol, plastic explosives and narcotics. The capability to determine molecular information from aspirin tablets inside their packaging is demonstrated. Material selectivity and the potential for a sample classification model is shown with principal component analysis, through which each different material can be clearly resolved.

Diamond sensors and polycapillary lenses for X-ray absorption spectroscopy.

PubMed

Ravel, B; Attenkofer, K; Bohon, J; Muller, E; Smedley, J

2013-10-01

Diamond sensors are evaluated as incident beam monitors for X-ray absorption spectroscopy experiments. These single crystal devices pose a challenge for an energy-scanning experiment using hard X-rays due to the effect of diffraction from the crystalline sensor at energies which meet the Bragg condition. This problem is eliminated by combination with polycapillary lenses. The convergence angle of the beam exiting the lens is large compared to rocking curve widths of the diamond. A ray exiting one capillary from the lens meets the Bragg condition for any reflection at a different energy from the rays exiting adjacent capillaries. This serves to broaden each diffraction peak over a wide energy range, allowing linear measurement of incident intensity over the range of the energy scan. Extended X-ray absorption fine structure data are measured with a combination of a polycapillary lens and a diamond incident beam monitor. These data are of comparable quality to data measured without a lens and with an ionization chamber monitoring the incident beam intensity.

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

Instrument and method for focusing x rays, gamma rays, and neutrons

DOEpatents

Smither, R.K.

1981-04-20

A crystal diffraction instrument is described which has an improved crystalline structure having a face for receiving a beam of photons or neutrons and diffraction planar spacing along that face with the spacing increasing progressively along the face to provide a decreasing Bragg angle and thereby increasing the usable area and acceptance angle. The increased planar spacing is provided by the use of a temperature differential across the crystalline structure, by assembling a plurality of crystalline structure with different compositions, by an individual crystalline structure with a varying composition and thereby a changing planar spacing along its face, and by combinations of these techniques.

High-energy synchrotron x-ray techniques for studying irradiated materials

DOE PAGES

Park, Jun-Sang; Zhang, Xuan; Sharma, Hemant; ...

2015-03-20

High performance materials that can withstand radiation, heat, multiaxial stresses, and corrosive environment are necessary for the deployment of advanced nuclear energy systems. Nondestructive in situ experimental techniques utilizing high energy x-rays from synchrotron sources can be an attractive set of tools for engineers and scientists to investigate the structure–processing–property relationship systematically at smaller length scales and help build better material models. In this paper, two unique and interconnected experimental techniques, namely, simultaneous small-angle/wide-angle x-ray scattering (SAXS/WAXS) and far-field high-energy diffraction microscopy (FF-HEDM) are presented. Finally, the changes in material state as Fe-based alloys are heated to high temperatures ormore » subject to irradiation are examined using these techniques.« less

Grazing-incidence X-ray diffraction from a crystal with subsurface defects

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

Gaevskii, A. Yu., E-mail: transilv@mail.ru; Golentus, I. E.

2015-03-15

The diffraction of X rays incident on a crystal surface under grazing angles under conditions of total external reflection has been investigated. An approach is proposed in which exact solutions to the dynamic problem of grazing-incidence diffraction in an ideal crystal are used as initial functions to calculate the diffuse component of diffraction in a crystal with defects. The diffuse component of diffraction is calculated for a crystal with surface defects of a dilatation-center type. Exact formulas of the continuum theory which take into account the mirror-image forces are used for defect-induced atomic displacements. Scattering intensity maps near Bragg peaksmore » are constructed for different scan modes, and the conditions for detecting primarily the diffuse component are determined. The results of dynamic calculations of grazing-incidence diffraction in defect-containing crystals are compared with calculations in the kinematic approximation.« less

X-ray crystallography

NASA Technical Reports Server (NTRS)

2001-01-01

X-rays diffracted from a well-ordered protein crystal create sharp patterns of scattered light on film. A computer can use these patterns to generate a model of a protein molecule. To analyze the selected crystal, an X-ray crystallographer shines X-rays through the crystal. Unlike a single dental X-ray, which produces a shadow image of a tooth, these X-rays have to be taken many times from different angles to produce a pattern from the scattered light, a map of the intensity of the X-rays after they diffract through the crystal. The X-rays bounce off the electron clouds that form the outer structure of each atom. A flawed crystal will yield a blurry pattern; a well-ordered protein crystal yields a series of sharp diffraction patterns. From these patterns, researchers build an electron density map. With powerful computers and a lot of calculations, scientists can use the electron density patterns to determine the structure of the protein and make a computer-generated model of the structure. The models let researchers improve their understanding of how the protein functions. They also allow scientists to look for receptor sites and active areas that control a protein's function and role in the progress of diseases. From there, pharmaceutical researchers can design molecules that fit the active site, much like a key and lock, so that the protein is locked without affecting the rest of the body. This is called structure-based drug design.

Structure of gel phase DMPC determined by X-ray diffraction.

PubMed Central

Tristram-Nagle, Stephanie; Liu, Yufeng; Legleiter, Justin; Nagle, John F

2002-01-01

The structure of fully hydrated gel phase dimyristoylphosphatidylcholine lipid bilayers was obtained at 10 degrees C. Oriented lipid multilayers were used to obtain high signal-to-noise intensity data. The chain tilt angle and an estimate of the methylene electron density were obtained from wide angle reflections. The chain tilt angle is measured to be 32.3 +/- 0.6 degrees near full hydration, and it does not change as the sample is mildly dehydrated from a repeat spacing of D = 59.9 A to D = 56.5 A. Low angle diffraction peaks were obtained up to the tenth order for 17 samples with variable D and prepared by three different methods with different geometries. In addition to the usual Fourier reconstructions of the electron density profiles, model electron density profiles were fit to all the low angle data simultaneously while constraining the model to include the wide-angle data and the measured lipid volume. Results are obtained for area/lipid (A = 47.2 +/- 0.5 A(2)), the compressibility modulus (K(A) = 500 +/- 100 dyn/cm), various thicknesses, such as the hydrocarbon thickness (2D(C) = 30.3 +/- 0.2 A), and the head-to-head spacing (D(HH) = 40.1 +/- 0.1 A). PMID:12496100

Sucrose lyophiles: a semi-quantitative study of residual water content by total X-ray diffraction analysis.

PubMed

Bates, S; Jonaitis, D; Nail, S

2013-10-01

Total X-ray Powder Diffraction Analysis (TXRPD) using transmission geometry was able to observe significant variance in measured powder patterns for sucrose lyophilizates with differing residual water contents. Integrated diffraction intensity corresponding to the observed variances was found to be linearly correlated to residual water content as measured by an independent technique. The observed variance was concentrated in two distinct regions of the lyophilizate powder pattern, corresponding to the characteristic sucrose matrix double halo and the high angle diffuse region normally associated with free-water. Full pattern fitting of the lyophilizate powder patterns suggested that the high angle variance was better described by the characteristic diffraction profile of a concentrated sucrose/water system rather than by the free-water diffraction profile. This suggests that the residual water in the sucrose lyophilizates is intimately mixed at the molecular level with sucrose molecules forming a liquid/solid solution. The bound nature of the residual water and its impact on the sucrose matrix gives an enhanced diffraction response between 3.0 and 3.5 beyond that expected for free-water. The enhanced diffraction response allows semi-quantitative analysis of residual water contents within the studied sucrose lyophilizates to levels below 1% by weight. Copyright © 2013 Elsevier B.V. All rights reserved.

Coherent X-ray diffraction from collagenous soft tissues

PubMed Central

Berenguer de la Cuesta, Felisa; Wenger, Marco P. E.; Bean, Richard J.; Bozec, Laurent; Horton, Michael A.; Robinson, Ian K.

2009-01-01

Coherent X-ray diffraction has been applied in the imaging of inorganic materials with great success. However, its application to biological specimens has been limited to some notable exceptions, due to the induced radiation damage and the extended nature of biological samples, the last limiting the application of most part of the phasing algorithms. X-ray ptychography, still under development, is a good candidate to overcome such difficulties and become a powerful imaging method for biology. We describe herein the feasibility of applying ptychography to the imaging of biological specimens, in particular collagen rich samples. We report here speckles in diffraction patterns from soft animal tissue, obtained with an optimized small angle X-ray setup that exploits the natural coherence of the beam. By phasing these patterns, dark field images of collagen within tendon, skin, bone, or cornea will eventually be obtained with a resolution of 60–70 nm. We present simulations of the contrast mechanism in collagen based on atomic force microscope images of the samples. Simulations confirmed the ‘speckled’ nature of the obtained diffraction patterns. Once inverted, the patterns will show the disposition and orientation of the fibers within the tissue, by enhancing the phase contrast between protein and no protein regions of the sample. Our work affords the application of the most innovative coherent X-ray diffraction tools to the study of biological specimens, and this approach will have a significant impact in biology and medicine because it overcomes many of the limits of current microscopy techniques. PMID:19706395

Coherent X-ray diffraction from collagenous soft tissues.

PubMed

Berenguer de la Cuesta, Felisa; Wenger, Marco P E; Bean, Richard J; Bozec, Laurent; Horton, Michael A; Robinson, Ian K

2009-09-08

Coherent X-ray diffraction has been applied in the imaging of inorganic materials with great success. However, its application to biological specimens has been limited to some notable exceptions, due to the induced radiation damage and the extended nature of biological samples, the last limiting the application of most part of the phasing algorithms. X-ray ptychography, still under development, is a good candidate to overcome such difficulties and become a powerful imaging method for biology. We describe herein the feasibility of applying ptychography to the imaging of biological specimens, in particular collagen rich samples. We report here speckles in diffraction patterns from soft animal tissue, obtained with an optimized small angle X-ray setup that exploits the natural coherence of the beam. By phasing these patterns, dark field images of collagen within tendon, skin, bone, or cornea will eventually be obtained with a resolution of 60-70 nm. We present simulations of the contrast mechanism in collagen based on atomic force microscope images of the samples. Simulations confirmed the 'speckled' nature of the obtained diffraction patterns. Once inverted, the patterns will show the disposition and orientation of the fibers within the tissue, by enhancing the phase contrast between protein and no protein regions of the sample. Our work affords the application of the most innovative coherent X-ray diffraction tools to the study of biological specimens, and this approach will have a significant impact in biology and medicine because it overcomes many of the limits of current microscopy techniques.

Soft x-ray transmission grating spectrometer for X-ray Surveyor and smaller missions with high resolving power

NASA Astrophysics Data System (ADS)

Heilmann, Ralf K.; Bruccoleri, Alexander; Schattenburg, Mark; Kolodziejczak, jeffery; Gaskin, Jessica; O'Dell, Stephen L.

2017-01-01

A number of high priority subjects in astrophysics are addressed by a state-of-the-art soft x-ray grating spectrometer, e.g. the role of Active Galactic Nuclei in galaxy and star formation, characterization of the WHIM and the “missing baryon” problem, characterization of halos around the Milky Way and nearby galaxies, and stellar coronae and surrounding winds and disks. An Explorer-scale, large-area (A > 1,000 cm2), high resolving power (R > 3,000) soft x-ray grating spectrometer is highly feasible based on Critical-Angle Transmission (CAT) grating technology, even for telescopes with angular resolution of 5-10 arcsec. Significantly higher performance could be provided by a CAT grating spectrometer on an X-ray-Surveyor-type mission (A > 4,000 cm2, R > 5,000). CAT gratings combine advantages of blazed reflection gratings (high efficiency, use of higher orders) with those of transmission gratings (low mass, relaxed alignment tolerances and temperature requirements, transparent at higher energies) with minimal mission resource requirements. Blazing is achieved through grazing-incidence reflection off the smooth silicon grating bar sidewalls. Silicon is well matched to the soft x-ray band, and 30% absolute diffraction efficiency has been acheived with clear paths for further improvement. CAT gratings with sidewalls made of high-Z elements allow extension of blazing to higher energies and larger dispersion angles, enabling higher resolving power at shorter wavelengths. X-ray data from CAT gratings coated with a thin layer of platinum using atomic layer deposition demonstrate efficient blazing to higher energies and much larger blaze angles than possible with silicon alone. Measurements of the resolving power of a breadboard CAT grating spectrometer consisting of a Wolter-I slumped-glass focusing optic from GSFC and CAT gratings, taken at the MSFC Stray Light Facility, have demonstrated resolving power > 10,000. Thus currently fabricated CAT gratings are compatible with the most advanced grating spectrometer instrument designs for future soft x-ray spectroscopy missions. We will review the most recent CAT grating fabrication and x-ray test results.

Femtosecond X-ray coherent diffraction of aligned amyloid fibrils on low background graphene.

PubMed

Seuring, Carolin; Ayyer, Kartik; Filippaki, Eleftheria; Barthelmess, Miriam; Longchamp, Jean-Nicolas; Ringler, Philippe; Pardini, Tommaso; Wojtas, David H; Coleman, Matthew A; Dörner, Katerina; Fuglerud, Silje; Hammarin, Greger; Habenstein, Birgit; Langkilde, Annette E; Loquet, Antoine; Meents, Alke; Riek, Roland; Stahlberg, Henning; Boutet, Sébastien; Hunter, Mark S; Koglin, Jason; Liang, Mengning; Ginn, Helen M; Millane, Rick P; Frank, Matthias; Barty, Anton; Chapman, Henry N

2018-05-09

Here we present a new approach to diffraction imaging of amyloid fibrils, combining a free-standing graphene support and single nanofocused X-ray pulses of femtosecond duration from an X-ray free-electron laser. Due to the very low background scattering from the graphene support and mutual alignment of filaments, diffraction from tobacco mosaic virus (TMV) filaments and amyloid protofibrils is obtained to 2.7 Å and 2.4 Å resolution in single diffraction patterns, respectively. Some TMV diffraction patterns exhibit asymmetry that indicates the presence of a limited number of axial rotations in the XFEL focus. Signal-to-noise levels from individual diffraction patterns are enhanced using computational alignment and merging, giving patterns that are superior to those obtainable from synchrotron radiation sources. We anticipate that our approach will be a starting point for further investigations into unsolved structures of filaments and other weakly scattering objects.

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

James, Veronica J.; ANU)

An early diagnosis of malignancies correlates directly with a better prognosis. Yet for many malignancies there are no readily available, noninvasive, cost-effective diagnostic tests with patients often presenting too late for effective treatment. This article describes for the first time the use of fiber diffraction patterns of skin or fingernails, using X-ray sources, as a biometric diagnostic method for detecting neoplastic disorders including but not limited to melanoma, breast, colon and prostate cancers. With suitable further development, an early low-cost, totally noninvasive yet reliable diagnostic test could be conducted on a regular basis in local radiology facilities, as a confirmatorymore » test for other diagnostic procedures or as a mass screening test using suitable small angle X-ray beam-lines at synchrotrons.« less

Three-energy focusing Laue monochromator for the diamond light source x-ray pair distribution function beamline I15-1

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

Sutter, John P., E-mail: john.sutter@diamond.ac.uk; Chater, Philip A.; Hillman, Michael R.

2016-07-27

The I15-1 beamline, the new side station to I15 at the Diamond Light Source, will be dedicated to the collection of atomic pair distribution function data. A Laue monochromator will be used consisting of three silicon crystals diffracting X-rays at a common Bragg angle of 2.83°. The crystals use the (1 1 1), (2 2 0), and (3 1 1) planes to select 40, 65, and 76 keV X-rays, respectively, and will be bent meridionally to horizontally focus the selected X-rays onto the sample. All crystals will be cut to the same optimized asymmetry angle in order to eliminate imagemore » broadening from the crystal thickness. Finite element calculations show that the thermal distortion of the crystals will affect the image size and bandpass.« less

In-Plane Anisotropic Photoconduction in Nonpolar Epitaxial a-Plane GaN.

PubMed

Pant, Rohit; Shetty, Arjun; Chandan, Greeshma; Roul, Basanta; Nanda, K K; Krupanidhi, S B

2018-05-16

Nonpolar a-plane GaN epitaxial films were grown on an r-plane sapphire using the plasma-assisted molecular beam epitaxy system, with various nitrogen plasma power conditions. The crystallinity of the films was characterized by high-resolution X-ray diffraction and reciprocal space mapping. Using the X-ray "rocking curve-phi scan", [0002], [1-100], and [1-102] azimuth angles were identified, and interdigitated electrodes along these directions were fabricated to evaluate the direction-dependent UV photoresponses. UV responsivity ( R) and internal gain ( G) were found to be dependent on the azimuth angle and in the order of [0002] > [1-102] > [1-100], which has been attributed to the enhanced crystallinity and lowest defect density along [0002] azimuth. The temporal response was very stable irrespective of growth conditions and azimuth angles. Importantly, response time, responsivity, and internal gain were 210 ms, 1.88 A W -1 , and 648.9%, respectively, even at a bias as low as 1 V. The results were validated using the Silvaco Atlas device simulator, and experimental observations were consistent with simulated results. Overall, the photoresponse is dependent on azimuth angles and requires further optimization, especially for materials with in-plane crystal anisotropy.

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

Amemiya, Kenta; Toyoshima, Akio; Kikuchi, Takashi

The design and commissioning of a new soft X-ray beamline, BL-16A, at the Photon Factory is presented. The beamline consists of a pre-focusing mirror, an entrance slit, a variable-included-angle varied-line-spacing plane grating monochromator, and a post-focusing system as usual, and provides circularly and linearly polarized soft X rays in the energy range 200-1500 eV with an APPLE-II type undulator. The commissioning procedure for the beamline optics is described in detail, especially the check of the focal position for the zero-th order and diffracted X rays.

Anomalous X-Ray yields under surface wave resonance during reflection high energy electron diffraction and adatom site determination

PubMed

Yamanaka; Ino

2000-05-08

In L x-ray emissions from a Si(111)-sqrt[3]xsqrt[3]-In surface induced by electron beam irradiation were measured as functions of the incident glancing angle. Under surface wave resonance conditions, anomalous x-ray intensities were clearly observed. Using dynamical calculations, these intensities are well explained as changes in density of the electron wave field at adatom positions. From these intensities, the adatom site was analyzed, and it was found that the T4 model is better than the H3 model.

Part I: an x-ray scattering study of cholera toxin penetration and induced phase transformations in lipid membranes.

PubMed

Miller, C E; Majewski, J; Watkins, E B; Kuhl, T L

2008-07-01

Cholera toxin is a highly efficient biotoxin, which is frequently used as a tool to investigate protein-membrane interactions and as a reporter for membrane rafts. Cholera toxin binds selectively to gangliosides with highest affinity to GM(1). However, the mechanism by which cholera toxin crosses the membrane remains unresolved. Using x-ray reflectivity and grazing incidence diffraction, we have been able to monitor the binding and penetration of cholera toxin into a model lipid monolayer containing the receptor GM(1) at the air-water interface. Very high toxin coverage was obtained allowing precise measurements of how toxin binding alters lipid packing. Grazing incidence x-ray diffraction revealed the coexistence of two monolayer phases after toxin binding. The first was identical to the monolayer before toxin binding. In regions where toxin was bound, a second membrane phase exhibited a decrease in order as evidenced by a larger area per molecule and tilt angle with concomitant thinning of the monolayer. These results demonstrate that cholera toxin binding induces the formation of structurally distinct, less ordered domains in gel phases. Furthermore, the largest decrease in lateral order to the monolayer occurred at low pH, supporting a low endosomal pH in the infection pathway. Surprisingly, at pH = 8 toxin penetration by the binding portion of the toxin, the B(5) pentamer, was also observed.

Biaxially oriented CdTe films on glass substrate through nanostructured Ge/CaF2 buffer layers

NASA Astrophysics Data System (ADS)

Lord, R. J.; Su, P.-Y.; Bhat, I.; Zhang, S. B.; Lu, T.-M.; Wang, G.-C.

2015-09-01

Heteroepitaxial CdTe films were grown by metal organic chemical vapor deposition on glass substrates through nanostructured Ge/CaF2 buffer layers which were biaxially oriented. It allows us to explore the structural properties of multilayer biaxial semiconductor films which possess small angle grain boundaries and to test the principle of a solar cell made of such low-cost, low-growth-temperature semiconductor films. Through the x-ray diffraction and x-ray pole figure analysis, the heteroepitaxial relationships of the mutilayered films are determined as [111] in the out-of-plane direction and <1\\bar{1}0>CdTe//<1\\bar{1}0>Ge//{< \\bar{1}10> }{{{CaF}}2} in the in-plane direction. The I-V curves measured from an ITO/CdS/CdTe/Ge/CaF2/glass solar cell test structure shows a power conversion efficiency of ˜η = 1.26%, illustrating the initial success of such an approach. The observed non-ideal efficiency is believed to be due to a low shunt resistance and high series resistance as well as some residual large-angle grain boundary effects, leaving room for significant further improvement.

Microstructural Characteristic of the Al-Fe-Cu Alloy During High-Speed Repetitive Continuous Extrusion Forming

NASA Astrophysics Data System (ADS)

Hu, Jiamin; Teng, Jie; Ji, Xiankun; Kong, Xiangxin; Jiang, Fulin; Zhang, Hui

2016-11-01

High-speed repetitive continuous extrusion forming process (R-Conform process) was performed on the Al-Fe-Cu alloy. The microstructural evolution and mechanical properties were studied by x-ray diffraction, electron backscatter diffraction, transmission electron microscopy and tensile testing. The results show that a significant improvement of tensile ductility concurs with a considerable loss of tensile strength before four passes, after that the process on mechanical properties variation tends to be steady, indicating an accelerated mechanical softening occurs when comparing to low-speed R-Conform process. Microstructure characterization indicates that the accumulated strain promotes the transformation of low angle boundaries to high angle boundaries, thus leading to the acceleration of continuous dynamic recrystallization process, and the precipitates are broken, spheroidized and homogeneously distribute in Al matrix as increasing R-Conform passes. Massive microshear bands are observed after initial passes of R-Conform process, which may promote continuous dynamic recrystallization and further grain refinement during high-speed R-Conform process.

Critical-angle transmission grating technology development for high resolving power soft x-ray spectrometers on Arcus and Lynx

NASA Astrophysics Data System (ADS)

Heilmann, Ralf K.; Bruccoleri, Alexander R.; Song, Jungki; Kolodziejczak, Jeffery; Gaskin, Jessica A.; O'Dell, Stephen L.; Cheimetz, Peter; Hertz, Edward; Smith, Randall K.; Burwitz, Vadim; Hartner, Gisela; La Caria, Marlis-Madeleine; Schattenburg, Mark L.

2017-08-01

Soft x-ray spectroscopy with high resolving power (R = λ/Δλ) and large effective area (A) addresses numerous unanswered science questions about the physical laws that lead to the structure of our universe. In the soft x-ray band R > 1000 can currently only be achieved with diffraction grating-based spectroscopy. Criticalangle transmission (CAT) gratings combine the advantages of blazed reflection gratings (high efficiency, use of higher diffraction orders) with those of conventional transmission gratings (relaxed alignment tolerances and temperature requirements, transparent at higher energies, low mass), resulting in minimal mission resource requirements, while greatly improving figures of merit. Diffraction efficiency > 33% and R > 10, 000 have been demonstrated for CAT gratings. Last year the technology has been certified at Technology Readiness Level 4 based on a probe class mission concept. The Explorer-scale (A > 450 cm2 , R > 2500) grating spectroscopy Arcus mission can be built with today's CAT grating technology and has been selected in the current Explorer round for a Phase A concept study. Its figure of merit for the detection of weak absorption lines will be an order of magnitude larger than current instruments on Chandra and XMM-Newton. Further CAT grating technology development and improvements in the angular resolution of x-ray optics can provide another order of magnitude improvement in performance, as is envisioned for the X-ray Surveyor/Lynx mission concept currently under development for input into the 2020 Decadal Survey. For Arcus we have tested CAT gratings in a spectrometer setup in combination with silicon pore optics (SPO) and obtained resolving power results that exceed Arcus requirements before and after environmental testing of the gratings. We have recently fabricated the largest (32 mm x 32 mm) CAT gratings to date, and plan to increase grating size further. We mounted two of these large gratings to frames and aligned them in the roll direction using a laser-based technique. Simultaneous x-ray illumination of both gratings with an SPO module demonstrated that we can exceed Arcus grating-to-grating alignment requirements without x rays.

Reconstitution of SNARE proteins into solid-supported lipid bilayer stacks and X-ray structure analysis.

PubMed

Xu, Yihui; Kuhlmann, Jan; Brennich, Martha; Komorowski, Karlo; Jahn, Reinhard; Steinem, Claudia; Salditt, Tim

2018-02-01

SNAREs are known as an important family of proteins mediating vesicle fusion. For various biophysical studies, they have been reconstituted into supported single bilayers via proteoliposome adsorption and rupture. In this study we extended this method to the reconstitution of SNAREs into supported multilamellar lipid membranes, i.e. oriented multibilayer stacks, as an ideal model system for X-ray structure analysis (X-ray reflectivity and diffraction). The reconstitution was implemented through a pathway of proteomicelle, proteoliposome and multibilayer. To monitor the structural evolution in each step, we used small-angle X-ray scattering for the proteomicelles and proteoliposomes, followed by X-ray reflectivity and grazing-incidence small-angle scattering for the multibilayers. Results show that SNAREs can be successfully reconstituted into supported multibilayers, with high enough orientational alignment for the application of surface sensitive X-ray characterizations. Based on this protocol, we then investigated the effect of SNAREs on the structure and phase diagram of the lipid membranes. Beyond this application, this reconstitution protocol could also be useful for X-ray analysis of many further membrane proteins. Copyright © 2017 Elsevier B.V. All rights reserved.

The path for long range conduction in high J(sub c) TlBa2Ca2Cu3O(8+x) spray-pyrolyzed deposits

NASA Astrophysics Data System (ADS)

Kroeger, D. M.; Goyal, A.; Specht, E. D.; Wang, Z. L.; Tkaczyk, J. E.; Sutliff, J. A.; Deluca, J. A.

Grain boundary misorientations and local texture in polycrystalline TlBa2Ca2Cu3O(8+x) deposits prepared by thallination of spray-pyrolyzed precursor deposits on yttria-stabilized zirconia have been determined from transmission electron microscopy, electron backscatter diffraction patterns, and x ray diffraction. The deposits were polycrystalline, had small grains, and excellent c-axis alignment. The deposits contained colonies of grains with similar but not identical a-axis orientations. Most grain boundaries within a colony have small misorientation angles and should not be weak links. It is proposed that long range current flow occurs through a percolative network of small angle grain boundaries at colony intersections.

Investigation of the Structural Stability of Ion-Implanted Gd 2Ti 2-xSn xO 7 Pyrochlore-Type Oxides by Glancing Angle X-ray Absorption Spectroscopy

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

Aluri, Esther Rani; Hayes, John R.; Walker, James D.S.

2016-03-24

Rare-earth titanate and stannate pyrochlore-type oxides have been investigated in the past for the sequestration of nuclear waste elements because of their resistance to radiation-induced structural damage. In order to enhance this property, it is necessary to understand the effect of radioactive decay of the incorporated actinide elements on the local chemical environment. In this study, Gd 2Ti 2–xSn xO 7 materials have been implanted with Au– ions to simulate radiation-induced structural damage. Glancing angle X-ray absorption near-edge spectroscopy (GA-XANES), glancing angle X-ray absorption fine structure (GA-EXAFS) analysis, and powder X-ray diffraction have been used to investigate changes in themore » local coordination environment of the metal atoms in the damaged surface layer. Examination of GA-XANES/EXAFS spectra from the implanted Gd 2Ti 2–xSn xO 7 materials collected at various glancing angles allowed for an investigation of how the local coordination environment around the absorbing atoms changed at different depths in the damaged surface layer. This study has shown the usefulness of GA-XANES to the examination of ion-implanted materials and has suggested that Gd 2Ti 2–xSn xO 7 becomes more susceptible to ion-beam-induced structural damage with increasing Sn concentration.« less

The Scherrer equation and the dynamical theory of X-ray diffraction.

PubMed

Muniz, Francisco Tiago Leitão; Miranda, Marcus Aurélio Ribeiro; Morilla Dos Santos, Cássio; Sasaki, José Marcos

2016-05-01

The Scherrer equation is a widely used tool to determine the crystallite size of polycrystalline samples. However, it is not clear if one can apply it to large crystallite sizes because its derivation is based on the kinematical theory of X-ray diffraction. For large and perfect crystals, it is more appropriate to use the dynamical theory of X-ray diffraction. Because of the appearance of polycrystalline materials with a high degree of crystalline perfection and large sizes, it is the authors' belief that it is important to establish the crystallite size limit for which the Scherrer equation can be applied. In this work, the diffraction peak profiles are calculated using the dynamical theory of X-ray diffraction for several Bragg reflections and crystallite sizes for Si, LaB6 and CeO2. The full width at half-maximum is then extracted and the crystallite size is computed using the Scherrer equation. It is shown that for crystals with linear absorption coefficients below 2117.3 cm(-1) the Scherrer equation is valid for crystallites with sizes up to 600 nm. It is also shown that as the size increases only the peaks at higher 2θ angles give good results, and if one uses peaks with 2θ > 60° the limit for use of the Scherrer equation would go up to 1 µm.

Determination of line profiles on nano-structured surfaces using EUV and x-ray scattering

NASA Astrophysics Data System (ADS)

Soltwisch, Victor; Wernecke, Jan; Haase, Anton; Probst, Jürgen; Schoengen, Max; Krumrey, Michael; Scholze, Frank; Pomplun, Jan; Burger, Sven

2014-09-01

Non-imaging techniques like X-ray scattering are supposed to play an important role in the further development of CD metrology for the semiconductor industry. Grazing Incidence Small Angle X-ray Scattering (GISAXS) provides directly assessable information on structure roughness and long-range periodic perturbations. The disadvantage of the method is the large footprint of the X-ray beam on the sample due to the extremely shallow angle of incidence. This can be overcome by using wavelengths in the extreme ultraviolet (EUV) spectral range, EUV small angle scattering (EUVSAS), which allows for much steeper angles of incidence but preserves the range of momentum transfer that can be observed. Generally, the potentially higher momentum transfer at shorter wavelengths is counterbalanced by decreasing diffraction efficiency. This results in a practical limit of about 10 nm pitch for which it is possible to observe at least the +/- 1st diffraction orders with reasonable efficiency. At the Physikalisch-Technische Bundesanstalt (PTB), the available photon energy range extends from 50 eV up to 10 keV at two adjacent beamlines. PTB commissioned a new versatile Ellipso-Scatterometer which is capable of measuring 6" square substrates in a clean, hydrocarbon-free environment with full flexibility regarding the direction of the incident light polarization. The reconstruction of line profiles using a geometrical model with six free parameters, based on a finite element method (FEM) Maxwell solver and a particle swarm based least-squares optimization yielded consistent results for EUV-SAS and GISAXS. In this contribution we present scatterometry data for line gratings and consistent reconstruction results of the line geometry for EUV-SAS and GISAXS.

Emerging surface characterization techniques for carbon steel corrosion: a critical brief review.

PubMed

Dwivedi, D; Lepkova, K; Becker, T

2017-03-01

Carbon steel is a preferred construction material in many industrial and domestic applications, including oil and gas pipelines, where corrosion mitigation using film-forming corrosion inhibitor formulations is a widely accepted method. This review identifies surface analytical techniques that are considered suitable for analysis of thin films at metallic substrates, but are yet to be applied to analysis of carbon steel surfaces in corrosive media or treated with corrosion inhibitors. The reviewed methods include time of flight-secondary ion mass spectrometry, X-ray absorption spectroscopy methods, particle-induced X-ray emission, Rutherford backscatter spectroscopy, Auger electron spectroscopy, electron probe microanalysis, near-edge X-ray absorption fine structure spectroscopy, X-ray photoemission electron microscopy, low-energy electron diffraction, small-angle neutron scattering and neutron reflectometry, and conversion electron Moessbauer spectrometry. Advantages and limitations of the analytical methods in thin-film surface investigations are discussed. Technical parameters of nominated analytical methods are provided to assist in the selection of suitable methods for analysis of metallic substrates deposited with surface films. The challenges associated with the applications of the emerging analytical methods in corrosion science are also addressed.

Emerging surface characterization techniques for carbon steel corrosion: a critical brief review

NASA Astrophysics Data System (ADS)

Dwivedi, D.; Lepkova, K.; Becker, T.

2017-03-01

Carbon steel is a preferred construction material in many industrial and domestic applications, including oil and gas pipelines, where corrosion mitigation using film-forming corrosion inhibitor formulations is a widely accepted method. This review identifies surface analytical techniques that are considered suitable for analysis of thin films at metallic substrates, but are yet to be applied to analysis of carbon steel surfaces in corrosive media or treated with corrosion inhibitors. The reviewed methods include time of flight-secondary ion mass spectrometry, X-ray absorption spectroscopy methods, particle-induced X-ray emission, Rutherford backscatter spectroscopy, Auger electron spectroscopy, electron probe microanalysis, near-edge X-ray absorption fine structure spectroscopy, X-ray photoemission electron microscopy, low-energy electron diffraction, small-angle neutron scattering and neutron reflectometry, and conversion electron Moessbauer spectrometry. Advantages and limitations of the analytical methods in thin-film surface investigations are discussed. Technical parameters of nominated analytical methods are provided to assist in the selection of suitable methods for analysis of metallic substrates deposited with surface films. The challenges associated with the applications of the emerging analytical methods in corrosion science are also addressed.

Emerging surface characterization techniques for carbon steel corrosion: a critical brief review

PubMed Central

Dwivedi, D.; Becker, T.

2017-01-01

Carbon steel is a preferred construction material in many industrial and domestic applications, including oil and gas pipelines, where corrosion mitigation using film-forming corrosion inhibitor formulations is a widely accepted method. This review identifies surface analytical techniques that are considered suitable for analysis of thin films at metallic substrates, but are yet to be applied to analysis of carbon steel surfaces in corrosive media or treated with corrosion inhibitors. The reviewed methods include time of flight-secondary ion mass spectrometry, X-ray absorption spectroscopy methods, particle-induced X-ray emission, Rutherford backscatter spectroscopy, Auger electron spectroscopy, electron probe microanalysis, near-edge X-ray absorption fine structure spectroscopy, X-ray photoemission electron microscopy, low-energy electron diffraction, small-angle neutron scattering and neutron reflectometry, and conversion electron Moessbauer spectrometry. Advantages and limitations of the analytical methods in thin-film surface investigations are discussed. Technical parameters of nominated analytical methods are provided to assist in the selection of suitable methods for analysis of metallic substrates deposited with surface films. The challenges associated with the applications of the emerging analytical methods in corrosion science are also addressed. PMID:28413351

Crystal structure and density of helium to 232 kbar

NASA Technical Reports Server (NTRS)

Mao, H. K.; Wu, Y.; Jephcoat, A. P.; Hemley, R. J.; Bell, P. M.; Bassett, W. A.

1988-01-01

The properties of helium and hydrogen at high pressure are topics of great interest to the understanding of planetary interiors. These materials constitute 95 percent of the entire solar system. A technique was presented for the measurement of X-ray diffraction from single-crystals of low-Z condenses gases in a diamond-anvil cell at high pressure. The first such single-crystal X-ray diffraction measurements on solid hydrogen to 26.5 GPa were presented. The application of this technique to the problem of the crystal structure, equation of state, and phase diagram of solid helium is reported. Crucial for X-ray diffraction studies of these materials is the use of a synchrotron radiation source which provides high brillance, narrow collimation of the incident and diffracted X-ray beams to reduce the background noise, and energy-dispersive diffraction techniques with polychromatic (white) radiation, which provides high detection efficiency.

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

Feng, Hao; Ashkar, Rana; Steinke, Nina

A method dubbed grating-based holography was recently used to determine the structure of colloidal fluids in the rectangular grooves of a diffraction grating from X-ray scattering measurements. Similar grating-based measurements have also been recently made with neutrons using a technique called spin-echo small-angle neutron scattering. The analysis of the X-ray diffraction data was done using an approximation that treats the X-ray phase change caused by the colloidal structure as a small perturbation to the overall phase pattern generated by the grating. In this paper, the adequacy of this weak phase approximation is explored for both X-ray and neutron grating holography.more » Additionally, it is found that there are several approximations hidden within the weak phase approximation that can lead to incorrect conclusions from experiments. In particular, the phase contrast for the empty grating is a critical parameter. Finally, while the approximation is found to be perfectly adequate for X-ray grating holography experiments performed to date, it cannot be applied to similar neutron experiments because the latter technique requires much deeper grating channels.« less

Lattice-Preferred Orientation in Deformed Novaculite - Comparison of in-situ Results Using BEARTEX and Post-Mortem EBSD Analyses

NASA Astrophysics Data System (ADS)

Willenweber, A.; Thomas, S.; Burnley, P. C.

2012-12-01

The Berkeley Texture Package BEARTEX is a Windows-based computer software that combines various algorithms to analyze lattice-preferred orientation in polycrystalline materials. BEARTEX was initially designed to interpret diffraction intensity data from pole figure goniometers. Recently it has been successfully used to process synthetic forsterite powder diffraction data from in-situ synchrotron X-ray diffraction taken during deformation (Bollinger et al. 2012). Our study aims to test the practicability of using BEARTEX to analyze the evolution of lattice-preferred orientation in natural polycrystalline quartz (novaculite) during deformation. In-situ X-ray diffraction data was collected during the deformation of novaculite at 2.5 GPa and up to 1000 °C in a D-DIA apparatus using the ten-element energy-dispersive detector at the NSLS beamline X17B2. Diffraction intensities are a function of crystal orientation, expressed in azimuth angle η and pole distance ψ. The latter is the angle between the normal of a given diffraction plane and the vertical direction of the D-DIA apparatus - our principal stress direction during compression. Orientation-dependent diffraction intensities were corrected for different responses of the single detectors and x-ray absorption effects of the anvils. Orientation distributions (ODs) and inverse pole figures were calculated using BEARTEX. In addition, electron backscatter diffraction (EBSD) analyses were carried out on the deformed novaculite samples. Generated pole figures were compared with those derived from BEARTEX. Textural properties of our novaculite starting material complicated the BEARTEX analyses. The relatively strong variation of grain sizes in our natural specimens caused non-random diffraction intensity distributions. Those lead to non-random distributions of crystal orientations when analyzed with BEARTEX, although pole figures from EBSD data clearly show random crystal orientations. In an attempt to solve this problem, we employed a scanning routine when recording in-situ synchrotron X-ray diffraction and so collected diffraction from multiple sample volumes rather than from one single spot. Here, we will present a comparison of pole figures derived from independent BEARTEX and EBSD analyses for a series of novaculite experiments and discuss the practicability of BEARTEX to analyze the evolution of lattice-preferred orientation in natural polycrystalline quartz. REFERENCES C. BOLLINGER, S. MERKEL AND P. RATERRON (2012): In situ quantitative analysis of stress and texture development in forsterite aggregates deformed at 6 GPa and 1373 K. J. Appl. Cryst., 45, 263-271.

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

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

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

2009-03-15

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

Physical properties of new binary antiferroelectric liquid crystal mixtures

NASA Astrophysics Data System (ADS)

Fitas, Jakub; Jaworska-Gołąb, Teresa; Deptuch, Aleksandra; Tykarska, Marzena; Kurp, Katarzyna; Żurowska, Magdalena; Marzec, Monika

2018-02-01

Three newly prepared binary mixtures exhibiting chiral tilted smectic phases have been studied using differential scanning calorimetry, dielectric spectroscopy and electro-optic method, as well as X-ray diffraction. Broad temperature range of ferroelectric and antiferroelectric phases was detected in these mixtures and temperature dependence of spontaneous polarization, tilt angle and switching time were measured for all of them. It's occurred that all of the studied mixtures are orthoconic antiferroelectric liquid crystals. Based on the X-ray diffraction results, the temperature dependence of layer thickness in the paraelectric, ferroelectric and antiferroelectric phases was found. By using dielectric spectroscopy, Goldstone mode was identified in the ferroelectric phase, while antiphase fluctuations of azimuthal angle have been found in the antiferroelectric phase. Based on the results of the complementary methods, the transition temperatures were found as well as the order of the para-ferroelectric phase transition was determined as non-continuous one with critical parameter β equal to ca. 0.25.

A high-transparency, micro-patternable chip for X-ray diffraction analysis of microcrystals under native growth conditions

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

Murray, Thomas D.; Johns Hopkins University School of Medicine, Baltimore, MD 21205; Lyubimov, Artem Y.

A highly X-ray-transparent, silicon nitride-based device has been designed and fabricated to harvest protein microcrystals for high-resolution X-ray diffraction data collection using microfocus beamlines and XFELs. Microcrystals present a significant impediment to the determination of macromolecular structures by X-ray diffraction methods. Although microfocus synchrotron beamlines and X-ray free-electron lasers (XFELs) can enable the collection of interpretable diffraction data from microcrystals, there is a need for efficient methods of harvesting small volumes (<2 µl) of microcrystals grown under common laboratory formats and delivering them to an X-ray beam source under native growth conditions. One approach that shows promise in overcoming themore » challenges intrinsic to microcrystal analysis is to pair so-called ‘fixed-target’ sample-delivery devices with microbeam-based X-ray diffraction methods. However, to record weak diffraction patterns it is necessary to fabricate devices from X-ray-transparent materials that minimize background scattering. Presented here is the design of a new micro-diffraction device consisting of three layers fabricated from silicon nitride, photoresist and polyimide film. The chip features low X-ray scattering and X-ray absorption properties, and uses a customizable blend of hydrophobic and hydrophilic surface patterns to help localize microcrystals to defined regions. Microcrystals in their native growth conditions can be loaded into the chips with a standard pipette, allowing data collection at room temperature. Diffraction data collected from hen egg-white lysozyme microcrystals (10–15 µm) loaded into the chips yielded a complete, high-resolution (<1.6 Å) data set sufficient to determine a high-quality structure by molecular replacement. The features of the chip allow the rapid and user-friendly analysis of microcrystals grown under virtually any laboratory format at microfocus synchrotron beamlines and XFELs.« less

Crystalline Stratification in Semiconducting Polymer Thin Film Quantified by Grazing Incidence X-ray Scattering

NASA Astrophysics Data System (ADS)

Gann, Eliot; Caironi, Mario; Noh, Yong-Young; Kim, Yun-Hi; McNeill, Christopher R.

The depth dependence of crystalline structure within thin films is critical for many technological applications, but has been impossible to measure directly using common techniques. In this work, by monitoring diffraction peak intensity and location and utilizing the highly angle-dependent waveguiding effects of X-rays near grazing incidence we quantitatively measure the thickness, roughness and orientation of stratified crystalline layers within thin films of a high-performance semiconducting polymer. In particular, this diffractive X-ray waveguiding reveals a self-organized 5-nm-thick crystalline surface layer with crystalline orientation orthogonal to the underlying 65-nm-thick layer. While demonstrated for an organic semiconductor film, this approach is applicable to any thin film material system where stratified crystalline structure and orientation can influence important interfacial processes such as charge injection and field-effect transport.

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 ...

Structural changes in shock compressed silicon observed using time-resolved x-ray diffraction at the Dynamic Compression Sector

NASA Astrophysics Data System (ADS)

Turneaure, Stefan; Zdanowicz, E.; Sinclair, N.; Graber, T.; Gupta, Y. M.

2015-06-01

Structural changes in shock compressed silicon were observed directly using time-resolved x-ray diffraction (XRD) measurements at the Dynamic Compression Sector at the Advanced Photon Source. The silicon samples were impacted by polycarbonate impactors accelerated to velocities greater than 5 km/s using a two-stage light gas gun resulting in impact stresses of about 25 GPa. The 23.5 keV synchrotron x-ray beam passed through the polycarbonate impactor, the silicon sample, and an x-ray window (polycarbonate or LiF) at an angle of 30 degrees relative to the impact plane. Four XRD frames (~ 100 ps snapshots) were obtained with 153.4 ns between frames near the time of impact. The XRD measurements indicate that in the peak shocked state, the silicon samples completely transformed to a high-pressure phase. XRD results for both shocked polycrystalline silicon and single crystal silicon will be presented and compared. Work supported by DOE/NNSA.

Anisotropic x-ray scattering and orientation fields in cardiac tissue cells

NASA Astrophysics Data System (ADS)

Bernhardt, M.; Nicolas, J.-D.; Eckermann, M.; Eltzner, B.; Rehfeldt, F.; Salditt, T.

2017-01-01

X-ray diffraction from biomolecular assemblies is a powerful technique which can provide structural information about complex architectures such as the locomotor systems underlying muscle contraction. However, in its conventional form, macromolecular diffraction averages over large ensembles. Progress in x-ray optics has now enabled to probe structures on sub-cellular scales, with the beam confined to a distinct organelle. Here, we use scanning small angle x-ray scattering (scanning SAXS) to probe the diffraction from cytoskeleton networks in cardiac tissue cells. In particular, we focus on actin-myosin composites, which we identify as the dominating contribution to the anisotropic diffraction patterns, by correlation with optical fluorescence microscopy. To this end, we use a principal component analysis approach to quantify direction, degree of orientation, nematic order, and the second moment of the scattering distribution in each scan point. We compare the fiber orientation from micrographs of fluorescently labeled actin fibers to the structure orientation of the x-ray dataset and thus correlate signals of two different measurements: the native electron density distribution of the local probing area versus specifically labeled constituents of the sample. Further, we develop a robust and automated fitting approach based on a power law expansion, in order to describe the local structure factor in each scan point over a broad range of the momentum transfer {q}{{r}}. Finally, we demonstrate how the methodology shown for freeze dried cells in the first part of the paper can be translated to alive cell recordings.

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

J Cai; B Hsiao; R Gross

Poly({omega}-pentadecalactone) (PPDL), a model polymer in the poly({omega}-hydroxyl fatty acids) family, is a new biopolymer with monomer synthesized by yeast-catalyzed {omega}-hydroxylation of fatty acids. In this study, deformation-induced structural changes in two PPDL samples with different molecular weights were studied by in situ wide-angle X-ray diffraction (WAXD) and small-angle X-ray scattering (SAXS) techniques. The high molecular weight PPDL (PPDL-high) sample exhibited notable strain hardening, while the low molecular weight PPDL (PPDL-low) sample did not. The behavior can be explained by the entanglement density concept. The evolution of crystallinity (from WAXD) as a function of strain could be divided into fourmore » distinct regions, but their respective mechanisms differ slightly in each sample. During stretching, a mesomorphic phase formed in both samples, bridging between the amorphous and strain-induced crystal phases. The SAXS data verified the effect of molecular weight (or the entanglement density) on the deformation-induced structure of PPDL. The parameters of chain orientation factor (f) calculated from the orthorhombic crystal cell as well as the nonorthorhombic crystal cell proposed by Wilchinsky were used to follow the orientation process during stretching of PPDLs. It was found that the different molecular entanglement network (i.e., PPDL-low versus PPDL-high) led to different crystal orientation behavior, especially in the low strain range.« less

Diffractive-refractive optics: X-ray splitter.

PubMed

Hrdý, Jaromír

2010-01-01

The possibility of splitting a thin (e.g. undulator) X-ray beam based on diffraction-refraction effects is discussed. The beam is diffracted from a crystal whose diffracting surface has the shape of a roof with the ridge lying in the plane of diffraction. The crystal is cut asymmetrically. One half of the beam impinges on the left-hand part of the roof and the other half impinges on the right-hand side of the roof. Owing to refraction the left part of the beam is deviated to the left whereas the right part is deviated to the right. The device proposed consists of two channel-cut crystals with roof-like diffraction surfaces; the crystals are set in a dispersive position. The separation of the beams after splitting is calculated at a distance of 10 m from the crystals for various asymmetry and inclination angles. It is shown that such a splitting may be utilized for long beamlines. Advantages and disadvantages of this method are discussed.

Measurement of fatigue accumulation in high-strength steels by microstructural examination

NASA Astrophysics Data System (ADS)

Nakagawa, Y. G.; Yoshizawa, H.; Lapides, M. E.

1990-07-01

Fatigue test bars fabricated from an SA508 class 3 low-carbon steel plate were cyclically deformed at 300 °C (constant low-cycle fatigue, total strain range Δɛ = 0.78 pct and 0.48 pct) to crack initiation (100 pct cumulative damage, CD) and to the factors 75, 50, and 25 pct CD. The test bars were cut perpendicular to the stress axis at the center of the gage length. The X-ray diffraction line-broadening (XRD) was performed on the cross sections created by the cuts. Thin foils (˜0.1-μm thick) were prepared from each cross section and used for the transmission electron microscope (TEM) and selected area diffraction (SAD) study. The half-value line breadth change measured by the XRD increased with the CD increase up to 50 pct, beyond which a significant reduction was observed for the 75 and 100 pct CD sample regardless of the incident X-ray beam angle. By the TEM, the undamaged material (0 pct CD) was characterized by high-angle boundaries, small carbide precipitates, and dislocation cell networks in grains. These characteristics did not show any appreciable changes in all of the samples with fatigue damage of the respective levels. Micro-orientation changes of the dislocation cells studied by the SAD of the foils and a statistical data analysis clearly demonstrated that the mean orientation difference in the cells and its standard deviation increased gradually as the CD increased.

The Molecular Architecture for the Intermediate Filaments of Hard α -Keratin Based on the Superlattice Data Obtained from a Study of Mammals Using Synchrotron Fibre Diffraction

DOE PAGES

James, Veronica

2011-01-01

High- and low-angle X-ray diffraction studies of hard α -keratin have been studied, and various models have been proposed over the last 70 years. Most of these studies have been confined to one or two forms of alpha keratin. This high- and low-angle synchrotron fibre diffraction study extends the study to cover all available data for all known forms of hard α -keratin including hairs, fingernails, hooves, horn, and quills from mammals, marsupials, and a monotreme, and it confirms that the model proposed is universally acceptable for all mammals. A complete Bragg analysis of the meridional diffraction patterns, including multiple-timemore » exposures to verify any weak reflections, verified the existence of a superlattice consisting of two infinite lattices and three finite lattices. An analysis of the equatorial patterns establishes the radii of the oligomeric levels of dimers, tetramers, and intermediate filaments (IFs) together with the centre to centre distance for the IFs, thus confirming the proposed helices within helices molecular architecture for hard α -keratin. The results verify that the structure proposed by Feughelman and James meets the criteria for a valid α -keratin structure.« less

The Molecular Architecture for the Intermediate Filaments of Hard [alpha]-Keratin Based on the Superlattice Data Obtained from a Study ofMammals Using Synchrotron Fibre Diffraction

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

James, Veronica

2014-09-24

High- and low-angle X-ray diffraction studies of hard {alpha}-keratin have been studied, and various models have been proposed over the last 70 years. Most of these studies have been confined to one or two forms of alpha keratin. This high- and low-angle synchrotron fibre diffraction study extends the study to cover all available data for all known forms of hard {alpha}-keratin including hairs, fingernails, hooves, horn, and quills from mammals, marsupials, and a monotreme, and it confirms that the model proposed is universally acceptable for all mammals. A complete Bragg analysis of the meridional diffraction patterns, including multiple-time exposures tomore » verify any weak reflections, verified the existence of a superlattice consisting of two infinite lattices and three finite lattices. An analysis of the equatorial patterns establishes the radii of the oligomeric levels of dimers, tetramers, and intermediate filaments (IFs) together with the centre to centre distance for the IFs, thus confirming the proposed helices within helices molecular architecture for hard {alpha}-keratin. The results verify that the structure proposed by Feughelman and James meets the criteria for a valid {alpha}-keratin structure.« less

The Molecular Architecture for the Intermediate Filaments of Hard α -Keratin Based on the Superlattice Data Obtained from a Study of Mammals Using Synchrotron Fibre Diffraction

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

James, Veronica

High- and low-angle X-ray diffraction studies of hard α -keratin have been studied, and various models have been proposed over the last 70 years. Most of these studies have been confined to one or two forms of alpha keratin. This high- and low-angle synchrotron fibre diffraction study extends the study to cover all available data for all known forms of hard α -keratin including hairs, fingernails, hooves, horn, and quills from mammals, marsupials, and a monotreme, and it confirms that the model proposed is universally acceptable for all mammals. A complete Bragg analysis of the meridional diffraction patterns, including multiple-timemore » exposures to verify any weak reflections, verified the existence of a superlattice consisting of two infinite lattices and three finite lattices. An analysis of the equatorial patterns establishes the radii of the oligomeric levels of dimers, tetramers, and intermediate filaments (IFs) together with the centre to centre distance for the IFs, thus confirming the proposed helices within helices molecular architecture for hard α -keratin. The results verify that the structure proposed by Feughelman and James meets the criteria for a valid α -keratin structure.« less

Instrument and method for focusing X-rays, gamma rays and neutrons

DOEpatents

Smither, Robert K.

1984-01-01

A crystal diffraction instrument or diffraction grating instrument with an improved crystalline structure or grating spacing structure having a face for receiving a beam of photons or neutrons and diffraction planar spacing or grating spacing along that face with the spacing increasing progressively along the face to provide a decreasing Bragg diffraction angle for a monochromatic radiation and thereby increasing the usable area and acceptance angle. The increased planar spacing for the diffraction crystal is provided by the use of a temperature differential across the crystalline structure, by assembling a plurality of crystalline structures with different compositions, by an individual crystalline structure with a varying composition and thereby a changing planar spacing along its face, and by combinations of these techniques. The increased diffraction grating element spacing is generated during the fabrication of the diffraction grating by controlling the cutting tool that is cutting the grooves or controlling the laser beam, electron beam or ion beam that is exposing the resist layer, etc. It is also possible to vary this variation in grating spacing by applying a thermal gradient to the diffraction grating in much the same manner as is done in the crystal diffraction case.

Instrument and method for focusing x rays, gamma rays, and neutrons

DOEpatents

Smither, R.K.

1982-03-25

A crystal-diffraction instrument or diffraction-grating instrument is described with an improved crystalline structure or grating spacing structure having a face for receiving a beam of photons or neutrons and diffraction planar spacing or grating spacing along that face with the spacing increasing progressively along the face to provide a decreasing Bragg diffraction angle for a monochromatic radiation and thereby increasing the usable area and acceptance angle. The increased planar spacing for the diffraction crystal is provided by the use of a temperature differential across the line structures with different compositions, by an individual crystalline structure with a varying composition and thereby a changing planar spacing along its face, and by combinations of these techniques. The increased diffraction grating element spacing is generated during the fabrication of the diffraction grating by controlling the cutting tool that is cutting the grooves or controlling the laser beam, electron beam, or ion beam that is exposing the resist layer, etc. It is also possible to vary this variation in grating spacing by applying a thermal gradient to the diffraction grating in much the same manner as is done in the crystal-diffraction case.

Influence of neutron irradiation on the microstructure of nuclear graphite: An X-ray diffraction study

NASA Astrophysics Data System (ADS)

Zhou, Z.; Bouwman, W. G.; Schut, H.; van Staveren, T. O.; Heijna, M. C. R.; Pappas, C.

2017-04-01

Neutron irradiation effects on the microstructure of nuclear graphite have been investigated by X-ray diffraction on virgin and low doses (∼ 1.3 and ∼ 2.2 dpa), high temperature (750° C) irradiated samples. The diffraction patterns were interpreted using a model, which takes into account the turbostratic disorder. Besides the lattice constants, the model introduces two distinct coherent lengths in the c-axis and the basal plane, that characterise the volumes from which X-rays are scattered coherently. The methodology used in this work allows to quantify the effect of irradiation damage on the microstructure of nuclear graphite seen by X-ray diffraction. The results show that the changes of the deduced structural parameters are in agreement with previous observations from electron microscopy, but not directly related to macroscopic changes.

Microfluidic Chips for In Situ Crystal X-ray Diffraction and In Situ Dynamic Light Scattering for Serial Crystallography.

PubMed

Gicquel, Yannig; Schubert, Robin; Kapis, Svetlana; Bourenkov, Gleb; Schneider, Thomas; Perbandt, Markus; Betzel, Christian; Chapman, Henry N; Heymann, Michael

2018-04-24

This protocol describes fabricating microfluidic devices with low X-ray background optimized for goniometer based fixed target serial crystallography. The devices are patterned from epoxy glue using soft lithography and are suitable for in situ X-ray diffraction experiments at room temperature. The sample wells are lidded on both sides with polymeric polyimide foil windows that allow diffraction data collection with low X-ray background. This fabrication method is undemanding and inexpensive. After the sourcing of a SU-8 master wafer, all fabrication can be completed outside of a cleanroom in a typical research lab environment. The chip design and fabrication protocol utilize capillary valving to microfluidically split an aqueous reaction into defined nanoliter sized droplets. This loading mechanism avoids the sample loss from channel dead-volume and can easily be performed manually without using pumps or other equipment for fluid actuation. We describe how isolated nanoliter sized drops of protein solution can be monitored in situ by dynamic light scattering to control protein crystal nucleation and growth. After suitable crystals are grown, complete X-ray diffraction datasets can be collected using goniometer based in situ fixed target serial X-ray crystallography at room temperature. The protocol provides custom scripts to process diffraction datasets using a suite of software tools to solve and refine the protein crystal structure. This approach avoids the artefacts possibly induced during cryo-preservation or manual crystal handling in conventional crystallography experiments. We present and compare three protein structures that were solved using small crystals with dimensions of approximately 10-20 µm grown in chip. By crystallizing and diffracting in situ, handling and hence mechanical disturbances of fragile crystals is minimized. The protocol details how to fabricate a custom X-ray transparent microfluidic chip suitable for in situ serial crystallography. As almost every crystal can be used for diffraction data collection, these microfluidic chips are a very efficient crystal delivery method.

Agglomeration dynamics of germanium islands on a silicon oxide substrate: A grazing incidence small-angle x-ray scattering study

NASA Astrophysics Data System (ADS)

Cheynis, F.; Leroy, F.; Passanante, T.; Müller, P.

2013-04-01

Grazing-incidence small-angle X-ray scattering (GISAXS) and grazing-incidence X-ray diffraction techniques are used to characterise the thermally induced solid-state dewetting of Ge(001) thin films leading to the formation of 3D Ge islands. A quantitative analysis based on the Kolmogorov-Johnson-Mehl-Avrami model is derived. The main physical parameters controlling the dewetting (activation energy and kinetic pre-factors) are determined. Assuming that the dewetting is driven by surface/interface minimisation and limited by surface diffusion, the Ge surface self-diffusion reads as Ds ,0c0 e-Ea/(kBT) ˜3×1018 e-2.6±0.3eV/(kBT) nm2/s. GISAXS technique enables to reconstruct the mean Ge-island shape, including facets.

High-resolution three-dimensional structural microscopy by single-angle Bragg ptychography

DOE PAGES

Hruszkewycz, S. O.; Allain, M.; Holt, M. V.; ...

2016-11-21

Coherent X-ray microscopy by phase retrieval of Bragg diffraction intensities enables lattice distortions within a crystal to be imaged at nanometre-scale spatial resolutions in three dimensions. While this capability can be used to resolve structure–property relationships at the nanoscale under working conditions, strict data measurement requirements can limit the application of current approaches. Here, in this work, we introduce an efficient method of imaging three-dimensional (3D) nanoscale lattice behaviour and strain fields in crystalline materials with a methodology that we call 3D Bragg projection ptychography (3DBPP). This method enables 3D image reconstruction of a crystal volume from a series ofmore » two-dimensional X-ray Bragg coherent intensity diffraction patterns measured at a single incident beam angle. Structural information about the sample is encoded along two reciprocal-space directions normal to the Bragg diffracted exit beam, and along the third dimension in real space by the scanning beam. Finally, we present our approach with an analytical derivation, a numerical demonstration, and an experimental reconstruction of lattice distortions in a component of a nanoelectronic prototype device.« less

Microstructural investigation of nickel silicide thin films and the silicide-silicon interface using transmission electron microscopy.

PubMed

Bhaskaran, M; Sriram, S; Mitchell, D R G; Short, K T; Holland, A S; Mitchell, A

2009-01-01

This article discusses the results of transmission electron microscopy (TEM)-based investigation of nickel silicide (NiSi) thin films grown on silicon. Nickel silicide is currently used as the CMOS technology standard for local interconnects and in electrical contacts. Films were characterized with a range of TEM-based techniques along with glancing angle X-ray diffraction. The nickel silicide thin films were formed by vacuum annealing thin films of nickel (50 nm) deposited on (100) silicon. The cross-sectional samples indicated a final silicide thickness of about 110 nm. This investigation studied and reports on three aspects of the thermally formed thin films: the uniformity in composition of the film using jump ratio maps; the nature of the interface using high resolution imaging; and the crystalline orientation of the thin films using selected-area electron diffraction (SAED). The analysis highlighted uniform composition in the thin films, which was also substantiated by spectroscopy techniques; an interface exhibiting the desired abrupt transition from silicide to silicon; and desired and preferential crystalline orientation corresponding to stoichiometric NiSi, supported by glancing angle X-ray diffraction results.

Imaging single cells in a beam of live cyanobacteria with an X-ray laser.

PubMed

van der Schot, Gijs; Svenda, Martin; Maia, Filipe R N C; Hantke, Max; DePonte, Daniel P; Seibert, M Marvin; Aquila, Andrew; Schulz, Joachim; Kirian, Richard; Liang, Mengning; Stellato, Francesco; Iwan, Bianca; Andreasson, Jakob; Timneanu, Nicusor; Westphal, Daniel; Almeida, F Nunes; Odic, Dusko; Hasse, Dirk; Carlsson, Gunilla H; Larsson, Daniel S D; Barty, Anton; Martin, Andrew V; Schorb, Sebastian; Bostedt, Christoph; Bozek, John D; Rolles, Daniel; Rudenko, Artem; Epp, Sascha; Foucar, Lutz; Rudek, Benedikt; Hartmann, Robert; Kimmel, Nils; Holl, Peter; Englert, Lars; Duane Loh, Ne-Te; Chapman, Henry N; Andersson, Inger; Hajdu, Janos; Ekeberg, Tomas

2015-02-11

There exists a conspicuous gap of knowledge about the organization of life at mesoscopic levels. Ultra-fast coherent diffractive imaging with X-ray free-electron lasers can probe structures at the relevant length scales and may reach sub-nanometer resolution on micron-sized living cells. Here we show that we can introduce a beam of aerosolised cyanobacteria into the focus of the Linac Coherent Light Source and record diffraction patterns from individual living cells at very low noise levels and at high hit ratios. We obtain two-dimensional projection images directly from the diffraction patterns, and present the results as synthetic X-ray Nomarski images calculated from the complex-valued reconstructions. We further demonstrate that it is possible to record diffraction data to nanometer resolution on live cells with X-ray lasers. Extension to sub-nanometer resolution is within reach, although improvements in pulse parameters and X-ray area detectors will be necessary to unlock this potential.

Systems and methods for detecting an image of an object using multi-beam imaging from an X-ray beam having a polychromatic distribution

DOEpatents

Parham, Christopher A; Zhong, Zhong; Pisano, Etta; Connor, Jr., Dean M

2015-03-03

Systems and methods for detecting an image of an object using a multi-beam imaging system from an x-ray beam having a polychromatic energy distribution are disclosed. According to one aspect, a method can include generating a first X-ray beam having a polychromatic energy distribution. Further, the method can include positioning a plurality of monochromator crystals in a predetermined position to directly intercept the first X-ray beam such that a plurality of second X-ray beams having predetermined energy levels are produced. Further, an object can be positioned in the path of the second X-ray beams for transmission of the second X-ray beams through the object and emission from the object as transmitted X-ray beams. The transmitted X-ray beams can each be directed at an angle of incidence upon one or more crystal analyzers. Further, an image of the object can be detected from the beams diffracted from the analyzer crystals.

Systems and methods for detecting an image of an object by use of an X-ray beam having a polychromatic distribution

DOEpatents

Parham, Christopher; Zhong, Zhong; Pisano, Etta; Connor, Dean; Chapman, Leroy D.

2010-06-22

Systems and methods for detecting an image of an object using an X-ray beam having a polychromatic energy distribution are disclosed. According to one aspect, a method can include detecting an image of an object. The method can include generating a first X-ray beam having a polychromatic energy distribution. Further, the method can include positioning a single monochromator crystal in a predetermined position to directly intercept the first X-ray beam such that a second X-ray beam having a predetermined energy level is produced. Further, an object can be positioned in the path of the second X-ray beam for transmission of the second X-ray beam through the object and emission from the object as a transmitted X-ray beam. The transmitted X-ray beam can be directed at an angle of incidence upon a crystal analyzer. Further, an image of the object can be detected from a beam diffracted from the analyzer crystal.

Effects of rare-earth co-doping on the local structure of rare-earth phosphate glasses using high and low energy X-ray diffraction.

PubMed

Cramer, Alisha J; Cole, Jacqueline M; FitzGerald, Vicky; Honkimaki, Veijo; Roberts, Mark A; Brennan, Tessa; Martin, Richard A; Saunders, George A; Newport, Robert J

2013-06-14

Rare-earth co-doping in inorganic materials has a long-held tradition of facilitating highly desirable optoelectronic properties for their application to the laser industry. This study concentrates specifically on rare-earth phosphate glasses, (R2O3)x(R'2O3)y(P2O5)(1-(x+y)), where (R, R') denotes (Ce, Er) or (La, Nd) co-doping and the total rare-earth composition corresponds to a range between metaphosphate, RP3O9, and ultraphosphate, RP5O14. Thereupon, the effects of rare-earth co-doping on the local structure are assessed at the atomic level. Pair-distribution function analysis of high-energy X-ray diffraction data (Q(max) = 28 Å(-1)) is employed to make this assessment. Results reveal a stark structural invariance to rare-earth co-doping which bears testament to the open-framework and rigid nature of these glasses. A range of desirable attributes of these glasses unfold from this finding; in particular, a structural simplicity that will enable facile molecular engineering of rare-earth phosphate glasses with 'dial-up' lasing properties. When considered together with other factors, this finding also demonstrates additional prospects for these co-doped rare-earth phosphate glasses in nuclear waste storage applications. This study also reveals, for the first time, the ability to distinguish between P-O and P[double bond, length as m-dash]O bonding in these rare-earth phosphate glasses from X-ray diffraction data in a fully quantitative manner. Complementary analysis of high-energy X-ray diffraction data on single rare-earth phosphate glasses of similar rare-earth composition to the co-doped materials is also presented in this context. In a technical sense, all high-energy X-ray diffraction data on these glasses are compared with analogous low-energy diffraction data; their salient differences reveal distinct advantages of high-energy X-ray diffraction data for the study of amorphous materials.

Radiation response of cubic mesoporous silicate and borosilicate thin films

NASA Astrophysics Data System (ADS)

Manzini, Ayelén; Alurralde, Martín; Luca, Vittorio

2018-01-01

The radiation response has been studied of cubic mesoporous silicate and borosilicate thin films having different boron contents prepared using the block copolymer template Brij 58 and the dip coating technique. The degree of pore ordering of the films was analysed using low-angle X-ray diffraction and film thickness measured by X-ray reflectivity. For films calcined at 350 °C, the incorporation of boron resulted in a reproducible oscillatory variation in the d-spacing and intensity of the primary reflection as a function of boron content. A clear peak was observed in the d-spacing at 5-10 mol% boron incorporation. For borosilicate films of a given composition an overall suppression of d-spacing was observed as a function of aging time relative to films that did not contain boron. This was ascribed to a slow condensation process. The films were irradiated in pile with neutrons and with iodine ions at energies of 180 keV and 70 MeV. Neutron irradiation of the silicate thin films for periods up to 30 days and aged for 400 days resulted in little reduction in either d-spacing or intensity of the primary low-angle X-ray reflection indicating that the films retained their mesopore ordering. In contrast borosilicate films for which the B (n, α) reaction was expected to result in enhanced displacement damage showed much larger variations in X-ray parameters. For these films short irradiation times resulted in a reduction of the d-spacing and intensity of the primary reflections considerably beyond that observed through aging. It is concluded that prolonged neutron irradiation and internal α irradiation have only a small, although measurable, impact on mesoporous borosilicate thin films increasing the degree of condensation and increasing unit cell contraction. When these borosilicate films were irradiated with iodine ions, more profound changes occurred. The pore ordering of the films was significantly degraded when low energy ions were used. In some cases the degree of damage was such that no low-angle reflection could be observed. This degradation of pore ordering was confirmed in scanning electron microscopy images of the irradiated films.

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

Mazuritskiy, M. I., E-mail: mazurmik@gmail.com; Lerer, A. M.; Makhno, P. V.

The angular distribution of the X-ray intensity at the exit of microchannel plates at grazing incidence of monochromatic radiation on the walls of microcapillaries has been investigated. The angles and energies of the primary radiation quanta at which the synchrotron beam excites X-ray fluorescence propagating inside polycapillary structures have been determined. The angular dependences of the intensity distribution of X-rays transmitted through the microcapillaries have been studied theoretically and experimentally for energies corresponding to the region of anomalous dispersion near the L{sub 2,3} absorption edges of silicon. The propagation of waves in hollow polycapillary waveguides, the excitation of X-ray fluorescence,more » and the X-ray diffraction at the exit of microchannel plates have been modeled mathematically. The mathematical model takes into account the presence of a transition layer on the microchannel surface.« less

Structure of nanocrystalline calcium silicate hydrates: insights from X-ray diffraction, synchrotron X-ray absorption and nuclear magnetic resonance.

PubMed

Grangeon, Sylvain; Claret, Francis; Roosz, Cédric; Sato, Tsutomu; Gaboreau, Stéphane; Linard, Yannick

2016-06-01

The structure of nanocrystalline calcium silicate hydrates (C-S-H) having Ca/Si ratios ranging between 0.57 ± 0.05 and 1.47 ± 0.04 was studied using an electron probe micro-analyser, powder X-ray diffraction, 29 Si magic angle spinning NMR, and Fourier-transform infrared and synchrotron X-ray absorption spectroscopies. All samples can be described as nanocrystalline and defective tobermorite. At low Ca/Si ratio, the Si chains are defect free and the Si Q 3 and Q 2 environments account, respectively, for up to 40.2 ± 1.5% and 55.6 ± 3.0% of the total Si, with part of the Q 3 Si being attributable to remnants of the synthesis reactant. As the Ca/Si ratio increases up to 0.87 ± 0.02, the Si Q 3 environment decreases down to 0 and is preferentially replaced by the Q 2 environment, which reaches 87.9 ± 2.0%. At higher ratios, Q 2 decreases down to 32.0 ± 7.6% for Ca/Si = 1.38 ± 0.03 and is replaced by the Q 1 environment, which peaks at 68.1 ± 3.8%. The combination of X-ray diffraction and NMR allowed capturing the depolymerization of Si chains as well as a two-step variation in the layer-to-layer distance. This latter first increases from ∼11.3 Å (for samples having a Ca/Si ratio <∼0.6) up to 12.25 Å at Ca/Si = 0.87 ± 0.02, probably as a result of a weaker layer-to-layer connectivity, and then decreases down to 11 Å when the Ca/Si ratio reaches 1.38 ± 0.03. The decrease in layer-to-layer distance results from the incorporation of interlayer Ca that may form a Ca(OH) 2 -like structure, nanocrystalline and intermixed with C-S-H layers, at high Ca/Si ratios.

Structural Order-Disorder Transformations Monitored by X-Ray Diffraction and Photoluminescence

ERIC Educational Resources Information Center

Lima, R. C.; Paris, E. C.; Leite, E. R.; Espinosa, J. W. M.; Souza, A. G.; Longo, E.

2007-01-01

A study was conducted to examine the structural order-disorder transformation promoted by controlled heat treatment using X-ray diffraction technique (XRD) and photoluminescence (PL) techniques as tools to monitor the degree of structural order. The experiment was observed to be versatile and easily achieved with low cost which allowed producing…

A high-transparency, micro-patternable chip for X-ray diffraction analysis of microcrystals under native growth conditions

DOE PAGES

Murray, Thomas D.; Lyubimov, Artem Y.; Ogata, Craig M.; ...

2015-08-11

Microcrystals present a significant impediment to the determination of macromolecular structures by X-ray diffraction methods. Although microfocus synchrotron beamlines and X-ray free-electron lasers (XFELs) can enable the collection of interpretable diffraction data from microcrystals, there is a need for efficient methods of harvesting small volumes (<2 µl) of microcrystals grown under common laboratory formats and delivering them to an X-ray beam source under native growth conditions. One approach that shows promise in overcoming the challenges intrinsic to microcrystal analysis is to pair so-called `fixed-target' sample-delivery devices with microbeam-based X-ray diffraction methods. However, to record weak diffraction patterns it is necessarymore » to fabricate devices from X-ray-transparent materials that minimize background scattering. Presented here is the design of a new micro-diffraction device consisting of three layers fabricated from silicon nitride, photoresist and polyimide film. The chip features low X-ray scattering and X-ray absorption properties, and uses a customizable blend of hydrophobic and hydrophilic surface patterns to help localize microcrystals to defined regions. Microcrystals in their native growth conditions can be loaded into the chips with a standard pipette, allowing data collection at room temperature. Diffraction data collected from hen egg-white lysozyme microcrystals (10–15 µm) loaded into the chips yielded a complete, high-resolution (<1.6 Å) data set sufficient to determine a high-quality structure by molecular replacement. In addition, the features of the chip allow the rapid and user-friendly analysis of microcrystals grown under virtually any laboratory format at microfocus synchrotron beamlines and XFELs.« less

A high-transparency, micro-patternable chip for X-ray diffraction analysis of microcrystals under native growth conditions

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

Murray, Thomas D.; Lyubimov, Artem Y.; Ogata, Craig M.

Microcrystals present a significant impediment to the determination of macromolecular structures by X-ray diffraction methods. Although microfocus synchrotron beamlines and X-ray free-electron lasers (XFELs) can enable the collection of interpretable diffraction data from microcrystals, there is a need for efficient methods of harvesting small volumes (<2 µl) of microcrystals grown under common laboratory formats and delivering them to an X-ray beam source under native growth conditions. One approach that shows promise in overcoming the challenges intrinsic to microcrystal analysis is to pair so-called `fixed-target' sample-delivery devices with microbeam-based X-ray diffraction methods. However, to record weak diffraction patterns it is necessarymore » to fabricate devices from X-ray-transparent materials that minimize background scattering. Presented here is the design of a new micro-diffraction device consisting of three layers fabricated from silicon nitride, photoresist and polyimide film. The chip features low X-ray scattering and X-ray absorption properties, and uses a customizable blend of hydrophobic and hydrophilic surface patterns to help localize microcrystals to defined regions. Microcrystals in their native growth conditions can be loaded into the chips with a standard pipette, allowing data collection at room temperature. Diffraction data collected from hen egg-white lysozyme microcrystals (10–15 µm) loaded into the chips yielded a complete, high-resolution (<1.6 Å) data set sufficient to determine a high-quality structure by molecular replacement. In addition, the features of the chip allow the rapid and user-friendly analysis of microcrystals grown under virtually any laboratory format at microfocus synchrotron beamlines and XFELs.« less

A high-transparency, micro-patternable chip for X-ray diffraction analysis of microcrystals under native growth conditions

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

Murray, Thomas D.; Lyubimov, Artem Y.; Ogata, Craig M.

Microcrystals present a significant impediment to the determination of macromolecular structures by X-ray diffraction methods. Although microfocus synchrotron beamlines and X-ray free-electron lasers (XFELs) can enable the collection of interpretable diffraction data from microcrystals, there is a need for efficient methods of harvesting small volumes (<2µl) of microcrystals grown under common laboratory formats and delivering them to an X-ray beam source under native growth conditions. One approach that shows promise in overcoming the challenges intrinsic to microcrystal analysis is to pair so-called `fixed-target' sample-delivery devices with microbeam-based X-ray diffraction methods. However, to record weak diffraction patterns it is necessary tomore » fabricate devices from X-ray-transparent materials that minimize background scattering. Presented here is the design of a new micro-diffraction device consisting of three layers fabricated from silicon nitride, photoresist and polyimide film. The chip features low X-ray scattering and X-ray absorption properties, and uses a customizable blend of hydrophobic and hydrophilic surface patterns to help localize microcrystals to defined regions. Microcrystals in their native growth conditions can be loaded into the chips with a standard pipette, allowing data collection at room temperature. Diffraction data collected from hen egg-white lysozyme microcrystals (10–15µm) loaded into the chips yielded a complete, high-resolution (<1.6Å) data set sufficient to determine a high-quality structure by molecular replacement. The features of the chip allow the rapid and user-friendly analysis of microcrystals grown under virtually any laboratory format at microfocus synchrotron beamlines and XFELs.« less

A high-transparency, micro-patternable chip for X-ray diffraction analysis of microcrystals under native growth conditions

PubMed Central

Murray, Thomas D.; Lyubimov, Artem Y.; Ogata, Craig M.; Vo, Huy; Uervirojnangkoorn, Monarin; Brunger, Axel T.; Berger, James M.

2015-01-01

Microcrystals present a significant impediment to the determination of macromolecular structures by X-ray diffraction methods. Although microfocus synchrotron beamlines and X-ray free-electron lasers (XFELs) can enable the collection of interpretable diffraction data from microcrystals, there is a need for efficient methods of harvesting small volumes (<2 µl) of microcrystals grown under common laboratory formats and delivering them to an X-ray beam source under native growth conditions. One approach that shows promise in overcoming the challenges intrinsic to microcrystal analysis is to pair so-called ‘fixed-target’ sample-delivery devices with microbeam-based X-ray diffraction methods. However, to record weak diffraction patterns it is necessary to fabricate devices from X-ray-transparent materials that minimize background scattering. Presented here is the design of a new micro-diffraction device consisting of three layers fabricated from silicon nitride, photoresist and polyimide film. The chip features low X-ray scattering and X-ray absorption properties, and uses a customizable blend of hydrophobic and hydrophilic surface patterns to help localize microcrystals to defined regions. Microcrystals in their native growth conditions can be loaded into the chips with a standard pipette, allowing data collection at room temperature. Diffraction data collected from hen egg-white lysozyme microcrystals (10–15 µm) loaded into the chips yielded a complete, high-resolution (<1.6 Å) data set sufficient to determine a high-quality structure by molecular replacement. The features of the chip allow the rapid and user-friendly analysis of microcrystals grown under virtually any laboratory format at microfocus synchrotron beamlines and XFELs. PMID:26457423

Deformational characteristics of thermoplastic elastomers

NASA Astrophysics Data System (ADS)

Indukuri, Kishore K.

This thesis focuses primarily on the structure-property relationships of poly (styrene-ethylene-butylene-styrene) triblock copolymer TPEs. First evidence for strain-induced crystallization occurring in certain SEBS block copolymers has been established using unique techniques like deformation calorimetry, combined in-situ small angle X-ray and wide angle X-ray diffraction (SAXD/WAXD). Also the ramifications of such strain-induced crystallization on the mechanical properties like cyclic hysteresis, stress relaxation/creep retention of these SEBS systems have been studied. In addition, the structural changes in the morphology of these systems on deformation have been investigated using combined SAXD/WAXD setup. Small angle X-ray diffraction probed the changes at the nano-scale of polystyrene (PS) cylinders, while wide angle X-ray diffraction probed the changes at molecular length scales of the amorphous/crystalline domains of the elastomeric mid-block in these systems. New structural features at both these length scales have been observed and incorporated into the overall deformation mechanisms of the material. Continuous processing techniques like extrusion have been used to obtain ultra long-range order and orientation in these SEBS systems. Thus well ordered crystal like hexagonal packing of cylinders, where in each element in this hexagonal lattice can be individually addressed without any grain boundaries can be realized using these robust techniques. The effect of long-range order/orientation on the mechanical properties has been studied. In addition, these well ordered systems serve as model systems for evaluating deformation mechanisms of these SEBS systems, where the relative contributions of each of the phases can be estimated. EPDM/i-PP thermoplastic vulcanizates (TPVs) have micron size scale phase separated morphologies of EPDM rubber dispersed in a semicrystalline i-PP matrix as a result of the dynamic vulcanization process. Confocal microscopy studies, along with scanning electron microscopy (SEM) studies show that the morphology of these EPDM/i-PP systems resembles a microcellular "filled" foam in which i-PP occupies the strut regions and EPDM the inner core. Based on this, an analytical model has been developed that takes into account composition information, molecular weight, cure state and morphology into account.

Outrunning damage: Electrons vs X-rays-timescales and mechanisms.

PubMed

Spence, John C H

2017-07-01

Toward the end of his career, Zewail developed strong interest in fast electron spectroscopy and imaging, a field to which he made important contributions toward his aim of making molecular movies free of radiation damage. We therefore compare here the atomistic mechanisms leading to destruction of protein samples in diffract-and-destroy experiments for the cases of high-energy electron beam irradiation and X-ray laser pulses. The damage processes and their time-scales are compared and relevant elastic, inelastic, and photoelectron cross sections are given. Inelastic mean-free paths for ejected electrons at very low energies in insulators are compared with the bioparticle size. The dose rate and structural damage rate for electrons are found to be much lower, allowing longer pulses, reduced beam current, and Coulomb interactions for the formation of smaller probes. High-angle electron scattering from the nucleus, which has no parallel in the X-ray case, tracks the slowly moving nuclei during the explosion, just as the gain of the XFEL (X-ray free-electron laser) has no parallel in the electron case. Despite reduced damage and much larger elastic scattering cross sections in the electron case, leading to not dissimilar elastic scattering rates (when account is taken of the greatly increased incident XFEL fluence), progress for single-particle electron diffraction is seen to depend on the effort to reduce emittance growth due to Coulomb interactions, and so allow formation of intense sub-micron beams no larger than a virus.

Nanoporous active carbons at ambient conditions: a comparative study using X-ray scattering and diffraction, Raman spectroscopy and N2 adsorption

NASA Astrophysics Data System (ADS)

Shiryaev, A. A.; Voloshchuk, A. M.; Volkov, V. V.; Averin, A. A.; Artamonova, S. D.

2017-05-01

Furfural-derived sorbents and activated carbonaceous fibers were studied using Small- and Wide-angle X-ray scattering (SWAXS), X-ray diffraction and multiwavelength Raman spectroscopy after storage at ambient conditions. Correlations between structural features with degree of activation and with sorption parameters are observed for samples obtained from a common precursor and differing in duration of activation. However, the correlations are not necessarily applicable to the carbons obtained from different precursors. Using two independent approaches we show that treatment of SWAXS results should be performed with careful analysis of applicability of the Porod law to the sample under study. In general case of a pore with rough/corrugated surface deviations from the Porod law may became significant and reflect structure of the pore-carbon interface. Ignorance of these features may invalidate extraction of closed porosity values. In most cases the pore-matrix interface in the studied samples is not atomically sharp, but is characterized by 1D or 2D fluctuations of electronic density responsible for deviations from the Porod law. Intensity of the pores-related small-angle scattering correlates positively with SBET values obtained from N2 adsorption.

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.

Irena : tool suite for modeling and analysis of small-angle scattering.

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

Ilavsky, J.; Jemian, P.

2009-04-01

Irena, a tool suite for analysis of both X-ray and neutron small-angle scattering (SAS) data within the commercial Igor Pro application, brings together a comprehensive suite of tools useful for investigations in materials science, physics, chemistry, polymer science and other fields. In addition to Guinier and Porod fits, the suite combines a variety of advanced SAS data evaluation tools for the modeling of size distribution in the dilute limit using maximum entropy and other methods, dilute limit small-angle scattering from multiple non-interacting populations of scatterers, the pair-distance distribution function, a unified fit, the Debye-Bueche model, the reflectivity (X-ray and neutron)more » using Parratt's formalism, and small-angle diffraction. There are also a number of support tools, such as a data import/export tool supporting a broad sampling of common data formats, a data modification tool, a presentation-quality graphics tool optimized for small-angle scattering data, and a neutron and X-ray scattering contrast calculator. These tools are brought together into one suite with consistent interfaces and functionality. The suite allows robust automated note recording and saving of parameters during export.« less

Characterization of biogenic ferrihydrite nanoparticles by means of SAXS, SRD and IBA methods

NASA Astrophysics Data System (ADS)

Balasoiu, M.; Kichanov, S.; Pantelica, A.; Pantelica, D.; Stolyar, S.; Iskhakov, R.; Aranghel, D.; Ionescu, P.; Badita, C. R.; Kurkin, S.; Orelovich, O.; Tiutiunikov, S.

2018-03-01

Investigations of biogenic ferrihydrite nanoparticles produced by bacteria Klebsiella oxytoca by applying small angle X-ray scattering, synchrotron radiation diffraction and ion beam analysis methods are reviewed. Different experimental data processing methods are used and analyzed.

Photoelectron diffraction from single oriented molecules: Towards ultrafast structure determination of molecules using x-ray free-electron lasers

NASA Astrophysics Data System (ADS)

Kazama, Misato; Fujikawa, Takashi; Kishimoto, Naoki; Mizuno, Tomoya; Adachi, Jun-ichi; Yagishita, Akira

2013-06-01

We provide a molecular structure determination method, based on multiple-scattering x-ray photoelectron diffraction (XPD) calculations. This method is applied to our XPD data on several molecules having different equilibrium geometries. Then it is confirmed that, by our method, bond lengths and bond angles can be determined with a resolution of less than 0.1 Å and 10∘, respectively. Differently from any other scenario of ultrafast structure determination, we measure the two- or three-dimensional XPD of aligned or oriented molecules in the energy range from 100 to 200 eV with a 4π detection velocity map imaging spectrometer. Thanks to the intense and ultrashort pulse properties of x-ray free-electron lasers, our approach exhibits the most probable method for obtaining ultrafast real-time structural information on small to medium-sized molecules consisting of light elements, i.e., a “molecular movie.”

Advancing X-ray scattering metrology using inverse genetic algorithms.

PubMed

Hannon, Adam F; Sunday, Daniel F; Windover, Donald; Kline, R Joseph

2016-01-01

We compare the speed and effectiveness of two genetic optimization algorithms to the results of statistical sampling via a Markov chain Monte Carlo algorithm to find which is the most robust method for determining real space structure in periodic gratings measured using critical dimension small angle X-ray scattering. Both a covariance matrix adaptation evolutionary strategy and differential evolution algorithm are implemented and compared using various objective functions. The algorithms and objective functions are used to minimize differences between diffraction simulations and measured diffraction data. These simulations are parameterized with an electron density model known to roughly correspond to the real space structure of our nanogratings. The study shows that for X-ray scattering data, the covariance matrix adaptation coupled with a mean-absolute error log objective function is the most efficient combination of algorithm and goodness of fit criterion for finding structures with little foreknowledge about the underlying fine scale structure features of the nanograting.

X-ray absorption fine structure and x-ray diffraction studies of crystallographic grains in nanocrystalline FePd:Cu thin films

NASA Astrophysics Data System (ADS)

Krupinski, M.; Perzanowski, M.; Polit, A.; Zabila, Y.; Zarzycki, A.; Dobrowolska, A.; Marszalek, M.

2011-03-01

FePd alloys have recently attracted considerable attention as candidates for ultrahigh density magnetic storage media. In this paper we investigate FePd thin alloy film with a copper admixture composed of nanometer-sized grains. [Fe(0.9 nm)/Pd(1.1 nm)/Cu(d nm)]×5 multilayers were prepared by thermal deposition at room temperature in UHV conditions on Si(100) substrates covered by 100 nm SiO2. The thickness of the copper layer has been changed from 0 to 0.4 nm. After deposition, the multilayers were rapidly annealed at 600 °C in a nitrogen atmosphere, which resulted in the creation of the FePd:Cu alloy. The structure of alloy films obtained this way was determined by x-ray diffraction (XRD), glancing angle x-ray diffraction, and x-ray absorption fine structure (EXAFS). The measurements clearly showed that the L10 FePd:Cu nanocrystalline phase has been formed during the annealing process for all investigated copper compositions. This paper concentrates on the crystallographic grain features of FePd:Cu alloys and illustrates that the EXAFS technique, supported by XRD measurements, can help to extend the information about grain size and grain shape of poorly crystallized materials. We show that, using an appropriate model of the FePd:Cu grains, the comparison of EXAFS and XRD results gives a reasonable agreement.

Triaxial X-Ray Diffraction Method and its Application to Monitor Residual Stress in Surface Layers after High-Feed Milling

NASA Astrophysics Data System (ADS)

Zaušková, Lucia; Czán, Andrej; Šajgalík, Michal; Pobijak, Jozef; Mikloš, Matej

2017-10-01

High-feed milling is a milling method characteristic with shallow depth of cut and high feed rate to maximize the amount of removed metal from a part, generating residual stresses in the surface and subsurface layers of the machined parts. The residual stress has a large influence on the functional properties of the components. The article is focused on the application of triaxial x-ray diffraction method to monitor residual stresses after high feed milling. Significance of triaxial measuring method is the capability of measuring in different angles so it is possible to acquire stress tensor containing normal and shear stress components.

Grafted chromium 13-membered dioxo-macrocyclic complex into aminopropyl-based nanoporous SBA-15

NASA Astrophysics Data System (ADS)

Tarlani, Aliakbar; Joharian, Monika; Narimani, Khashayar; Muzart, Jacques; Fallah, Mahtab

2013-07-01

In a new approach, chromium (III) tetraaza dioxo ligand was grafted onto functionalized SBA-15 after four step reactions by using coordinating ability of anchored amino functionalized SBA-15. After the termination of each step, the obtained product was characterized by FT-IR, low-angle X-ray diffraction (LA-XRD), N2 adsorption-desorption isotherms (Brunauer-Emmett-Teller (BET)-Barret-Joyner-Halenda (BJH)) and thermogravimetric analysis (TGA), and used as catalyst for the efficient and regioselective alcoholysis of styrene oxide to 2-alkoxy-1-phenylethanol product at ambient temperature.

Effect of chlorine in clay-mineral specimens prepared on silver metal-membrane mounts for X-ray powder diffraction analysis

USGS Publications Warehouse

Poppe, L.J.; Commeau, J.A.; Pense, G.M.

1989-01-01

Silver metal-membrane filters are commonly used as substrates in the preparation of oriented clay-mineral specimens for X-ray powder diffraction (XRD). They are relatively unaffected by organic solvent treatments and specimens can be prepared rapidly. The filter mounts are adaptable to automatic sample changers, have few discrete reflections at higher 20 angles, and, because of the high atomic number of silver, produce a relatively low overall background compared with other membrane filters, such as cellulose (Poppe and Hathaway, 1979). The silver metal-membrane filters, however, present some problems after heat treatment if either the filters or the samples contain significant amounts of chlorine. At elevated temperature, the chloride ions react with the silver substrate to form crystalline compounds. These compounds change the mass-absorption coefficient of the sample, reducing peak intensities and areas and, therefore, complicating the semiquantitative estimation of clay minerals. A simple procedure that eliminates most of the chloride from a sample and the silver metal-membrane substrate is presented here.

Transmission Grating and Optics Technology Development for the Arcus Explorer Mission

NASA Astrophysics Data System (ADS)

Heilmann, Ralf; Arcus Team

2018-01-01

Arcus is a high-resolution x-ray spectroscopy MIDEX mission selected for a Phase A concept study. It is designed to explore structure formation through measurements of hot baryon distributions, feedback from black holes, and the formation and evolution of stars, disks, and exoplanet atmospheres. The design provides unprecedented sensitivity in the 1.2-5 nm wavelength band with effective area above 450 sqcm and spectral resolution R > 2500. The Arcus technology is based on 12 m-focal length silicon pore optics (SPO) developed for the European Athena mission, and critical-angle transmission (CAT) x-ray diffraction gratings and x-ray CCDs developed at MIT. The modular design consists of four parallel channels, each channel holding an optics petal, followed by a grating petal. CAT gratings are lightweight, alignment insensitive, high-efficiency x-ray transmission gratings that blaze into high diffraction orders, leading to high spectral resolution. Each optics petal represents an azimuthal sub-aperture of a full Wolter optic. The sub-aperturing effect increases spectral resolving power further. Two CCD readout strips receive photons from each channel, including higher-energy photons in 0th order. Each optics petal holds 34 SPO modules. Each grating petal holds 34 grating windows, and each window holds 4-6 grating facets. A grating facet consists of a silicon grating membrane, bonded to a flexure frame that interfaces with the grating window. We report on a sequence of tests with increasing complexity that systematically increase the Technology Readiness Level (TRL) for the combination of CAT gratings and SPOs towards TLR 6. CAT gratings have been evaluated in x rays for diffraction efficiency (> 30% at 2.5 nm) and for resolving power (R> 10,000). A CAT grating/SPO combination was measured at R ~ 3100 at blaze angles smaller than design values, exceeding Arcus requirements. Efficiency and resolving power were not impacted by vibration and thermal testing of gratings. A pair of large (32 mm x 32 mm) gratings was aligned using laser metrology, and alignment was verified under x rays. We present results on simultaneous illumination of the aligned grating pair, and describe our progress towards further tests.

Explosive vessel for coupling dynamic experiments to the X-ray beam at the Advanced Photon Source

NASA Astrophysics Data System (ADS)

Owens, Charles; Sanchez, Nathaniel; Sorensen, Christian; Jensen, Brian

2017-06-01

Recent experiments at the Advanced Photon Source have been successful in coupling gun systems to the synchrotron to take advantage of the advanced X-ray diagnostics available including X-ray diffraction and X-ray phase contrast imaging (PCI) to examine matter at extreme conditions. There are many experiments that require explosive loading capabilities, e.g. detonator and initiator dynamics, small angle X-ray scattering (SAXS), ejecta formation, and explosively driven flyer experiments. The current work highlights a new explosive vessel that was designed specifically for use at a synchrotron facility with requirements to confine up to 15 grams of explosives (TNT equivalent), couple the vessel to the X-ray beam line, and reliably position samples remotely. A description of the system and capability will be provided along with the results from qualification testing to bring the system into service (LA-UR-17-21381).

Dual-scale rough multifunctional superhydrophobic ITO coatings prepared by air annealing of sputtered indium-tin alloy thin films

NASA Astrophysics Data System (ADS)

Gupta, Nitant; Sasikala, S.; Mahadik, D. B.; Rao, A. V.; Barshilia, Harish C.

2012-10-01

A novel method to fabricate multifunctional indium tin oxide (ITO) coatings is discussed. Superhydrophobic ITO coatings are fabricated by radio frequency balanced magnetron sputter deposition of indium-tin alloy on glass substrates followed by complete oxidation of the samples in air. The chemical nature and structure of the coatings are verified by X-ray diffraction, X-ray photoelectron spectroscopy and micro-Raman spectroscopy. Field emission scanning electron microscopic studies of the coatings display rod-like and blob-like microstructures, together with fractal-like nanostructures infused on top. Microscale roughness of the ITO coatings is measured by three-dimensional profilometry and is found to be in the range of 0.1-3 μm. Thus the presence of micro- and nano- sized structures result in dual-scale roughness. The variation in the contact angle with the deposition time is studied using a contact angle goniometer. High water contact angles (>160°) and low contact angle hysteresis (5°) are obtained at an optimum microscale roughness. The ITO coatings also exhibit other functional properties, such as low sheet resistance and semi-transparent behaviour in the visible region. The loss in the transparency of the ITO coatings is attributed to the presence of higher scale of roughness. The photoluminescence measurements show large photoemission in the visible region. It is expected that further improvements in the multifunctional properties of transparent conducting oxides will open new frontiers in designing novel materials with exotic properties.

Time-resolved structural studies at synchrotrons and X-ray free electron lasers: opportunities and challenges

PubMed Central

Neutze, Richard; Moffat, Keith

2012-01-01

X-ray free electron lasers (XFELs) are potentially revolutionary X-ray sources because of their very short pulse duration, extreme peak brilliance and high spatial coherence, features that distinguish them from today’s synchrotron sources. We review recent time-resolved Laue diffraction and time-resolved wide angle X-ray scattering (WAXS) studies at synchrotron sources, and initial static studies at XFELs. XFELs have the potential to transform the field of time-resolved structural biology, yet many challenges arise in devising and adapting hardware, experimental design and data analysis strategies to exploit their unusual properties. Despite these challenges, we are confident that XFEL sources are poised to shed new light on ultrafast protein reaction dynamics. PMID:23021004

Influence of ceramide on the internal structure and hydration of the phospholipid bilayer studied by neutron and X-ray scattering

NASA Astrophysics Data System (ADS)

Kiselev, M. A.; Zemlyanaya, E. V.; Ryabova, N. Y.; Hauss, T.; Almasy, L.; Funari, S. S.; Zbytovska, J.; Lombardo, D.

2014-07-01

Small angle neutron scattering (SANS), neutron diffraction and X-ray powder diffraction were used to investigate influence of N-stearoyl phytosphingosine (CER[NP]) and α-hydroxy- N-stearoyl phytosphingosine (CER[AP]) on the internal structure and hydration of DMPC membrane in fully and partly hydrated states at T = 30 °C. Application of Fourier analysis for diffraction data and model calculations for the SANS data evidence that addition of both CER[NP] and CER[AP] in small concentrations promotes significant changes in the organization of DMPC bilayers, such as the increase of the hydrophobic core region. SANS data evidence a decrease in the average radius and polydispersity of the vesicles that can be ascribed to hydrogen bonds interactions that favor tight lipid packing with a compact, more rigid character.

Soft X-ray multilayers produced by sputtering and molecular beam epitaxy (MBE) - Substrate and interfacial roughness

NASA Astrophysics Data System (ADS)

Kearney, Patrick A.; Slaughter, J. M.; Powers, K. D.; Falco, Charles M.

1988-01-01

Roughness measurements were made on uncoated silicon wafers and float glass using a WYKO TOPO-3D phase shifting interferometry, and the results are reported. The wafers are found to be slightly smoother than the flat glass. The effects of different cleaning methods and of the deposition of silicon 'buffer layers' on substrate roughness are examined. An acid cleaning method is described which gives more consistent results than detergent cleaning. Healing of the roughness due to sputtered silicon buffer layers was not observed on the length scale probed by the WYKO. Sputtered multilayers are characterized using both the WYKO interferometer and low-angle X-ray diffraction in order to yield information about the roughness of the top surface and of the multilayer interfaces. Preliminary results on film growth using molecular beam epitaxy are also presented.

Off-plane x-ray reflection grating fabrication

NASA Astrophysics Data System (ADS)

Peterson, Thomas J.; DeRoo, Casey T.; Marlowe, Hannah; McEntaffer, Randall L.; Miles, Drew M.; Tutt, James H.; Schultz, Ted B.

2015-09-01

Off-plane X-ray diffraction gratings with precision groove profiles at the submicron scale will be used in next generation X-ray spectrometers. Such gratings will be used on a current NASA suborbital rocket mission, the Off-plane Grating Rocket Experiment (OGRE), and have application for future grating missions. The fabrication of these gratings does not come without challenges. High performance off-plane gratings must be fabricated with precise radial grating patterns, optically at surfaces, and specific facet angles. Such gratings can be made using a series of common micro-fabrication techniques. The resulting process is highly customizable, making it useful for a variety of different mission architectures. In this paper, we detail the fabrication method used to produce high performance off-plane gratings and report the results of a preliminary qualification test of a grating fabricated in this manner. The grating was tested in the off-plane `Littrow' configuration, for which the grating is most efficient for a given diffraction order, and found to achieve 42% relative efficiency in the blaze order with respect to all diffracted light.

Mechanical response of longleaf pine to variation in microfibril angle, chemistry associated wavelengths, density, and radial position

Treesearch

B. K. Via; C. L. So; T. F. Shupe; L. H. Groom; J. Wikaira

2009-01-01

The composite structure of the S2 layer in the wood cell wall is defined by the angle of the cellulose microfibrils and concentration of polymers and this structure impacts strength and stiffness. The objective of this study was to use near infrared spectroscopy and X-ray diffraction to determine the effect of lignin and cellulose associated wavelengths,...

Structural Mineral Physics at Extreme Conditions

NASA Astrophysics Data System (ADS)

Chariton, S.; Dubrovinsky, L. S.; Dubrovinskaia, N.

2017-12-01

Laser heating techniques in diamond anvil cells (DACs) cover a wide pressure-temperature range - above 300 GPa and up to 5000 K. Recent advantages in on-line laser heating techniques resulted in a significant improvement of reliability of in situ X-ray powder diffraction studies in laser-heated DACs, which have become routine at a number of synchrotron facilities including specialized beam-lines at the 3rd generation synchrotrons. However, until recently, existing DAC laser-heating systems could not be used for structural X-ray diffraction studies aimed at structural refinements, i.e. measuring of the diffraction intensities, and not only at determining of lattice parameters. The reason is that in existing DAC laser-heating facilities the laser beam enters the cell at a fixed angle, and a partial rotation of the DAC, as required in monochromatic structural X-ray diffraction experiments, results in a loss of the target crystal and may be even dangerous if the powerful laser light starts to scatter in arbitrary directions by the diamond anvils. In order to overcome this problem we have develop a portable laser heating system and implement it at different diffraction beam lines. We demonstrate the application of this system for simultaneous high-pressure and high-temperature powder and single crystal diffraction studies using examples of studies of chemical and phase relations in the Fe-O system, transition metals carbonates, and silicate perovskites.

Grazing incidence x-ray diffraction analysis of zeolite NaA membranes on porous alumina tubes.

PubMed

Kyotani, Tomohiro

2006-07-01

Zeolite NaA-type membranes hydrothermally synthesized on porous alumina tubes, for dehydration process, were characterized by grazing incidence 2 theta scan X-ray diffraction analysis (GIXRD). The fine structure of the membrane was studied fractionally for surface layer and for materials embedded in the porous alumina tube. The thickness of the surface layer on the porous alumina tube in the membranes used in this study was approximately 2-3 microm as determined from transmission electron microscopy with focused ion beam thin-layer specimen preparation technique (FIB-TEM). To discuss the effects of the membrane surface morphology on the GIXRD measurements, CaA-type membrane prepared by ion exchange from the NaA-type membrane and surface-damaged NaA-type membrane prepared by water leaching were also studied. For the original NaA-type membrane, 2 theta scan GIXRD patterns could be clearly measured at X-ray incidence angles (alpha) ranging from 0.1 to 2.0 deg in increments of 0.1 deg. The surface layers of the 2 - 3 microm on the porous alumina tube correspond to the alpha values up to ca. 0.2 deg. For the CaA-type and the surface-damaged NaA-type membranes, however, diffraction patterns from the surface layer could not be successfully detected and the others were somewhat broad. For all the three samples, diffraction intensities of both zeolite and alumina increased with depth (X-ray incidence angle, alpha) in the porous alumina tube region. The depth profile analysis of the membranes based on the GIXRD first revealed that amount of zeolite crystal embedded in the porous alumina tube is much larger than that in the surface layer. Thus, the 2 theta scan GIXRD is a useful method to study zeolite crystal growth mechanism around (both inside and outside) the porous alumina support during hydrothermal synthesis and to study water permeation behavior in the dehydration process.

Impact of Ion Bombardment on the Structure and Magnetic Properties of Fe78Si13B9 Amorphous Alloy

NASA Astrophysics Data System (ADS)

Wu, Yingwei; Peng, Kun

2018-06-01

Amorphous Fe78Si13B9 alloy ribbons were bombarded by ion beams with different incident angles ( θ ). The evolution of the microstructure and magnetic properties of ribbons caused by ion beam bombardment was investigated by x-ray diffraction, transmission electron microscope and vibrating sample magnetometer analysis. Low-incident-angle bombardment led to atomic migration in the short range, and high-incident-angle bombardment resulted in the crystallization of amorphous alloys. Ion bombardment induces magnetic anisotropy and affects magnetic properties. The effective magnetic anisotropy was determined by applying the law of approach to saturation, and it increased with the increase of the ion bombardment angle. The introduction of effective magnetic anisotropy will reduce the permeability and increase the relaxation frequency. Excellent high-frequency magnetic properties can be obtained by selecting suitable ion bombardment parameters.

Protein crystal structure from non-oriented, single-axis sparse X-ray data

DOE PAGES

Wierman, Jennifer L.; Lan, Ti-Yen; Tate, Mark W.; ...

2016-01-01

X-ray free-electron lasers (XFELs) have inspired the development of serial femtosecond crystallography (SFX) as a method to solve the structure of proteins. SFX datasets are collected from a sequence of protein microcrystals injected across ultrashort X-ray pulses. The idea behind SFX is that diffraction from the intense, ultrashort X-ray pulses leaves the crystal before the crystal is obliterated by the effects of the X-ray pulse. The success of SFX at XFELs has catalyzed interest in analogous experiments at synchrotron-radiation (SR) sources, where data are collected from many small crystals and the ultrashort pulses are replaced by exposure times that aremore » kept short enough to avoid significant crystal damage. The diffraction signal from each short exposure is so `sparse' in recorded photons that the process of recording the crystal intensity is itself a reconstruction problem. Using theEMCalgorithm, a successful reconstruction is demonstrated here in a sparsity regime where there are no Bragg peaks that conventionally would serve to determine the orientation of the crystal in each exposure. In this proof-of-principle experiment, a hen egg-white lysozyme (HEWL) crystal rotating about a single axis was illuminated by an X-ray beam from an X-ray generator to simulate the diffraction patterns of microcrystals from synchrotron radiation. Millions of these sparse frames, typically containing only ~200 photons per frame, were recorded using a fast-framing detector. It is shown that reconstruction of three-dimensional diffraction intensity is possible using theEMCalgorithm, even with these extremely sparse frames and without knowledge of the rotation angle. Further, the reconstructed intensity can be phased and refined to solve the protein structure using traditional crystallographic software. In conclusion, this suggests that synchrotron-based serial crystallography of micrometre-sized crystals can be practical with the aid of theEMCalgorithm even in cases where the data are sparse.« less

Protein crystal structure from non-oriented, single-axis sparse X-ray data

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

Wierman, Jennifer L.; Lan, Ti-Yen; Tate, Mark W.

X-ray free-electron lasers (XFELs) have inspired the development of serial femtosecond crystallography (SFX) as a method to solve the structure of proteins. SFX datasets are collected from a sequence of protein microcrystals injected across ultrashort X-ray pulses. The idea behind SFX is that diffraction from the intense, ultrashort X-ray pulses leaves the crystal before the crystal is obliterated by the effects of the X-ray pulse. The success of SFX at XFELs has catalyzed interest in analogous experiments at synchrotron-radiation (SR) sources, where data are collected from many small crystals and the ultrashort pulses are replaced by exposure times that aremore » kept short enough to avoid significant crystal damage. The diffraction signal from each short exposure is so `sparse' in recorded photons that the process of recording the crystal intensity is itself a reconstruction problem. Using theEMCalgorithm, a successful reconstruction is demonstrated here in a sparsity regime where there are no Bragg peaks that conventionally would serve to determine the orientation of the crystal in each exposure. In this proof-of-principle experiment, a hen egg-white lysozyme (HEWL) crystal rotating about a single axis was illuminated by an X-ray beam from an X-ray generator to simulate the diffraction patterns of microcrystals from synchrotron radiation. Millions of these sparse frames, typically containing only ~200 photons per frame, were recorded using a fast-framing detector. It is shown that reconstruction of three-dimensional diffraction intensity is possible using theEMCalgorithm, even with these extremely sparse frames and without knowledge of the rotation angle. Further, the reconstructed intensity can be phased and refined to solve the protein structure using traditional crystallographic software. In conclusion, this suggests that synchrotron-based serial crystallography of micrometre-sized crystals can be practical with the aid of theEMCalgorithm even in cases where the data are sparse.« less

In situ electrochemical high-energy X-ray diffraction using a capillary working electrode cell geometry

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

Young, Matthias J.; Bedford, Nicholas M.; Jiang, Naisheng

The ability to generate new electrochemically active materials for energy generation and storage with improved properties will likely be derived from an understanding of atomic-scale structure/function relationships during electrochemical events. Here, the design and implementation of a new capillary electrochemical cell designed specifically forin situhigh-energy X-ray diffraction measurements is described. By increasing the amount of electrochemically active material in the X-ray path while implementing low-Zcell materials with anisotropic scattering profiles, an order of magnitude enhancement in diffracted X-ray signal over traditional cell geometries for multiple electrochemically active materials is demonstrated. This signal improvement is crucial for high-energy X-ray diffraction measurementsmore » and subsequent Fourier transformation into atomic pair distribution functions for atomic-scale structural analysis. As an example, clear structural changes in LiCoO 2under reductive and oxidative conditions using the capillary cell are demonstrated, which agree with prior studies. Accurate modeling of the LiCoO 2diffraction data using reverse Monte Carlo simulations further verifies accurate background subtraction and strong signal from the electrochemically active material, enabled by the capillary working electrode geometry.« less

The effect of the cation substitution on the structural and vibrational properties of Cs2NaGaxSc1-xF6 solid solution

NASA Astrophysics Data System (ADS)

Doriguetto, A. C.; Boschi, T. M.; Pizani, P. S.; Mascarenhas, Y. P.; Ellena, J.

2004-08-01

Raman scattering and x-ray diffration were used to characterize the structural and vibrational properties of the Cs2NaGaxSc1-xF6 solid solutions, for x ranging from 0.0 to 1.0. The Raman spectra, taken at room and low temperature, allow us to follow the phase evolution in detail and indicate the breaking of the local symmetry since low Ga concentration levels. Five compositions were studied by x-ray diffraction: x=0.0, 0.2, 0.5, 0.8, and 1.0. A cubic space group, Fm3¯m, was found to x=0.0 and x=0.2 and a trigonal one was found to x=0.5, 0.8, and 1.0. Details of both phases are presented and the correlation between x-ray diffraction and Raman scattering is discussed.

Diffraction leveraged modulation of X-ray pulses using MEMS-based X-ray optics

DOEpatents

Lopez, Daniel; Shenoy, Gopal; Wang, Jin; Walko, Donald A.; Jung, Il-Woong; Mukhopadhyay, Deepkishore

2016-08-09

A method and apparatus are provided for implementing Bragg-diffraction leveraged modulation of X-ray pulses using MicroElectroMechanical systems (MEMS) based diffractive optics. An oscillating crystalline MEMS device generates a controllable time-window for diffraction of the incident X-ray radiation. The Bragg-diffraction leveraged modulation of X-ray pulses includes isolating a particular pulse, spatially separating individual pulses, and spreading a single pulse from an X-ray pulse-train.

Time-dependent gel to gel transformation of a peptide based supramolecular gelator.

PubMed

Baral, Abhishek; Basak, Shibaji; Basu, Kingshuk; Dehsorkhi, Ashkan; Hamley, Ian W; Banerjee, Arindam

2015-06-28

A dipeptide with a long fatty acid chain at its N-terminus gives hydrogels in phosphate buffer in the pH range 7.0-8.5. The hydrogel with a gelator concentration of 0.45% (w/v) at pH 7.46 (physiological pH) provides a very good platform to study dynamic changes within a supramolecular framework as it exhibits remarkable change in its appearance with time. Interestingly, the first formed transparent hydrogel gradually transforms into a turbid gel within 2 days. These two forms of the hydrogel have been thoroughly investigated by using small angle X-ray scattering (SAXS), powder X-ray diffraction (PXRD), field emission scanning electron microscopic (FE-SEM) and high-resolution transmission electron microscopic (HR-TEM) imaging, FT-IR and rheometric analyses. The SAXS and low angle PXRD studies substantiate different packing arrangements for the gelator molecules for these two different gel states (the freshly prepared and the aged hydrogel). Moreover, rheological studies of these two gels reveal that the aged gel is stiffer than the freshly prepared gel.

Study on Iron Distribution and Electrical Activities at Grain Boundaries in Polycrystalline Silicon Substrate for Solar Cells

NASA Astrophysics Data System (ADS)

Arafune, Koji; Ohishi, Eichiro; Sai, Hitoshi; Terada, Yasuko; Ohshita, Yoshio; Yamaguchi, Masafumi

2006-08-01

To clarify the role of grain boundaries in iron sinks and carrier recombination centers, iron distributions and their chemical states were studied before and after gettering. They were measured by the X-ray microprobe fluorescence and the X-ray absorption in the near-edge structure using the beamline 37XU at the SPring-8 third-generation synchrotron facility. To determine the crystallographic orientation of the grain boundaries, electron backscatter diffraction measurements were performed. The distribution of electric active defects was characterized by electron-beam-induced current measurements. Before gettering, the iron was distributed in the small grain and its chemical state was similar to that of iron oxide. After gettering, the iron was redistributed along the small angle grain boundary, and its chemical state was similar to the iron silicide complexed with the iron oxide. Regarding the electrical activity, high carrier recombination was observed along the small-angle grain boundary. On the contrary, Σ 3 grain boundaries were relatively weak impurity sinks and showed low recombination activity.

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

PubMed

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

2015-06-16

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

Mass density images from the diffraction enhanced imaging technique.

PubMed

Hasnah, M O; Parham, C; Pisano, E D; Zhong, Z; Oltulu, O; Chapman, D

2005-02-01

Conventional x-ray radiography measures the projected x-ray attenuation of an object. It requires attenuation differences to obtain contrast of embedded features. In general, the best absorption contrast is obtained at x-ray energies where the absorption is high, meaning a high absorbed dose. Diffraction-enhanced imaging (DEI) derives contrast from absorption, refraction, and extinction. The refraction angle image of DEI visualizes the spatial gradient of the projected electron density of the object. The projected electron density often correlates well with the projected mass density and projected absorption in soft-tissue imaging, yet the mass density is not an "energy"-dependent property of the object, as is the case of absorption. This simple difference can lead to imaging with less x-ray exposure or dose. In addition, the mass density image can be directly compared (i.e., a signal-to-noise comparison) with conventional radiography. We present the method of obtaining the mass density image, the results of experiments in which comparisons are made with radiography, and an application of the method to breast cancer imaging.

Metrology of variable-line-spacing x-ray gratings using the APS Long Trace Profiler

NASA Astrophysics Data System (ADS)

Sheung, Janet; Qian, Jun; Sullivan, Joseph; Thomasset, Muriel; Manton, Jonathan; Bean, Sunil; Takacs, Peter; Dvorak, Joseph; Assoufid, Lahsen

2017-09-01

As resolving power targets have increased with each generation of beamlines commissioned in synchrotron radiation facilities worldwide, diffraction gratings are quickly becoming crucial optical components for meeting performance targets. However, the metrology of variable-line-spacing (VLS) gratings for high resolution beamlines is not widespread; in particular, no metrology facility at any US DOE facility is currently equipped to fully characterize such gratings. To begin to address this issue, the Optics Group at the Advanced Photon Source at Argonne, in collaboration with SOLEIL and with support from Brookhaven National Laboratory (BNL), has developed an alternative beam path addition to the Long Trace Profiler (LTP) at Argonne's Advanced Photon Source. This significantly expands the functionality of the LTP not only to measure mirrors surface slope profile at normal incidence, but also to characterize the groove density of VLS diffraction gratings in the Littrow incidence up to 79°, which covers virtually all diffraction gratings used at synchrotrons in the first order. The LTP light source is a 20mW HeNe laser, which yields enough signal for diffraction measurements to be performed on low angle blazed gratings optimized for soft X-ray wavelengths. We will present the design of the beam path, technical requirements for the optomechanics, and our data analysis procedure. Finally, we discuss challenges still to be overcome and potential limitations with use of the LTP to perform metrology on diffraction gratings.

Small Angle X-Ray Scattering Detector

DOEpatents

Hessler, Jan P.

2004-06-15

A detector for time-resolved small-angle x-ray scattering includes a nearly constant diameter, evacuated linear tube having an end plate detector with a first fluorescent screen and concentric rings of first fiber optic bundles for low angle scattering detection and an annular detector having a second fluorescent screen and second fiber optic bundles concentrically disposed about the tube for higher angle scattering detection. With the scattering source, i.e., the specimen under investigation, located outside of the evacuated tube on the tube's longitudinal axis, scattered x-rays are detected by the fiber optic bundles, to each of which is coupled a respective photodetector, to provide a measurement resolution, i.e., dq/q, where q is the momentum transferred from an incident x-ray to an x-ray scattering specimen, of 2% over two (2) orders of magnitude in reciprocal space, i.e., q.sub.max /q.sub.min.congruent.100.

Development of graphite/copper composites utilizing engineered interfaces. M.S. Thesis Final Report

NASA Technical Reports Server (NTRS)

Devincent, Sandra M.

1991-01-01

In situ measurements of graphite/copper alloy contact angles were made using the sessile drop method. The interfacial energy values obtained from these measurements were then applied to a model for the fiber matrix interfacial debonding phenomenon found in graphite/copper composites. The formation obtained from the sessile drop tests led to the development of a copper alloy that suitably wets graphite. Characterization of graphite/copper alloy interfaces subjected to elevated temperatures was conducted using Scanning Electron Microscopy, Energy Dispersive Spectroscopy, Auger Electron Spectroscopy, and X Ray Diffraction analyses. These analyses indicated that during sessile drop tests conducted at 1130 C for 1 hour, copper alloys containing greater than 0.98 at pct chromium form continuous reaction layers of approx. 10 microns in thickness. The reaction layers are adherent to the graphite surface. The copper wets the reaction layer to form a contact angle of 60 deg or less. X ray diffraction results indicate that the reaction layer is Cr3C2.

Characterization of white poplar and eucalyptus after ionic liquid pretreatment as a function of biomass loading using X-ray diffraction and small angle neutron scattering

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

Yuan, Xueming; Duan, Yonghao; He, Lilin

A systematic study was done to understand interactions among biomass loading during ionic liquid (IL) pretreatment, biomass type and biomass structures. White poplar and eucalyptus samples were pretreated using 1-ethyl-3-methylimidazolium acetate (EmimOAc) at 110 °C for 3 h at biomass loadings of 5, 10, 15, 20 and 25 wt%. All of the samples were chemically characterized and tested for enzymatic hydrolysis. Physical structures including biomass crystallinity and porosity were measured by X-ray diffraction (XRD) and small angle neutron scattering (SANS), respectively. SANS detected pores of radii ranging from ~25 to 625 Å, enabling assessment of contributions of pores with different sizes to increased porositymore » after pretreatment. Contrasting dependences of sugar conversion on white poplar and eucalyptus as a function of biomass loading were observed and cellulose crystalline structure was found to play an important role.« less

Characterization of white poplar and eucalyptus after ionic liquid pretreatment as a function of biomass loading using X-ray diffraction and small angle neutron scattering.

PubMed

Yuan, Xueming; Duan, Yonghao; He, Lilin; Singh, Seema; Simmons, Blake; Cheng, Gang

2017-05-01

A systematic study was performed to understand interactions among biomass loading during ionic liquid (IL) pretreatment, biomass type and biomass structures. White poplar and eucalyptus samples were pretreated using 1-ethyl-3-methylimidazolium acetate (EmimOAc) at 110°C for 3h at biomass loadings of 5, 10, 15, 20 and 25wt%. All of the samples were chemically characterized and tested for enzymatic hydrolysis. Physical structures including biomass crystallinity and porosity were measured by X-ray diffraction (XRD) and small angle neutron scattering (SANS), respectively. SANS detected pores of radii ranging from ∼25 to 625Å, enabling assessment of contributions of pores with different sizes to increased porosity after pretreatment. Contrasting dependences of sugar conversion on white poplar and eucalyptus as a function of biomass loading were observed and cellulose crystalline structure was found to play an important role. Copyright © 2017 Elsevier Ltd. All rights reserved.

In-situ synchrotron wide-angle X-ray diffraction as a rapid method for cocrystal/salt screening.

PubMed

Dong, Pin; Lin, Ling; Li, Yongcheng; Huang, Zhengwei; Lang, Tianqun; Wu, Chuanbin; Lu, Ming

2015-12-30

The purpose of this work was to explore in-situ synchrotron wide-angle X-ray diffraction (WAXD) as a rapid and accurate tool to screen and monitor the formation of cocrystal/salts during heating. The active pharmaceutical ingredients (caffeine, carbamazepine and lamotrigine) were respectively mixed with the coformer (saccharin), and then heated by the hot stage. Real-time process monitoring was performed using synchrotron WAXD to assess cocrystal formation and subsequently compared to differential scanning calorimetry (DSC) measurements. The effect of heating rates and cocrystal growth behavior were investigated. Synchrotron WAXD was fast and sensitive to detect cocrystal formation with the appearance of characteristic diffraction rings, even at the heating rate of 30°C/min, while DSC curves showed overlapped peaks. Unlike the indirect characterization of DSC on endo/exothermic peaks, synchrotron WAXD can directly and qualitatively determine cocrystal by diffraction peaks. The diffraction intensity-temperature curves and the corresponding first-derivative curves clearly exhibited the growth behavior of cocrystal upon heating, providing useful information to optimize the process temperature of hot melt extrusion to continuously manufacture cocrystal. The study suggests that in-situ synchrotron WAXD could provide a one-step process to screen cocrystal at high efficiency and reveal the details of cocrystal/salts growth behavior. Copyright © 2015 Elsevier B.V. All rights reserved.

Facile fabrication of corrosion-resistant superhydrophobic and superoleophilic surfaces with MnWO(4):Dy(3+) microbouquets.

PubMed

Li, Taohai; Li, Quanguo; Yan, Jing; Li, Feng

2014-04-21

Superhydrophobic and superoleophilic MnWO4:Dy(3+) microbouquets were successfully fabricated via a facile hydrothermal process. The surface morphologies and chemical composition were investigated by scanning electron microscopy (SEM) and X-ray powder diffraction (XRD). The wettability of the as-synthesized MnWO4:Dy(3+) microbouquet film was studied by measuring the water contact angle (CA). A static CA for water of 165° and a very low sliding angle (SA) were observed, which were closely related to both the MnWO4:Dy(3+) microbouquet structure and chemical modification. Furthermore, the as-prepared MnWO4:Dy(3+) surface showed superhydrophobicity for some corrosive liquids such as aqueous basic and salt solutions.

Walking peptide on Au(110) surface: Origin and nature of interfacial process

NASA Astrophysics Data System (ADS)

Humblot, V.; Tejeda, A.; Landoulsi, J.; Vallée, A.; Naitabdi, A.; Taleb, A.; Pradier, C.-M.

2014-10-01

IGF tri-peptide adsorption on Au(110)-(1 × 2) under Ultra High Vacuum (UHV) conditions has been investigated using surface science techniques such as synchrotron based Angle Resolved X-ray Photoemission Spectroscopy (AR-PES or AR-XPS), Low Energy Electron Diffraction (LEED) and Scanning Tunnelling Microscopy (STM). The behaviour of IGF molecules has been revealed to be coverage dependent; at low coverage, there is formation of islands presenting a chiral self-organised molecular network with a (4 2, - 3 2) symmetry as shown by Low Energy Electron Diffraction (LEED) and Scanning Tunnelling Microscopy (STM) on the unaltered Au(110)-(1 × 2) reconstruction, suggesting significant intermolecular interactions. When the coverage is increased, the islands grow bigger, and one can observe the disappearance of the self-organised network, along with a remarkable destruction of the (1 × 2) substrate reconstruction, as shown by STM. The effect of IGF on the surface gold atoms has been further confirmed by angle-resolved photoemission measurements which suggest a modification of the electronic states with the (1 × 2) symmetry. The resulting molecular organisation, and overall the gold surface disorganisation, prove a strong surface-molecule interaction, which may be probably be explained by a covalent bonding.

Structural analysis of polymer thin films using GISAXS in the tender X-ray region: Concept and design of GISAXS experiments using the tender X-ray energy at BL-15A2 at the Photon Factory

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

Takagi, H., E-mail: takagih@post.kek.jp; Igarashi, N.; Mori, T.

If small angle X-ray scattering (SAXS) utilizing the soft X-ray region is available, advanced and unique experiments, which differ from traditional SAXS methods, can be realized. For example, grazing-incidence small angle X-ray scattering (GISAXS) using hard X-ray is a powerful tool for understanding the nanostructure in both vertical and lateral directions of thin films, while GISAXS utilizing the tender X-ray region (SX-GISAXS) enables depth-resolved analysis as well as a standard GISAXS analysis in thin films. Thus, at BL-15A2 at the Photon Factory, a dedicated diffractometer for SX-GISAXS (above 2.1 keV) was constructed. This diffractometer is composed of four vacuum chambers andmore » can be converted into the vacuum state from the sample chamber in front of the detector surface. Diffractions are clearly observed until 12th peak when measuring collagen by SAXS with an X-ray energy of 2.40 keV and a camera length of 825 mm. Additionally, we conducted the model experiment using SX-GISAXS with an X-ray energy of 2.40 keV to confirm that a poly(methyl methacrylate)-poly(n-butyl acrylate) block copolymer thin film has a microphase-separated structure in the thin film, which is composed of lamellae aligned both parallel and perpendicular to the substrate surface. Similarly, in a polystyrene-poly(methyl methacrylate) block copolymer thin film, SX-GISAXS with 3.60 keV and 5.73 keV revealed that hexagonally packed cylinders are aligned parallel to the substrate surface. The incident angle dependence of the first order peak position of the q{sub z} direction obtained from experiments at various incident X-ray energies agrees very well with the theoretical one calculated from the distorted wave Born approximation.« less

Surface and grain boundary interdiffusion in nanometer-scale LSMO/BFO bilayer

NASA Astrophysics Data System (ADS)

Kumar, Virendra; Gaur, Anurag; Choudhary, R. J.; Gupta, Mukul

2016-05-01

Epitaxial 150 nm thick LSMO/BFO bilayer is deposited on STO (100) substrate by pulsed laser deposition, to study magnetoelectric effect. Unexpected low value of room temperature magnetization in bilayer indicates towards the possibility of interdiffusion. Further, sharp fall in the value of TC (53 K) also added our anxiety towards possible interdiffusion in BFO/LSMO system. Low-angle x-ray diffraction technique is used to investigate interdiffusion phenomena, and the temperature-dependent interdiffusivity is obtained by accurately monitoring the decay of the first-order modulation peak as a function of annealing time. It has been found that the diffusivity at different temperatures follows Arrhenius-type behavior. X-ray reflection (XRR) pattern obtained for the bilayer could not be fitted in the Parratt's formalism, which confirms the interdiffusion in it. Depth profiles of 209Bi, 56Fe ions measured by secondary ion mass spectroscope (SIMS) further substantiate the diffusion of these ions from upper BFO layer into lower LSMO layer.

X-ray diffraction evidence for myelin disorder in brain from humans with Alzheimer's disease.

PubMed

Chia, L S; Thompson, J E; Moscarello, M A

1984-09-05

Wide-angle X-ray diffraction studies revealed that the lipid phase transition temperature of myelin from brain tissue of humans with Alzheimer's disease was about 12 degrees C lower than that of normal age-matched controls, indicating differences in the physical organization of the myelin lipid bilayer. Elevated levels of malondialdehyde and conjugated diene were found in brain tissue from humans with Alzheimer's disease, indicating an increased amount of lipid peroxidation over the controls. An increase in myelin disorder and in lipid peroxidation can both be correlated with aging in human brain, but the changes in myelin from humans with Alzheimer's disease are more pronounced than in normal aging. These changes might represent severe or accelerated aging.

Evidence of monotropic hexatic tilted smectic phase in the phase sequence of ferroelectric liquid crystal

NASA Astrophysics Data System (ADS)

Różycka, Anna; Deptuch, Aleksandra; Jaworska-Gołąb, Teresa; Węgłowska, Dorota; Marzec, Monika

2018-02-01

Physical properties of a new ferroelectric liquid crystal have been studied by complementary methods: differential scanning calorimetry, polarizing optical microscopy, dielectric and X-ray diffraction. It was found that next to enantiotropic ferroelectric smectic C* phase, the monotropic smectic phase appears at cooling. X-ray diffraction measurements allowed to identify this phase as hexatic tilted smectic. Temperature dependence of spontaneous polarization, tilt angle of molecules and switching time were found in both liquid crystalline phases at cooling. Based on the dielectric results, the dielectric processes were identified as Goldstone mode in the smectic C* phase, whereas as the bond-orientation-like phason and the bulk domain mode in the monotropic hexatic tilted smectic phase.

Rotator Phases of n-Heptane under High Pressure: Raman Scattering and X-ray Diffraction Studies

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

C Ma; Q Zhou; F Li

2011-12-31

We performed high-pressure Raman scattering and angle-dispersive synchrotron X-ray diffraction measurements on n-heptane at room temperature. It has been found that n-heptane undergoes a liquid to rotator phase III (R{sub III}) transition at 1.2 GPa and then transforms into another rotator phase R{sub IV} at about 3 GPa. As the pressure reaches 7.5 GPa, a transition from an orientationally disordered R{sub IV} phase to an ordered crystalline state starts and is completed around 14.5 GPa. Our results clearly present the high-pressure phase transition sequence (liquid-R{sub III}-R{sub IV}-crystal) of n-heptane, similar to that of normal alkanes.

Spider Silk: From Protein-Rich Gland Fluids to Diverse Biopolymer Fibers

DTIC Science & Technology

2016-01-06

characterize the protein-rich fluid in the various spider silk producing glands. We have been using a battery of magnetic resonance methods including...solution and solid-state nuclear magnetic resonance (NMR) and micro imaging (MRI) in combination with wide angle and small angle X-ray diffraction...range of magnetic resonance methods. We successfully developed magnetic resonance imaging (MRI) techniques with localized spectroscopy to probe the silk

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

Berenguer de la Cuesta, Felisa; Wenger, Marco P.E.; Bean, Richard J.

Coherent X-ray diffraction has been applied in the imaging of inorganic materials with great success. However, its application to biological specimens has been limited to some notable exceptions, due to the induced radiation damage and the extended nature of biological samples, the last limiting the application of most part of the phasing algorithms. X-ray ptychography, still under development, is a good candidate to overcome such difficulties and become a powerful imaging method for biology. We describe herein the feasibility of applying ptychography to the imaging of biological specimens, in particular collagen rich samples. We report here speckles in diffraction patternsmore » from soft animal tissue, obtained with an optimized small angle X-ray setup that exploits the natural coherence of the beam. By phasing these patterns, dark field images of collagen within tendon, skin, bone, or cornea will eventually be obtained with a resolution of 60-70 nm. We present simulations of the contrast mechanism in collagen based on atomic force microscope images of the samples. Simulations confirmed the 'speckled' nature of the obtained diffraction patterns. Once inverted, the patterns will show the disposition and orientation of the fibers within the tissue, by enhancing the phase contrast between protein and no protein regions of the sample. Our work affords the application of the most innovative coherent X-ray diffraction tools to the study of biological specimens, and this approach will have a significant impact in biology and medicine because it overcomes many of the limits of current microscopy techniques.« less

Comparative properties of cellulose nano-crystals from native and mercerized cotton fibers

USDA-ARS?s Scientific Manuscript database

Stable aqueous suspensions of cellulose nano-crystals (CNCs) were fabricated from both native and mercerized cotton fibers by sulfuric acid hydrolysis, followed by high-pressure homogenization. Fourier Transform Infrared Spectrometry and Wide-angle X-Ray Diffraction data showed that the fibers had b...

Ionic depletion at the crystalline Gibbs layer of PEG-capped gold nanoparticle brushes at aqueous surfaces

NASA Astrophysics Data System (ADS)

Wang, Wenjie; Zhang, Honghu; Mallapragada, Surya; Travesset, Alex; Vaknin, David

2017-12-01

In situ surface-sensitive x-ray diffraction and grazing incidence x-ray fluorescence spectroscopy (GIXFS) methods are combined to determine the ionic distributions across the liquid/vapor interfaces of thiolated-polyethylene-glycol-capped gold nanoparticle (PEG-AuNP) solutions. Induced by the addition of salts (i.e., Cs2SO4 ) to PEG-AuNPs solutions, two-dimensional hexagonal lattices of PEG-AuNPs form spontaneously at the aqueous surfaces, as is demonstrated by x-ray reflectivity and grazing incidence small-angle x-ray scattering. By taking advantage of element specificity with the GIXFS method, we find that the cation Cs+ concentration at the crystalline film is significantly reduced in parts of the PEG-AuNP film compared with that in the bulk.

An instrument for 3D x-ray nano-imaging

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

Holler, M.; Raabe, J.; Diaz, A.

We present an instrument dedicated to 3D scanning x-ray microscopy, allowing a sample to be precisely scanned through a beam while the angle of x-ray incidence can be changed. The position of the sample is controlled with respect to the beam-defining optics by laser interferometry. The instrument achieves a position stability better than 10 nm standard deviation. The instrument performance is assessed using scanning x-ray diffraction microscopy and we demonstrate a resolution of 18 nm in 2D imaging of a lithographic test pattern while the beam was defined by a pinhole of 3 {mu}m in diameter. In 3D on amore » test object of copper interconnects of a microprocessor, a resolution of 53 nm is achieved.« less

Combined synchrotron X-ray tomography and X-ray powder diffraction using a fluorescing metal foil.

PubMed

Kappen, P; Arhatari, B D; Luu, M B; Balaur, E; Caradoc-Davies, T

2013-06-01

This study realizes the concept of simultaneous micro-X-ray computed tomography and X-ray powder diffraction using a synchrotron beamline. A thin zinc metal foil was placed in the primary, monochromatic synchrotron beam to generate a divergent wave to propagate through the samples of interest onto a CCD detector for tomographic imaging, thus removing the need for large beam illumination and high spatial resolution detection. Both low density materials (kapton tubing and a piece of plant) and higher density materials (Egyptian faience) were investigated, and elemental contrast was explored for the example of Cu and Ni meshes. The viability of parallel powder diffraction using the direct beam transmitted through the foil was demonstrated. The outcomes of this study enable further development of the technique towards in situ tomography∕diffraction studies combining micrometer and crystallographic length scales, and towards elemental contrast imaging and reconstruction methods using well defined fluorescence outputs from combinations of known fluorescence targets (elements).

Outrunning damage: Electrons vs X-rays—timescales and mechanisms

PubMed Central

Spence, John C. H.

2017-01-01

Toward the end of his career, Zewail developed strong interest in fast electron spectroscopy and imaging, a field to which he made important contributions toward his aim of making molecular movies free of radiation damage. We therefore compare here the atomistic mechanisms leading to destruction of protein samples in diffract-and-destroy experiments for the cases of high-energy electron beam irradiation and X-ray laser pulses. The damage processes and their time-scales are compared and relevant elastic, inelastic, and photoelectron cross sections are given. Inelastic mean-free paths for ejected electrons at very low energies in insulators are compared with the bioparticle size. The dose rate and structural damage rate for electrons are found to be much lower, allowing longer pulses, reduced beam current, and Coulomb interactions for the formation of smaller probes. High-angle electron scattering from the nucleus, which has no parallel in the X-ray case, tracks the slowly moving nuclei during the explosion, just as the gain of the XFEL (X-ray free-electron laser) has no parallel in the electron case. Despite reduced damage and much larger elastic scattering cross sections in the electron case, leading to not dissimilar elastic scattering rates (when account is taken of the greatly increased incident XFEL fluence), progress for single-particle electron diffraction is seen to depend on the effort to reduce emittance growth due to Coulomb interactions, and so allow formation of intense sub-micron beams no larger than a virus. PMID:28653018

Single photon energy dispersive x-ray diffraction

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

Higginbotham, Andrew; Patel, Shamim; Ciricosta, Orlando

2014-03-15

With the pressure range accessible to laser driven compression experiments on solid material rising rapidly, new challenges in the diagnosis of samples in harsh laser environments are emerging. When driving to TPa pressures (conditions highly relevant to planetary interiors), traditional x-ray diffraction techniques are plagued by increased sources of background and noise, as well as a potential reduction in signal. In this paper we present a new diffraction diagnostic designed to record x-ray diffraction in low signal-to-noise environments. By utilising single photon counting techniques we demonstrate the ability to record diffraction patterns on nanosecond timescales, and subsequently separate, photon-by-photon, signalmore » from background. In doing this, we mitigate many of the issues surrounding the use of high intensity lasers to drive samples to extremes of pressure, allowing for structural information to be obtained in a regime which is currently largely unexplored.« less

Real-time x-ray diffraction measurements of shocked polycrystalline tin and aluminum.

PubMed

Morgan, Dane V; Macy, Don; Stevens, Gerald

2008-11-01

A new, fast, single-pulse x-ray diffraction (XRD) diagnostic for determining phase transitions in shocked polycrystalline materials has been developed. The diagnostic consists of a 37-stage Marx bank high-voltage pulse generator coupled to a needle-and-washer electron beam diode via coaxial cable, producing line and bremsstrahlung x-ray emission in a 35 ns pulse. The characteristic K(alpha) lines from the selected anodes of silver and molybdenum are used to produce the diffraction patterns, with thin foil filters employed to remove the characteristic K(beta) line emission. The x-ray beam passes through a pinhole collimator and is incident on the sample with an approximately 3 x 6 mm(2) spot and 1 degrees full width half maximum angular divergence in a Bragg-reflecting geometry. For the experiments described in this report, the angle between the incident beam and the sample surface was 8.5 degrees . A Debye-Scherrer diffraction image was produced on a phosphor located 76 mm from the polycrystalline sample surface. The phosphor image was coupled to a charge-coupled device camera through a coherent fiber-optic bundle. Dynamic single-pulse XRD experiments were conducted with thin foil samples of tin, shock loaded with a 1 mm vitreous carbon back window. Detasheet high explosive with a 2-mm-thick aluminum buffer was used to shock the sample. Analysis of the dynamic shock-loaded tin XRD images revealed a phase transformation of the tin beta phase into an amorphous or liquid state. Identical experiments with shock-loaded aluminum indicated compression of the face-centered-cubic aluminum lattice with no phase transformation.

Vibrational cross-angles in condensed molecules: a structural tool.

PubMed

Chen, Hailong; Zhang, Yufan; Li, Jiebo; Liu, Hongjun; Jiang, De-En; Zheng, Junrong

2013-09-05

The fluctuations of three-dimensional molecular conformations of a molecule in different environments play critical roles in many important chemical and biological processes. X-ray diffraction (XRD) techniques and nuclear magnetic resonance (NMR) methods are routinely applied to monitor the molecular conformations in condensed phases. However, some special requirements of the methods have prevented them from exploring many molecular phenomena at the current stage. Here, we introduce another method to resolve molecular conformations based on an ultrafast MIR/T-Hz multiple-dimensional vibrational spectroscopic technique. The model molecule (4'-methyl-2'-nitroacetanilide, MNA) is prepared in two of its crystalline forms and liquid samples. Two polarized ultrafast infrared pulses are then used to determine the cross-angles of vibrational transition moment directions by exciting one vibrational band and detecting the induced response on another vibrational band of the molecule. The vibrational cross-angles are then converted into molecular conformations with the aid of calculations. The molecular conformations determined by the method are supported by X-ray diffraction and molecular dynamics simulation results. The experimental results suggest that thermodynamic interactions with solvent molecules are not altering the molecular conformations of MNA in the solutions to control their ultimate conformations in the crystals.

Multiple image x-radiography for functional lung imaging

NASA Astrophysics Data System (ADS)

Aulakh, G. K.; Mann, A.; Belev, G.; Wiebe, S.; Kuebler, W. M.; Singh, B.; Chapman, D.

2018-01-01

Detection and visualization of lung tissue structures is impaired by predominance of air. However, by using synchrotron x-rays, refraction of x-rays at the interface of tissue and air can be utilized to generate contrast which may in turn enable quantification of lung optical properties. We utilized multiple image radiography, a variant of diffraction enhanced imaging, at the Canadian light source to quantify changes in unique x-ray optical properties of lungs, namely attenuation, refraction and ultra small-angle scatter (USAXS or width) contrast ratios as a function of lung orientation in free-breathing or respiratory-gated mice before and after intra-nasal bacterial endotoxin (lipopolysaccharide) instillation. The lung ultra small-angle scatter and attenuation contrast ratios were significantly higher 9 h post lipopolysaccharide instillation compared to saline treatment whereas the refraction contrast decreased in magnitude. In ventilated mice, end-expiratory pressures result in an increase in ultra small-angle scatter contrast ratio when compared to end-inspiratory pressures. There were no detectable changes in lung attenuation or refraction contrast ratio with change in lung pressure alone. In effect, multiple image radiography can be applied towards following optical properties of lung air-tissue barrier over time during pathologies such as acute lung injury.

PSICHE: a new beamline dedicated to X-ray diffraction and tomography at high pressure at synchrotron SOLEIL

NASA Astrophysics Data System (ADS)

Guignot, N.; Itié, J.; Zerbino, P.; Delmotte, A.; Moreno, T.

2013-12-01

The PSICHE beamline (for 'Pressure, Structure and Imaging by Contrast at High Energy') is a new facility opened for high pressure experiments at synchrotron SOLEIL (St-Aubin, France). With its source, optics, detectors and 3 experimental stations, it can handle a large variety of experimental setups. High energy photons are produced with an in-vacuum wiggler. The white beam obtained, with photons energy ranging continuously from 15 to 80 keV (from a 2.75 GeV machine), is used on the first experimental station for energy dispersive X-ray diffraction (EDX) measurements using different pressure cells. The main setup is a 1200 tons load capacity multi-anvil press featuring a (100) DIA compression module with a 15° horizontal aperture, allowing measurements up to 30° in 2theta by rotating the press. Other setups are a Paris-Edinburgh (PE) large volume press and diamond anvil cells (DACs). On the detection side we have a rotating Ge detector, based on the CAESAR design described by Wang et al. (2004) (combination of EDX and angular dispersive X-ray diffraction, ADX). One of the difficulties when building such setups is the rotation mechanism which cannot be physically attached to the rotation axis, potentially leading to large circle of confusions on the horizontal position of this axis. Thanks to translation corrections done at each angle step, the circle of confusion is minimized to 3x6 μm2 along the 35° travel, making possible measurements on very small objects. Combining EDX and ADX has a lot of advantages and we will present our first results obtained using this setup. The PSICHE focusing optics and monochromator are also used to focus monochromatic beams (up to 52 keV) on 2 different experimental stations. The first focal point at 31 m gives a beam size of 100x50 μm2 (HxV) and is useful for low pressure experiments and experiments done with the PE press associated with Soller slits. A PerkinElmer flatpanel detector can be precisely scanned in 3 directions, making ADX measurements at the highest possible resolution on this beamline. This station will also be used for diffraction tomography experiments. The second focal point at 37.6 m is located behind KB mirrors on the third experimental station. 10x10 μm2 beam sizes (full width) are expected. This station will be used for DAC experiments, with or without our future laser heating setup. Finally, parallel beams can be produced with sizes up to 15x5 mm2 (HxV) for tomography experiments, in pink (filtered white) beam or monochromatic beam. We plan to use rotating anvils presses such as the rotoPEc (J. Philippe et al., 2013) to take full advantage of this beam mode, but it can be opened to other techniques. The PSICHE beamline is opened for users since July 2013. Some stations are not available yet, and will be opened through 2014 and 2015. References X. Dong et al., Ray tracing application in hard x-ray optical development: Soleil first wiggler beamline (PSICHÉ) case" (2011), Proc. SPIE 8141, 814113 Y. Wang et al., A new technique for angle-dispersive powder diffraction using an energy-dispersive setup and synchrotron radiation (2004), J. Appl. Cryst. 37, 947-956 J. Philippe, Y. Le Godec, F. Bergame et M. Morand, Patent INPI 11 62335 (2013)

a-Si:H TFT-silicon hybrid low-energy x-ray detector

DOE PAGES

Shin, Kyung -Wook; Karim, Karim S.

2017-03-15

Direct conversion crystalline silicon X-ray imagers are used for low-energy X-ray photon (4-20 keV) detection in scientific research applications such as protein crystallography. In this paper, we demonstrate a novel pixel architecture that integrates a crystalline silicon X-ray detector with a thin-film transistor amorphous silicon pixel readout circuit. We describe a simplified two-mask process to fabricate a complete imaging array and present preliminary results that show the fabricated pixel to be sensitive to 5.89-keV photons from a low activity Fe-55 gamma source. Furthermore, this paper presented can expedite the development of high spatial resolution, low cost, direct conversion imagers formore » X-ray diffraction and crystallography applications.« less

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

High-resolution study of dynamical diffraction phenomena accompanying the Renninger (222/113) case of three-beam diffraction in silicon

PubMed Central

Kazimirov, A.; Kohn, V. G.

2010-01-01

X-ray optical schemes capable of producing a highly monochromatic beam with high angular collimation in both the vertical and horizontal planes have been evaluated and utilized to study high-resolution diffraction phenomena in the Renninger (222/113) case of three-beam diffraction in silicon. The effect of the total reflection of the incident beam into the nearly forbidden reflected beam was observed for the first time with the maximum 222 reflectivity at the 70% level. We have demonstrated that the width of the 222 reflection can be varied many times by tuning the azimuthal angle by only a few µrad in the vicinity of the three-beam diffraction region. This effect, predicted theoretically more than 20 years ago, is explained by the enhancement of the 222 scattering amplitude due to the virtual two-stage 000 113 222 process which depends on the azimuthal angle. PMID:20555185

Synthesis and synchrotron characterisation of novel dual-template of hydroxyapatite scaffolds with controlled size porous distribution

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

Lima, Thiago A. R. M.; Ilavsky, Jan; Hammons, Joshua

Hydroxyapatite (HAP) scaffolds with a hierarchical porous architecture were prepared by a new dual-template (corn starch and cetyltrimethylammonium bromide (CTAB) surfactant) used to cast HAP nanoparticles and development scaffolds with size hierarchical porous distribution. The Powder X-Ray diffraction (XRD) results showed that only the HAP crystalline phase is present in the samples after calcination; the Scanning Electron Microscopy (SEM) combined with Small Angle (SAXS) and Ultra-Small Angle X-ray Scattering (USAXS) techniques showed that the porous arrangement is promoted by needle-like HAP nanoparticles, and that the pore size distributions depend on the drip-order of the calcium and the phosphate solutions duringmore » the template preparation stage.« less

Calcium phosphate coatings modified with zinc- or copper- incorporation on Ti-40Nb alloy

NASA Astrophysics Data System (ADS)

Komarova, E. G.; Sedelnikova, M. B.; Sharkeev, Yu P.; Kazakbaeva, A. A.; Glukhov, I. A.; Khimich, M. A.

2017-05-01

The influence of the microarc oxidation parameters and electrolyte composition on the structure, properties and composition of CaP coatings modified with Zn- or Cu- incorporation on the Ti-40mas.%Nb (Ti-40Nb) alloy was investigated. The linear growth of thickness, roughness, and size of structural elements with process voltage increasing has been revealed. It was shown that the CaP coatings have the low contact angles with liquids and, consequently, high free surface energy. This indicates a high hydrophilicity of the coatings. X-ray diffraction analysis showed that the coatings have X-ray amorphous structure. The increase of the process voltage leads to the formation of such crystalline phases as CaHPO4 and β-Ca2P2O7 in the coatings. The maximum Ca/P atomic ratio was equal to 0.4, and Zn or Cu contents was equal to 0.3 or 0.2 at.%, respectively.

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

Willey, Trevor M.; Lauderbach, Lisa; Gagliardi, Franco

HMX-based explosives LX-10 and PBX-9501 were heated through the β-δ phase transition. Ultra-small angle x-ray scattering (USAXS) and molecular diffraction were simultaneously recorded as the HMX was heated. Mesoscale voids and structure dramatically change promptly with the β-δ phase transition, rather than with other thermal effects. Also, x-ray induced damage, observed in the USAXS, occurs more readily at elevated temperatures; as such, the dose was reduced to mitigate this effect. Optical microscopy performed during a similar heating cycle gives an indication of changes on longer length scales, while x-ray microtomography, performed before and after heating, shows the character of extensivemore » microstructural damage resulting from the temperature cycle and solid-state phase transition.« less

Sealed-tube synthesis and phase diagram of Li{sub x}TiS{sub 2} (0 ≤ x ≤1)

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

Zhang, Ziping; National Laboratory for Superconductivity, Institute of Physics, Chinese Academy of Science, Beijing 100190; Dong, Cheng, E-mail: chengdon@aphy.iphy.ac.cn

2015-01-15

Graphical abstract: We reported a new method to prepare Li{sub x}TiS{sub 2} (0 ≤ x ≤ 1) at 600 °C in sealed tube using Li{sub 2}S aslithium source. A schematic phase diagram of the Li{sub x}TiS{sub 2} system has been constructed based on the DTA and XRD data. - Abstract: We reported a new method to prepare Li{sub x}TiS{sub 2} (0 ≤ x ≤ 1) at 600 °C in sealed tube using Li{sub 2}S as lithium source. The Li{sub x}TiS{sub 2} samples were characterized by powder X-ray diffraction, scanning electron microscopy, energy dispersive X-ray spectroscopy, and differential thermal analysis. Themore » variations of the lattice parameters with lithium content x in Li{sub x}TiS{sub 2} were determined by X-ray powder diffraction analysis for both 1T and 3R phases. The phase transition between low-temperature 1T phase and high-temperature 3R phase was confirmed by the powder X-ray diffraction analysis. Based on the differential thermal analysis and X-ray diffraction results, a schematic phase diagram of the Li{sub x}TiS{sub 2} system has been constructed, providing a guideline to synthesize Li{sub x}TiS{sub 2} in 1T structure or 3R structure.« less

The structure of biocoats based on TiO2 doped with nitrogen study

NASA Astrophysics Data System (ADS)

Boytsova, E. L.; Leonova, L. A.; Pichugin, V. F.

2018-04-01

Nitrogen-doped titanium dioxide (N-TiO2) nanofilms were deposited by reactive magnetron sputtering under different bias voltage. The mode of sputtering influences to formation and properties of titanium films. X-ray diffraction (XRD) was used to study the phase transition and crystallinity of the nanofilms. A technique of layer-by-layer measurement of Raman scattering from nanostructured titanium dioxide films based on a preliminary sputtering of the films by argon beam under an angle of 45° and less has been developed. Experimentally confirmed low dissolution rate of the coating in NaCl saline (0.9%).

Synthesis on structure and properties of zinc nanocrystal in high ordered 3D nanostructures

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

Sathyaseelan, B., E-mail: bsseelan03@gmail.com; Manigandan, A.; Anbarasu, V.

2015-06-24

The wet impregnation method was employed to prepare ZnO encapsulated in mesoporous silica (ZnO/KIT-6). The prepared ZnO/KIT-6 samples have been studied by X-ray diffraction, transmission electron microscope, and nitrogen adsorption–desorption isotherm. The low angle powder XRD patterns of Calcined ZnO/KIT-6 materials showed a phase that can be indexed to cubic Ia3d. Tem images revealed well ordered cubic 3D nanoporous chennels. The ZnO encapsulated in KIT-6 can be used as light-emitting diodes and ultraviolet nanolasers.

Experimental evidences for molecular origin of low-Q peak in neutron/x-ray scattering of 1-alkyl-3-methylimidazolium bis(trifluoromethanesulfonyl)amide ionic liquids

NASA Astrophysics Data System (ADS)

Fujii, Kenta; Kanzaki, Ryo; Takamuku, Toshiyuki; Kameda, Yasuo; Kohara, Shinji; Kanakubo, Mitsuhiro; Shibayama, Mitsuhiro; Ishiguro, Shin-ichi; Umebayashi, Yasuhiro

2011-12-01

Short- and long-range liquid structures of [CnmIm+][TFSA-] with n = 2, 4, 6, 8, 10, and 12 have been studied by high-energy x-ray diffraction (HEXRD) and small-angle neutron scattering (SANS) experiments with the aid of MD simulations. Observed x-ray structure factor, S(Q), for the ionic liquids with the alkyl-chain length n > 6 exhibited a characteristic peak in the low-Q range of 0.2-0.4 Å -1, indicating the heterogeneity of their ionic liquids. SANS profiles IH(Q) and ID(Q) for the normal and the alkyl group deuterated ionic liquids, respectively, showed significant peaks for n = 10 and 12 without no form factor component for large spherical or spheroidal aggregates like micelles in solution. The peaks for n = 10 and 12 evidently disappeared in the difference SANS profiles ΔI(Q) [=ID(Q) - IH(Q)], although that for n = 12 slightly remained. This suggests that the long-range correlations originated from the alkyl groups hardly contribute to the low-Q peak intensity in SANS. To reveal molecular origin of the low-Q peak, we introduce here a new function; x-ray structure factor intensity at a given Q as a function of r, SQpeak(r). The SQpeak(r) function suggests that the observed low-Q peak intensity depending on n is originated from liquid structures at two r-region of 5-8 and 8-15 Å for all ionic liquids examined except for n = 12. Atomistic MD simulations are consistent with the HEXRD and SANS experiments, and then we discussed the relationship between both variations of low-Q peak and real-space structure with lengthening the alkyl group of the CnmIm.

CARNAÚBA: The Coherent X-Ray Nanoprobe Beamline for the Brazilian Synchrotron SIRIUS/LNLS

NASA Astrophysics Data System (ADS)

Tolentino, Hélio C. N.; Soares, Márcio M.; Perez, Carlos A.; Vicentin, Flávio C.; Abdala, Dalton B.; Galante, Douglas; Teixeira, Verônica de C.; de Araújo, Douglas H. C.; Westfahl, Harry, Jr.

2017-06-01

The CARNAÚBA beamline is the tender-to-hard X-ray (2 - 15 keV) scanning nanoprobe planned for the 4th generation storage ring SIRIUS at the LNLS. CARNAÚBA uses an undulator source with vertical linear polarization in a low-beta straight section and grazing incidence-focusing mirrors to create a nanoprobe at 143 m from the source. The beamline optic is based on KB mirrors and provides high brilliance at an achromatic focal spot down to the diffraction limit diameter of ˜30 nm with a working distance of ˜6 cm. These characteristics are crucial for studying nanometric samples in experiments involving complex stages and environments. The CARNAÚBA beamline aims to perform raster scans using x-ray fluorescence, x-ray absorption spectroscopy, x-ray diffraction and coherent x-ray imaging techniques. Computed tomography will extend these methods to three dimensions.

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.

Design of a multilayer-based collimated plane-grating monochromator for tender X-ray range.

PubMed

Yang, Xiaowei; Wang, Hongchang; Hand, Matthew; Sawhney, Kawal; Kaulich, Burkhard; Kozhevnikov, Igor V; Huang, Qiushi; Wang, Zhanshan

2017-01-01

Collimated plane-grating monochromators (cPGMs), consisting of a plane mirror and plane diffraction grating, are essential optics in synchrotron radiation sources for their remarkable flexibility and good optical characteristics in the soft X-ray region. However, the poor energy transport efficiency of a conventional cPGM (single-layer-coated) degrades the source intensity and leaves reduced flux at the sample, especially for the tender X-ray range (1-4 keV) that covers a large number of K- and L-edges of medium-Z elements, and M-edges of high-Z elements. To overcome this limitation, the use of a multilayer-based cPGM is proposed, combining a multilayer-coated plane mirror with blazed multilayer gratings. With this combination, the effective efficiency of cPGMs can be increased by an order of magnitude compared with the conventional single-layer cPGMs. In addition, higher resolving power can be achieved with improved efficiency by increasing the blaze angle and working at higher diffraction order.

Design of a multilayer-based collimated plane-grating monochromator for tender X-ray range

PubMed Central

Yang, Xiaowei; Wang, Hongchang; Hand, Matthew; Sawhney, Kawal; Kaulich, Burkhard; Kozhevnikov, Igor V.; Huang, Qiushi; Wang, Zhanshan

2017-01-01

Collimated plane-grating monochromators (cPGMs), consisting of a plane mirror and plane diffraction grating, are essential optics in synchrotron radiation sources for their remarkable flexibility and good optical characteristics in the soft X-ray region. However, the poor energy transport efficiency of a conventional cPGM (single-layer-coated) degrades the source intensity and leaves reduced flux at the sample, especially for the tender X-ray range (1–4 keV) that covers a large number of K- and L-edges of medium-Z elements, and M-edges of high-Z elements. To overcome this limitation, the use of a multilayer-based cPGM is proposed, combining a multilayer-coated plane mirror with blazed multilayer gratings. With this combination, the effective efficiency of cPGMs can be increased by an order of magnitude compared with the conventional single-layer cPGMs. In addition, higher resolving power can be achieved with improved efficiency by increasing the blaze angle and working at higher diffraction order. PMID:28009556

Reintroducing electrostatics into macromolecular crystallographic refinement: application to neutron crystallography and DNA hydration.

PubMed

Fenn, Timothy D; Schnieders, Michael J; Mustyakimov, Marat; Wu, Chuanjie; Langan, Paul; Pande, Vijay S; Brunger, Axel T

2011-04-13

Most current crystallographic structure refinements augment the diffraction data with a priori information consisting of bond, angle, dihedral, planarity restraints, and atomic repulsion based on the Pauli exclusion principle. Yet, electrostatics and van der Waals attraction are physical forces that provide additional a priori information. Here, we assess the inclusion of electrostatics for the force field used for all-atom (including hydrogen) joint neutron/X-ray refinement. Two DNA and a protein crystal structure were refined against joint neutron/X-ray diffraction data sets using force fields without electrostatics or with electrostatics. Hydrogen-bond orientation/geometry favors the inclusion of electrostatics. Refinement of Z-DNA with electrostatics leads to a hypothesis for the entropic stabilization of Z-DNA that may partly explain the thermodynamics of converting the B form of DNA to its Z form. Thus, inclusion of electrostatics assists joint neutron/X-ray refinements, especially for placing and orienting hydrogen atoms. Copyright © 2011 Elsevier Ltd. All rights reserved.

Reintroducing Electrostatics into Macromolecular Crystallographic Refinement: Application to Neutron Crystallography and DNA Hydration

PubMed Central

Fenn, Timothy D.; Schnieders, Michael J.; Mustyakimov, Marat; Wu, Chuanjie; Langan, Paul; Pande, Vijay S.; Brunger, Axel T.

2011-01-01

Summary Most current crystallographic structure refinements augment the diffraction data with a priori information consisting of bond, angle, dihedral, planarity restraints and atomic repulsion based on the Pauli exclusion principle. Yet, electrostatics and van der Waals attraction are physical forces that provide additional a priori information. Here we assess the inclusion of electrostatics for the force field used for all-atom (including hydrogen) joint neutron/X-ray refinement. Two DNA and a protein crystal structure were refined against joint neutron/X-ray diffraction data sets using force fields without electrostatics or with electrostatics. Hydrogen bond orientation/geometry favors the inclusion of electrostatics. Refinement of Z-DNA with electrostatics leads to a hypothesis for the entropic stabilization of Z-DNA that may partly explain the thermodynamics of converting the B form of DNA to its Z form. Thus, inclusion of electrostatics assists joint neutron/X-ray refinements, especially for placing and orienting hydrogen atoms. PMID:21481775

Glancing-incidence X-ray diffraction of Ag nanoparticles in gold lustre decoration of Italian Renaissance pottery

NASA Astrophysics Data System (ADS)

Bontempi, E.; Colombi, P.; Depero, L. E.; Cartechini, L.; Presciutti, F.; Brunetti, B. G.; Sgamellotti, A.

2006-06-01

Lustre is known as one of the most significant decorative techniques of Medieval and Renaissance pottery in the Mediterranean basin, characterized by brilliant gold and red metallic reflections and iridescence effects. Previous studies by various techniques (SEM-EDS and TEM, UV-VIS, XRF, RBS and EXAFS) demonstrated that lustre consists of a heterogeneous metal-glass composite film, formed by Cu and Ag nanoparticles dispersed within the outer layer of a tin-opacified lead glaze. In the present work the investigation of an original gold lustre sample from Deruta has been carried out by means of glancing-incidence X-ray diffraction techniques (GIXRD). The study was aimed at providing information on structure and depth distribution of Ag nanoparticles. Exploiting the capability of controlling X-ray penetration in the glaze by changing the incidence angle, we used GIXRD measurements to estimate non-destructively thickness and depth of silver particles present in the first layers of the glaze.

Pink-beam serial crystallography

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

Meents, A.; Wiedorn, M. O.; Srajer, V.

Serial X-ray crystallography allows macromolecular structure determination at both X-ray free electron lasers (XFELs) and, more recently, synchrotron sources. The time resolution for serial synchrotron crystallography experiments has been limited to millisecond timescales with monochromatic beams. The polychromatic, “pink”, beam provides a more than two orders of magnitude increased photon flux and hence allows accessing much shorter timescales in diffraction experiments at synchrotron sources. Here we report the structure determination of two different protein samples by merging pink-beam diffraction patterns from many crystals, each collected with a single 100 ps X-ray pulse exposure per crystal using a setup optimized formore » very low scattering background. In contrast to experiments with monochromatic radiation, data from only 50 crystals were required to obtain complete datasets. The high quality of the diffraction data highlights the potential of this method for studying irreversible reactions at sub-microsecond timescales using high-brightness X-ray facilities.« less

Pink-beam serial crystallography

DOE PAGES

Meents, A.; Wiedorn, M. O.; Srajer, V.; ...

2017-11-03

Serial X-ray crystallography allows macromolecular structure determination at both X-ray free electron lasers (XFELs) and, more recently, synchrotron sources. The time resolution for serial synchrotron crystallography experiments has been limited to millisecond timescales with monochromatic beams. The polychromatic, “pink”, beam provides a more than two orders of magnitude increased photon flux and hence allows accessing much shorter timescales in diffraction experiments at synchrotron sources. Here we report the structure determination of two different protein samples by merging pink-beam diffraction patterns from many crystals, each collected with a single 100 ps X-ray pulse exposure per crystal using a setup optimized formore » very low scattering background. In contrast to experiments with monochromatic radiation, data from only 50 crystals were required to obtain complete datasets. The high quality of the diffraction data highlights the potential of this method for studying irreversible reactions at sub-microsecond timescales using high-brightness X-ray facilities.« less

Digital Image Correlation of 2D X-ray Powder Diffraction Data for Lattice Strain Evaluation

PubMed Central

Zhang, Hongjia; Sui, Tan; Daisenberger, Dominik; Fong, Kai Soon

2018-01-01

High energy 2D X-ray powder diffraction experiments are widely used for lattice strain measurement. The 2D to 1D conversion of diffraction patterns is a necessary step used to prepare the data for full pattern refinement, but is inefficient when only peak centre position information is required for lattice strain evaluation. The multi-step conversion process is likely to lead to increased errors associated with the ‘caking’ (radial binning) or fitting procedures. A new method is proposed here that relies on direct Digital Image Correlation analysis of 2D X-ray powder diffraction patterns (XRD-DIC, for short). As an example of using XRD-DIC, residual strain values along the central line in a Mg AZ31B alloy bar after 3-point bending are calculated by using both XRD-DIC and the conventional ‘caking’ with fitting procedures. Comparison of the results for strain values in different azimuthal angles demonstrates excellent agreement between the two methods. The principal strains and directions are calculated using multiple direction strain data, leading to full in-plane strain evaluation. It is therefore concluded that XRD-DIC provides a reliable and robust method for strain evaluation from 2D powder diffraction data. The XRD-DIC approach simplifies the analysis process by skipping 2D to 1D conversion, and opens new possibilities for robust 2D powder diffraction data analysis for full in-plane strain evaluation. PMID:29543728

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.

Solid-State Spun Fibers from 1 mm Long Carbon Nanotube Forests Synthesized by Water-Assisted Chemical Vapor Deposition

NASA Technical Reports Server (NTRS)

Zhang, Shanju; Zhu, Lingbo; Minus, Marilyn L.; Chae, han Gi; Jagannathan, Sudhakar; Wong, Ching-Ping; Kowalik, Janusz; Roberson, Luke B.; Kumar, Satish

2007-01-01

In this work, we report continuous carbon nanotube fibers dry-drawn directly from water-assisted CVD grown forests with millimeter scale length. As-drawn nanotube fibers exist as aerogel and can be transformed into more compact fibers through twisting or densification with a volatile liquid. Nanotube fibers are characterized by scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), Raman microscopy and wide-angle X-ray diffraction (WAXD). Mechanical behavior and electrical conductivity of the post-treated nanotube fibers are investigated.

Nanoscale interfacial mixing of Au/Bi layers using MeV ion beams

NASA Astrophysics Data System (ADS)

Prusty, Sudakshina; Siva, V.; Ojha, S.; Kabiraj, D.; Sahoo, P. K.

2017-05-01

We have studied nanoscale mixing of thermally deposited double bilayer films of Au/Bi after irradiating them by 1.5 MeV Au2+ ions. Post irradiation effects on the morphology and elemental identification in these films are studied by Scanning electron microscopy (SEM) and Energy dispersive X-ray spectroscopy (EDS). Glancing angle X-ray diffraction (GAXRD) of the samples indicate marginal changes in the irradiated samples due to combined effect of nuclear and electronic energy loss. The interfacial mixing is studied by Rutherford backscattering (RBS).

Oxygen "getter" effects on microstructure and carrier transport in low temperature combustion-processed a-InXZnO (X = Ga, Sc, Y, La) transistors.

PubMed

Hennek, Jonathan W; Smith, Jeremy; Yan, Aiming; Kim, Myung-Gil; Zhao, Wei; Dravid, Vinayak P; Facchetti, Antonio; Marks, Tobin J

2013-07-24

In oxide semiconductors, such as those based on indium zinc oxide (IXZO), a strong oxygen binding metal ion ("oxygen getter"), X, functions to control O vacancies and enhance lattice formation, hence tune carrier concentration and transport properties. Here we systematically study, in the IXZO series, the role of X = Ga(3+) versus the progression X = Sc(3+) → Y(3+) → La(3+), having similar chemical characteristics but increasing ionic radii. IXZO films are prepared from solution over broad composition ranges for the first time via low-temperature combustion synthesis. The films are characterized via thermal analysis of the precursor solutions, grazing incidence angle X-ray diffraction (GIAXRD), atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), and scanning transmission electron microscopy (STEM) with high angle annular dark field (HAADF) imaging. Excellent thin-film transistor (TFT) performance is achieved for all X, with optimal compositions after 300 °C processing exhibiting electron mobilities of 5.4, 2.6, 2.4, and 1.8 cm(2) V(-1) s(-1) for Ga(3+), Sc(3+), Y(3+), and La(3+), respectively, and with I(on)/I(off) = 10(7)-10(8). Analysis of the IXZO TFT positive bias stress response shows X = Ga(3+) to be superior with mobilities (μ) retaining >95% of the prestress values and threshold voltage shifts (ΔV(T)) of <1.6 V, versus <85% μ retention and ΔV(T) ≈ 20 V for the other trivalent ions. Detailed microstructural analysis indicates that Ga(3+) most effectively promotes oxide lattice formation. We conclude that the metal oxide lattice formation enthalpy (ΔH(L)) and metal ionic radius are the best predictors of IXZO oxygen getter efficacy.

Opportunities and challenges for time-resolved studies of protein structural dynamics at X-ray free-electron lasers.

PubMed

Neutze, Richard

2014-07-17

X-ray free-electron lasers (XFELs) are revolutionary X-ray sources. Their time structure, providing X-ray pulses of a few tens of femtoseconds in duration; and their extreme peak brilliance, delivering approximately 10(12) X-ray photons per pulse and facilitating sub-micrometre focusing, distinguish XFEL sources from synchrotron radiation. In this opinion piece, I argue that these properties of XFEL radiation will facilitate new discoveries in life science. I reason that time-resolved serial femtosecond crystallography and time-resolved wide angle X-ray scattering are promising areas of scientific investigation that will be advanced by XFEL capabilities, allowing new scientific questions to be addressed that are not accessible using established methods at storage ring facilities. These questions include visualizing ultrafast protein structural dynamics on the femtosecond to picosecond time-scale, as well as time-resolved diffraction studies of non-cyclic reactions. I argue that these emerging opportunities will stimulate a renaissance of interest in time-resolved structural biochemistry.

Formation and characterization of Ni/Al Ohmic contact on n+-type GeSn

NASA Astrophysics Data System (ADS)

Zhang, Xu; Zhang, Dongliang; Zheng, Jun; Liu, Zhi; He, Chao; Xue, Chunlai; Zhang, Guangze; Li, Chuanbo; Cheng, Buwen; Wang, Qiming

2015-12-01

In this study, a Ni/Al Ohmic contact on a highly doped n-type GeSn has been investigated. A specific contact resistivity as low as (2.26 ± 0.11) × 10-4 Ω cm2 was obtained with the GeSn sample annealed at a temperature of 450 °C for 30 s. The linear Ohmic behavior was attributed to the low resistance of the Ni(GeSn) phase; this behavior was determined using glancing-angle X-ray diffraction, and the quantum tunneling current through the Schottky barrier narrowed because of high doping; this phenomenon was confirmed from the contact resistance characteristics at different temperatures from 45 to 205 K.

X-ray diffraction and infrared spectroscopy studies of Ba(Fe1/2Nb1/2)O3-(Na1/2Bi1/2)TiO3 ceramics

NASA Astrophysics Data System (ADS)

Chandra, K. P.; Yadav, Anjana; Prasad, K.

2018-05-01

Ceramics (1-x)Ba(Fe1/2Nb1/2)O3-x(Na1/2Bi1/2)TiO3; 0≤x≤1.0 were prepared by conventional ceramic synthesis technique. Rietveld refinements of X-ray diffraction data of these ceramics were carried out using FullProf software and determined their crystal symmetry, space group and unit cell dimensions. Rietveld refinement revealed that Ba(Fe1/2Nb1/2)O3 has cubic structure with space group Pm 3 ¯ m and Na1/2Bi1/2)TiO3 has rhombohedral structure with space group R3c. Addition of (Na1/2Bi1/2)TiO3 to Ba(Fe1/2Nb1/2)O3 resulted in the change of unit cell structure from cubic to tetragonal (P4/mmm) for x = 0.75 and the X-Ray diffraction peaks slightly shift towards higher Bragg's angle, suggesting slight decrease in unit cell volume. SEM studies were carried out in order to access the quality of the prepared ceramics which showed a change in grain shapes with the increase of (Na1/2Bi1/2)TiO3 content. FTIR spectra confirmed the formation of perovskite type solid solutions.

Unusual Thermal Stability of High-Entropy Alloy Amorphous Structure

DTIC Science & Technology

2012-06-20

incident angle X - ray diffractometer (GIAXRD, RIGAKU D/MAX2500) with Cu Kα radiation and at the incident angle of 1°. The surface morphology and...microanalyzer (EPMA, JEOL JAX-8800). The crystallographic structures of as-deposited and annealed metallic films were characterized utilizing a glancing ...field image and selected-area- diffraction (SAD) patterns of (a) 800 °C-, (b) 850 °C- and (c) 900 °C-annealed alloy thin films, respectively. Both

Portable X-ray diffractometer equipped with XRF for archaeometry

NASA Astrophysics Data System (ADS)

Uda, M.; Ishizaki, A.; Satoh, R.; Okada, K.; Nakajima, Y.; Yamashita, D.; Ohashi, K.; Sakuraba, Y.; Shimono, A.; Kojima, D.

2005-09-01

A portable X-ray diffractometer equipped with an X-ray fluorescence spectrometer was improved so as to get a diffraction pattern and a fluorescence spectrum simultaneously in air from one and the same small area on a specimen. Here, diffraction experiments were performed in two modes, i.e. an angle rotation mode and an energy dispersive mode. In the latter a diffraction pattern and a fluorescence spectrum were simultaneously recorded in a short time, 100 s or less, on one display. The diffractometer was tested in the field to confirm its performance. Targets chosen for this purpose were a bronze mirror from the Eastern Han Dynasty (25-220), and a stupa and its pedestal which are part of the painted statue of "Tamonten holding a stupa" from the Heian Period (794-1192), enshrined in the Engyouji temple founded in 996. The bronze mirror was identified as a product of the Han Dynasty from its chemical composition and the existence of the δ phase in the Cu-Sn alloy. The stupa and its pedestal were decorated with gold powder and gold leaf, respectively. From the XRF data of the pedestal, the underlying layer of gold leaf seems to have been painted with emerald green.

Correcting intensity loss errors in the absence of texture-free reference samples during pole figure measurement

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

Saleh, Ahmed A., E-mail: asaleh@uow.edu.au

Even with the use of X-ray polycapillary lenses, sample tilting during pole figure measurement results in a decrease in the recorded X-ray intensity. The magnitude of this error is affected by the sample size and/or the finite detector size. These errors can be typically corrected by measuring the intensity loss as a function of the tilt angle using a texture-free reference sample (ideally made of the same alloy as the investigated material). Since texture-free reference samples are not readily available for all alloys, the present study employs an empirical procedure to estimate the correction curve for a particular experimental configuration.more » It involves the use of real texture-free reference samples that pre-exist in any X-ray diffraction laboratory to first establish the empirical correlations between X-ray intensity, sample tilt and their Bragg angles and thereafter generate correction curves for any Bragg angle. It will be shown that the empirically corrected textures are in very good agreement with the experimentally corrected ones. - Highlights: •Sample tilting during X-ray pole figure measurement leads to intensity loss errors. •Texture-free reference samples are typically used to correct the pole figures. •An empirical correction procedure is proposed in the absence of reference samples. •The procedure relies on reference samples that pre-exist in any texture laboratory. •Experimentally and empirically corrected textures are in very good agreement.« less

Structure of nanocrystalline calcium silicate hydrates: insights from X-ray diffraction, synchrotron X-ray absorption and nuclear magnetic resonance

PubMed Central

Grangeon, Sylvain; Claret, Francis; Roosz, Cédric; Sato, Tsutomu; Gaboreau, Stéphane; Linard, Yannick

2016-01-01

The structure of nanocrystalline calcium silicate hydrates (C–S–H) having Ca/Si ratios ranging between 0.57 ± 0.05 and 1.47 ± 0.04 was studied using an electron probe micro-analyser, powder X-ray diffraction, 29Si magic angle spinning NMR, and Fourier-transform infrared and synchrotron X-ray absorption spectroscopies. All samples can be described as nanocrystalline and defective tobermorite. At low Ca/Si ratio, the Si chains are defect free and the Si Q 3 and Q 2 environments account, respectively, for up to 40.2 ± 1.5% and 55.6 ± 3.0% of the total Si, with part of the Q 3 Si being attributable to remnants of the synthesis reactant. As the Ca/Si ratio increases up to 0.87 ± 0.02, the Si Q 3 environment decreases down to 0 and is preferentially replaced by the Q 2 environment, which reaches 87.9 ± 2.0%. At higher ratios, Q 2 decreases down to 32.0 ± 7.6% for Ca/Si = 1.38 ± 0.03 and is replaced by the Q 1 environment, which peaks at 68.1 ± 3.8%. The combination of X-ray diffraction and NMR allowed capturing the depolymerization of Si chains as well as a two-step variation in the layer-to-layer distance. This latter first increases from ∼11.3 Å (for samples having a Ca/Si ratio <∼0.6) up to 12.25 Å at Ca/Si = 0.87 ± 0.02, probably as a result of a weaker layer-to-layer connectivity, and then decreases down to 11 Å when the Ca/Si ratio reaches 1.38 ± 0.03. The decrease in layer-to-layer distance results from the incorporation of interlayer Ca that may form a Ca(OH)2-like structure, nanocrystalline and intermixed with C–S–H layers, at high Ca/Si ratios. PMID:27275135

Evaluation of the molecular lipid organization in millimeter-sized stratum corneum by synchrotron X-ray diffraction.

PubMed

Suzuki, T; Uchino, T; Hatta, I; Miyazaki, Y; Kato, S; Sasaki, K; Kagawa, Y

2018-04-29

The aim of this study was to investigate whether the lamellar and lateral structure of intercellular lipid of stratum corneum (SC) can be evaluated from millimeter-sized SC (MSC) by X-ray diffraction. A 12 mm × 12 mm SC sheet from hairless mouse was divided into 16 pieces measuring 3 mm × 3 mm square. From another sheet, 4 pieces of ultramillimeter-sized SC (USC:1.5 mm × 1.5 mm square) were prepared. Small and wide-angle X-ray diffraction (SAXD and WAXD) measurements were performed on each piece. For MSC and USC, changes in the lamellar and lateral structure after the application of d-limonene were measured. The intensity of SAXD peaks due to the lamellar phase of long periodicity phase (LPP) and WAXD peaks due to the lateral hydrocarbon chain-packing structures varied in MSC and USC pieces, although over the 12 mm × 12 mm SC sheet. These results indicated that the intercellular lipid components and their proportion appeared nearly uniform. Application of d-limonene on MSC and USC piece with strong peaks in SAXD and the WAXD resulted in the disappearance of peaks due to the lamellar phase of LPP and decrease in peak intensity for the lateral hydrocarbon chain-packing structures. These changes are consistent with normal-sized sample results. We found that the selection of a sample piece with strong diffraction peaks due to the lamellar and lateral structure enabled evaluation of the SC structure in small-sized samples by X-ray diffraction. © 2018 John Wiley & Sons A/S. Published by John Wiley & Sons Ltd.

Quick measurement of crystal truncation rod profiles in simultaneous multi-wavelength dispersive mode

NASA Astrophysics Data System (ADS)

Matsushita, T.; Takahashi, T.; Shirasawa, T.; Arakawa, E.; Toyokawa, H.; Tajiri, H.

2011-11-01

To conduct time-resolved measurements in the wide momentum transfer (q = 4π sinθ/λ, θ: the glancing angle of the x-ray beam, λ: x-ray wavelength) range of interest, we developed a method that can simultaneously measure the whole profile of x-ray diffraction and crystal truncation rod scattering of interest with no need of rotation of the specimen, detector, and monochromator crystal during the measurement. With a curved crystal polychromator (Si 111 diffraction), a horizontally convergent x-ray beam having a one-to-one correlation between wavelength (energy: 16.24-23.0 keV) and direction is produced. The convergent x-ray beam components of different wavelengths are incident on the specimen in a geometry where θ is the same for all the x-ray components and are diffracted within corresponding vertical scattering planes by a specimen ([GaAs(12ML)/AlAs(8 ML)]50 on GaAs(001) substrate) placed at the focal point. Although θ is the same for all the directions, q continuously varies because λ changes as a function of direction. The normalized horizontal intensity distribution across the beam, as measured using a two-dimensional pixel array detector downstream of the specimen, represents the reflectivity curve profile both near to and far from the Bragg point. As for the crystal truncation rod scattering around the 002 reflection, the diffraction profile from the Bragg peak down to reflectivity of 1.0 × 10-9 was measured with a sufficient data collection time (1000-2000 s). With data collection times of 100, 10, 1.0, and 0.1 s, profiles down to a reflectivity of ˜6 × 10-9, ˜2 × 10-8, ˜8 × 10-8, and ˜8 × 10-7 were measured, respectively. To demonstrate the time-resolving capability of the system, reflectivity curves were measured with time resolutions of 1.0 s while rotating the specimen. We have also measured the diffraction profile around the 113 reflection in the non-specular reflection geometry.

Crystallization and preliminary X-ray analysis of a low density lipoprotein from human plasma.

PubMed

Prassl, R; Chapman, J M; Nigon, F; Sara, M; Eschenburg, S; Betzel, C; Saxena, A; Laggner, P

1996-11-15

Single crystals of human plasma low density lipoprotein (LDL), the major transport vehicle for cholesterol in blood, have been produced with a view to analysis of the three-dimensional structure by x-ray crystallography. Crystals with dimensions of approximately 200 x 100 x 50 microm have been reproducibly obtained from highly homogeneous LDL particle subspecies, isolated in the density ranges d = 1.0271-1. 0297 g/ml and d = 1.0297-1.0327 g/ml. Electron microscopic imaging of ultrathin-sectioned preparations of the crystals confirmed the existence of a regular, quasihexagonal arrangement of spherical particles of approximately 18 nm in diameter, thereby resembling the dimensions characteristic of LDL after dehydration and fixation. X-ray diffraction with synchrotron radiation under cryogenic conditions revealed the presence of well resolved diffraction spots, to a resolution of about 29 A. The diffraction patterns are indexed in terms of a triclinic lattice with unit cell dimensions of a = 16. 1 nm, b = 39.0 nm, c = 43.9 nm; alpha = 96.2 degrees, beta = 92.1 degrees, gamma = 102 degrees, and with space group P1.

X-ray measurements of the strain and shape of dielectric/metallic wrap-gated InAs nanowires

NASA Astrophysics Data System (ADS)

Eymery, J.; Favre-Nicolin, V.; Fröberg, L.; Samuelson, L.

2009-03-01

Wrap-gate (111) InAs nanowires (NWs) were studied after HfO2 dielectric coating and Cr metallic deposition by a combination of grazing incidence x-ray techniques. In-plane and out-of-plane x-ray diffraction (crystal truncation rod analysis) allow determining the strain tensor. The longitudinal contraction, increasing with HfO2 and Cr deposition, is significantly larger than the radial dilatation. For the Cr coating, the contraction along the growth axis is quite large (-0.95%), and the longitudinal/radial deformation ratio is >10, which may play a role on the NW transport properties. Small angle x-ray scattering shows a smoothening of the initial hexagonal bare InAs NW shape and gives the respective core/shell thicknesses, which are compared to flat surface values.

Ionic depletion at the crystalline Gibbs layer of PEG-capped gold nanoparticle brushes at aqueous surfaces

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

Wang, Wenjie; Zhang, Honghu; Mallapragada, Surya

In situ surface-sensitive x-ray diffraction and grazing incidence x-ray fluorescence spectroscopy (GIXFS) methods are combined to determine the ionic distributions across the liquid/vapor interfaces of thiolated-polyethylene-glycol–capped gold nanoparticle (PEG-AuNP) solutions. Induced by the addition of salts (i.e., Cs 2SO 4) to PEG-AuNPs solutions, two-dimensional hexagonal lattices of PEG-AuNPs form spontaneously at the aqueous surfaces, as is demonstrated by x-ray reflectivity and grazing incidence small-angle x-ray scattering. In conclusion, by taking advantage of element specificity with the GIXFS method, we find that the cation Cs + concentration at the crystalline film is significantly reduced in parts of the PEG-AuNP film comparedmore » with that in the bulk.« less

Ionic depletion at the crystalline Gibbs layer of PEG-capped gold nanoparticle brushes at aqueous surfaces

DOE PAGES

Wang, Wenjie; Zhang, Honghu; Mallapragada, Surya; ...

2017-12-14

In situ surface-sensitive x-ray diffraction and grazing incidence x-ray fluorescence spectroscopy (GIXFS) methods are combined to determine the ionic distributions across the liquid/vapor interfaces of thiolated-polyethylene-glycol–capped gold nanoparticle (PEG-AuNP) solutions. Induced by the addition of salts (i.e., Cs 2SO 4) to PEG-AuNPs solutions, two-dimensional hexagonal lattices of PEG-AuNPs form spontaneously at the aqueous surfaces, as is demonstrated by x-ray reflectivity and grazing incidence small-angle x-ray scattering. In conclusion, by taking advantage of element specificity with the GIXFS method, we find that the cation Cs + concentration at the crystalline film is significantly reduced in parts of the PEG-AuNP film comparedmore » with that in the bulk.« less

Manufacturing and characterization of Ni-free N-containing ODS austenitic alloy

NASA Astrophysics Data System (ADS)

Mori, A.; Mamiya, H.; Ohnuma, M.; Ilavsky, J.; Ohishi, K.; Woźniak, Jarosław; Olszyna, A.; Watanabe, N.; Suzuki, J.; Kitazawa, H.; Lewandowska, M.

2018-04-01

Ni-free N-containing oxide dispersion strengthened (ODS) austenitic alloys were manufactured by mechanical alloying (MA) followed by spark plasma sintering (SPS). The phase evolutions during milling under a nitrogen atmosphere and after sintering were studied by X-ray diffraction (XRD). Transmission electron microcopy (TEM) and alloy contrast variation analysis (ACV), including small-angle neutron scattering (SANS) and ultra-small-angle X-ray scattering (USAXS), revealed the existence of nanoparticles with a diameter of 3-51 nm for the samples sintered at 950 °C. Sintering at 1000 °C for 5 and 15 min caused slight growth and a significant coarsening of the nanoparticles, up to 70 nm and 128 nm, respectively. The ACV analysis indicated the existence of two populations of Y2O3, ε-martensite and MnO. The dispersive X-ray spectrometry (EDS) confirmed two kinds of nanoparticles, Y2O3 and MnO. The material was characterized by superior micro-hardness, of above 500 HV0.1.

Synthesis and characterization of Mn-Bi alloy

NASA Astrophysics Data System (ADS)

Mishra, Ashutosh; Patil, Harsha; Jain, G.; Mishra, N.

2012-06-01

High purity MnBi low temperature phase has been prepared and analyzed using X-ray diffraction, Lorentz-Polarization Factor and Fourier transforms infrared measurement. After synthesis of samples structural characterization has done on samples by X-ray diffraction, which shows that after making the bulk sample is in no single phase MnBi has been prepared by sintering Mn and Bi powders. By Lorentz-Polarization Factor is affecting the relative intensity of diffraction lines on a powder form. And by FTIR which shows absorption peaks of MnBi alloys.

Refractive optics to compensate x-ray mirror shape-errors

NASA Astrophysics Data System (ADS)

Laundy, David; Sawhney, Kawal; Dhamgaye, Vishal; Pape, Ian

2017-08-01

Elliptically profiled mirrors operating at glancing angle are frequently used at X-ray synchrotron sources to focus X-rays into sub-micrometer sized spots. Mirror figure error, defined as the height difference function between the actual mirror surface and the ideal elliptical profile, causes a perturbation of the X-ray wavefront for X- rays reflecting from the mirror. This perturbation, when propagated to the focal plane results in an increase in the size of the focused beam. At Diamond Light Source we are developing refractive optics that can be used to locally cancel out the wavefront distortion caused by figure error from nano-focusing elliptical mirrors. These optics could be used to correct existing optical components on synchrotron radiation beamlines in order to give focused X-ray beam sizes approaching the theoretical diffraction limit. We present our latest results showing measurement of the X-ray wavefront error after reflection from X-ray mirrors and the translation of the measured wavefront into a design for refractive optical elements for correction of the X-ray wavefront. We show measurement of the focused beam with and without the corrective optics inserted showing reduction in the size of the focus resulting from the correction to the wavefront.

Electron paramagnetic resonance, scanning electron microscopy with energy dispersion X-ray spectrometry, X-ray powder diffraction, and NMR characterization of iron-rich fired clays.

PubMed

Presciutti, Federica; Capitani, Donatella; Sgamellotti, Antonio; Brunetti, Brunetto Giovanni; Costantino, Ferdinando; Viel, Stéphane; Segre, Annalaura

2005-12-01

The aim of this study is to clarify the structure of an iron-rich clay and the structural changes involved in the firing process as a preliminary step to get information on ancient ceramic technology. To this purpose, illite-rich clay samples fired at different temperatures were characterized using a multitechnique approach, i.e., by electron paramagnetic resonance, scanning electron microscopy with electron dispersion X-ray spectrometry, X-ray powder diffraction, magic angle spinning and multiple quantum magic angle spinning NMR. During firing, four main reaction processes occur: dehydration, dehydroxylation, structural breakdown, and recrystallization. When the results are combined from all characterization methods, the following conclusions could be obtained. Interlayer H2O is located close to aluminum in octahedral sites and is driven off at temperatures lower than 600 degrees C. Between 600 and 700 degrees C dehydroxylation occurs whereas, between 800 and 900 degrees C, the aluminum in octahedral sites disappears, due to the breakdown of the illite structure, and all iron present is oxidized to Fe3+. In samples fired at 1000 and 1100 degrees C iron clustering was observed as well as large single crystals of iron with the occurrence of ferro- or ferrimagnetic effects. Below 900 degrees C the aluminum in octahedral sites presents a continuous distribution of chemical shift, suggesting the presence of slightly distorted sites. Finally, over the whole temperature range, the presence of at least two tetrahedral aluminum sites was revealed, characterized by different values of the quadrupolar coupling constant.

Wave-optical assessment of alignment tolerances in nano-focusing with ellipsoidal mirror

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

Yumoto, Hirokatsu, E-mail: yumoto@spring8.or.jp; Koyama, Takahisa; Matsuyama, Satoshi

2016-01-28

High-precision ellipsoidal mirrors, which can efficiently focus X-rays to the nanometer dimension with a mirror, have not been realized because of the difficulties in the fabrication process. The purpose of our study was to develop nano-focusing ellipsoidal mirrors in the hard X-ray region. We developed a wave-optical focusing simulator for investigating alignment tolerances in nano-focusing with a designed ellipsoidal mirror, which produce a diffraction-limited focus size of 30 × 35 nm{sup 2} in full width at half maximum at an X-ray energy of 7 keV. The simulator can calculate focusing intensity distributions around the focal point under conditions of misalignment. Themore » wave-optical simulator enabled the calculation of interference intensity distributions, which cannot be predicted by the conventional ray-trace method. The alignment conditions with a focal length error of ≲ ±10 µm, incident angle error of ≲ ±0.5 µrad, and in-plane rotation angle error of ≲ ±0.25 µrad must be satisfied for nano-focusing.« less

Valence fluctuating compound α-YbAlB4 studied by 174Yb Mössbauer spectroscopy and X-ray diffraction using synchrotron radiation

NASA Astrophysics Data System (ADS)

Oura, Momoko; Ikeda, Shugo; Masuda, Ryo; Kobayashi, Yasuhiro; Seto, Makoto; Yoda, Yoshitaka; Hirao, Naohisa; Kawaguchi, Saori I.; Ohishi, Yasuo; Suzuki, Shintaro; Kuga, Kentaro; Nakatsuji, Satoru; Kobayashi, Hisao

2018-05-01

The structural properties and the Yb 4 f electronic state of the valence fluctuating α-YbAlB4 have been investigated by powder X-ray diffraction under pressure and 174Yb Mössbauer spectroscopy with magnetic fields at low temperature, respectively, using synchrotron radiation. Powder X-ray diffraction patterns showed that the crystal structure does not change up to p ∼ 18 GPa at 8 K and the volume decreases smoothly. However, the pressure dependence of the difference in the structure factor between the (060) and (061) diffraction lines changes at ∼ 3.4 GPa, indicating the change of atomic coordination parameters. The 174Yb Mössbauer spectroscopy measurements at 2 K with 10 and 50 kOe suggest that the electrical quadrupole interaction changes by applied magnetic fields.

Anomalous Thermal Expansion of HoCo0.5Cr0.5O3 Probed by X-ray Synchrotron Powder Diffraction.

PubMed

Hreb, Vasyl; Vasylechko, Leonid; Mykhalichko, Vitaliya; Prots, Yurii

2017-12-01

Mixed holmium cobaltite-chromite HoCo 0.5 Cr 0.5 O 3 with orthorhombic perovskite structure (structure type GdFeO 3 , space group Pbnm) was obtained by solid state reaction of corresponding oxides in air at 1373 K. Room- and high-temperature structural parameters were derived from high-resolution X-ray synchrotron powder diffraction data collected in situ in the temperature range of 300-1140 K. Analysis of the results obtained revealed anomalous thermal expansion of HoCo 0.5 Cr 0.5 O 3 , which is reflected in a sigmoidal temperature dependence of the unit cell parameters and in abnormal increase of the thermal expansion coefficients with a broad maxima near 900 K. Pronounced anomalies are also observed for interatomic distances and angles within Co/CrO 6 octahedra, tilt angles of octahedra and atomic displacement parameters. The observed anomalies are associated with the changes of spin state of Co 3+ ions and insulator-metal transition occurring in HoCo 0.5 Cr 0.5 O 3 .

Anomalous Thermal Expansion of HoCo0.5Cr0.5O3 Probed by X-ray Synchrotron Powder Diffraction

NASA Astrophysics Data System (ADS)

Hreb, Vasyl; Vasylechko, Leonid; Mykhalichko, Vitaliya; Prots, Yurii

2017-07-01

Mixed holmium cobaltite-chromite HoCo0.5Cr0.5O3 with orthorhombic perovskite structure (structure type GdFeO3, space group Pbnm) was obtained by solid state reaction of corresponding oxides in air at 1373 K. Room- and high-temperature structural parameters were derived from high-resolution X-ray synchrotron powder diffraction data collected in situ in the temperature range of 300-1140 K. Analysis of the results obtained revealed anomalous thermal expansion of HoCo0.5Cr0.5O3, which is reflected in a sigmoidal temperature dependence of the unit cell parameters and in abnormal increase of the thermal expansion coefficients with a broad maxima near 900 K. Pronounced anomalies are also observed for interatomic distances and angles within Co/CrO6 octahedra, tilt angles of octahedra and atomic displacement parameters. The observed anomalies are associated with the changes of spin state of Co3+ ions and insulator-metal transition occurring in HoCo0.5Cr0.5O3.

Melting-solidification transition of Zn nanoparticles embedded in SiO2: Observation by synchrotron x-ray and ultraviolet-visible-near-infrared light

NASA Astrophysics Data System (ADS)

Amekura, H.; Tanaka, M.; Katsuya, Y.; Yoshikawa, H.; Ohnuma, M.; Matsushita, Y.; Kobayashi, K.; Kishimoto, N.

2010-11-01

Melting-solidification transition of Zn nanoparticles (NPs) with the mean diameter of 11.5 nm, embedded in silica glass, was investigated by glancing incident x-ray diffraction (GIXRD) at high temperatures using synchrotron radiation (SR). With increasing temperature, 101Zn diffraction peak gradually decreases up to ˜360 °C and then steeply decreases. This is due to the melting of Zn NPs, which completes around 420 °C. With decreasing temperature, the solidification of the NPs begins around ˜310 °C. The temperature hysteresis with a width of ˜110 °C was observed. With temperature, the diffraction angle shows a shift without hysteresis, which is ascribed to thermal expansion of Zn NP lattice. Thermal expansion coefficient of Zn NPs was determined as 24.4×10-6 K-1 along the ⟨101⟩ direction. Optical absorption spectroscopy shows a broad ultraviolet (UV) peak which was observed at even higher temperatures than the melting temperature but shifts to the low-energy side with the melting. The energy shift in the UV peak also shows the temperature hysteresis which resembles with the melting-solidification hysteresis recorded by SR-GIXRD. The melting-solidification transition is also detectable by the optical absorption spectroscopy in the UV-visible-near-infrared region.

Evidence for weak ferromagnetism, isostructural phase transition, and linear magnetoelectric coupling in the multiferroic Bi0.8Pb0.2Fe0.9Nb0.1O3 solid solution

NASA Astrophysics Data System (ADS)

Patel, Jay Prakash; Senyshyn, Anatoliy; Fuess, Hartmut; Pandey, Dhananjai

2013-09-01

Magnetization, dielectric, and calorimetric studies on Bi0.8 Pb0.2 Fe0.9 Nb0.1O3 (BF-0.2PFN) reveal very weak ferromagnetism but strong dielectric anomaly at the antiferromagnetic transition temperature (TN) characteristic of magnetoelectric coupling. We correlate these results with nuclear and magnetic structure studies using x-ray and neutron powder diffraction techniques, respectively. Rietveld refinements using x-ray powder diffraction data in the temperature range 300 to 673 K reveal pronounced anomalies in the unit cell parameters at TN, indicating strong magnetoelastic coupling. The nuclear and magnetic structures of BF-0.2PFN were determined from neutron powder diffraction data using a representation theory approach. They show the occurrence of a first-order isostructural phase transition (IPT) accompanying the magnetic ordering below TN˜566 K, leading to significant discontinuous change in the ionic polarization (ΔPz˜1.6(3) μC/cm2) and octahedral tilt angle (˜0.3°) at TN. The ionic polarization obtained from refined positional coordinates of the nuclear structure and Born effective charges is shown to scale linearly with sublattice magnetization, confirming the presence of linear magnetoelectric coupling in BF-0.2PFN at the atomic level, despite the very low value of remanent magnetization (Mr).

Open data set of live cyanobacterial cells imaged using an X-ray laser

NASA Astrophysics Data System (ADS)

van der Schot, Gijs; Svenda, Martin; Maia, Filipe R. N. C.; Hantke, Max F.; Deponte, Daniel P.; Seibert, M. Marvin; Aquila, Andrew; Schulz, Joachim; Kirian, Richard A.; Liang, Mengning; Stellato, Francesco; Bari, Sadia; Iwan, Bianca; Andreasson, Jakob; Timneanu, Nicusor; Bielecki, Johan; Westphal, Daniel; Nunes de Almeida, Francisca; Odić, Duško; Hasse, Dirk; Carlsson, Gunilla H.; Larsson, Daniel S. D.; Barty, Anton; Martin, Andrew V.; Schorb, Sebastian; Bostedt, Christoph; Bozek, John D.; Carron, Sebastian; Ferguson, Ken; Rolles, Daniel; Rudenko, Artem; Epp, Sascha W.; Foucar, Lutz; Rudek, Benedikt; Erk, Benjamin; Hartmann, Robert; Kimmel, Nils; Holl, Peter; Englert, Lars; Loh, N. Duane; Chapman, Henry N.; Andersson, Inger; Hajdu, Janos; Ekeberg, Tomas

2016-08-01

Structural studies on living cells by conventional methods are limited to low resolution because radiation damage kills cells long before the necessary dose for high resolution can be delivered. X-ray free-electron lasers circumvent this problem by outrunning key damage processes with an ultra-short and extremely bright coherent X-ray pulse. Diffraction-before-destruction experiments provide high-resolution data from cells that are alive when the femtosecond X-ray pulse traverses the sample. This paper presents two data sets from micron-sized cyanobacteria obtained at the Linac Coherent Light Source, containing a total of 199,000 diffraction patterns. Utilizing this type of diffraction data will require the development of new analysis methods and algorithms for studying structure and structural variability in large populations of cells and to create abstract models. Such studies will allow us to understand living cells and populations of cells in new ways. New X-ray lasers, like the European XFEL, will produce billions of pulses per day, and could open new areas in structural sciences.

Open data set of live cyanobacterial cells imaged using an X-ray laser.

PubMed

van der Schot, Gijs; Svenda, Martin; Maia, Filipe R N C; Hantke, Max F; DePonte, Daniel P; Seibert, M Marvin; Aquila, Andrew; Schulz, Joachim; Kirian, Richard A; Liang, Mengning; Stellato, Francesco; Bari, Sadia; Iwan, Bianca; Andreasson, Jakob; Timneanu, Nicusor; Bielecki, Johan; Westphal, Daniel; Nunes de Almeida, Francisca; Odić, Duško; Hasse, Dirk; Carlsson, Gunilla H; Larsson, Daniel S D; Barty, Anton; Martin, Andrew V; Schorb, Sebastian; Bostedt, Christoph; Bozek, John D; Carron, Sebastian; Ferguson, Ken; Rolles, Daniel; Rudenko, Artem; Epp, Sascha W; Foucar, Lutz; Rudek, Benedikt; Erk, Benjamin; Hartmann, Robert; Kimmel, Nils; Holl, Peter; Englert, Lars; Loh, N Duane; Chapman, Henry N; Andersson, Inger; Hajdu, Janos; Ekeberg, Tomas

2016-08-01

Structural studies on living cells by conventional methods are limited to low resolution because radiation damage kills cells long before the necessary dose for high resolution can be delivered. X-ray free-electron lasers circumvent this problem by outrunning key damage processes with an ultra-short and extremely bright coherent X-ray pulse. Diffraction-before-destruction experiments provide high-resolution data from cells that are alive when the femtosecond X-ray pulse traverses the sample. This paper presents two data sets from micron-sized cyanobacteria obtained at the Linac Coherent Light Source, containing a total of 199,000 diffraction patterns. Utilizing this type of diffraction data will require the development of new analysis methods and algorithms for studying structure and structural variability in large populations of cells and to create abstract models. Such studies will allow us to understand living cells and populations of cells in new ways. New X-ray lasers, like the European XFEL, will produce billions of pulses per day, and could open new areas in structural sciences.

Open data set of live cyanobacterial cells imaged using an X-ray laser

PubMed Central

van der Schot, Gijs; Svenda, Martin; Maia, Filipe R.N.C.; Hantke, Max F.; DePonte, Daniel P.; Seibert, M. Marvin; Aquila, Andrew; Schulz, Joachim; Kirian, Richard A.; Liang, Mengning; Stellato, Francesco; Bari, Sadia; Iwan, Bianca; Andreasson, Jakob; Timneanu, Nicusor; Bielecki, Johan; Westphal, Daniel; Nunes de Almeida, Francisca; Odić, Duško; Hasse, Dirk; Carlsson, Gunilla H.; Larsson, Daniel S.D.; Barty, Anton; Martin, Andrew V.; Schorb, Sebastian; Bostedt, Christoph; Bozek, John D.; Carron, Sebastian; Ferguson, Ken; Rolles, Daniel; Rudenko, Artem; Epp, Sascha W.; Foucar, Lutz; Rudek, Benedikt; Erk, Benjamin; Hartmann, Robert; Kimmel, Nils; Holl, Peter; Englert, Lars; Loh, N. Duane; Chapman, Henry N.; Andersson, Inger; Hajdu, Janos; Ekeberg, Tomas

2016-01-01

Structural studies on living cells by conventional methods are limited to low resolution because radiation damage kills cells long before the necessary dose for high resolution can be delivered. X-ray free-electron lasers circumvent this problem by outrunning key damage processes with an ultra-short and extremely bright coherent X-ray pulse. Diffraction-before-destruction experiments provide high-resolution data from cells that are alive when the femtosecond X-ray pulse traverses the sample. This paper presents two data sets from micron-sized cyanobacteria obtained at the Linac Coherent Light Source, containing a total of 199,000 diffraction patterns. Utilizing this type of diffraction data will require the development of new analysis methods and algorithms for studying structure and structural variability in large populations of cells and to create abstract models. Such studies will allow us to understand living cells and populations of cells in new ways. New X-ray lasers, like the European XFEL, will produce billions of pulses per day, and could open new areas in structural sciences. PMID:27479514

Macromolecular Topography Leaps into the Digital Age

NASA Technical Reports Server (NTRS)

Lovelace, J.; Bellamy, H.; Snell, E. H.; Borgstahl, G.

2003-01-01

A low-cost, real-time digital topography system is under development which will replace x-ray film and nuclear emulsion plates. The imaging system is based on an inexpensive surveillance camera that offers a 1000x1000 array of 8 im square pixels, anti-blooming circuitry, and very quick read out. Currently, the system directly converts x-rays to an image with no phosphor. The system is small and light and can be easily adapted to work with other crystallographic equipment. Preliminary images have been acquired of cubic insulin at the NSLS x26c beam line. NSLS x26c was configured for unfocused monochromatic radiation. Six reflections were collected with stills spaced from 0.002 to 0.001 degrees apart across the entire oscillation range that the reflections were in diffracting condition. All of the reflections were rotated to the vertical to reduce Lorentz and beam related effects. This particular CCD is designed for short exposure applications (much less than 1 sec) and so has a relatively high dark current leading to noisy raw images. The images are processed to remove background and other system noise with a multi-step approach including the use of wavelets, histogram, and mean window filtering. After processing, animations were constructed with the corresponding reflection profile to show the diffraction of the crystal volume vs. the oscillation angle as well as composite images showing the parts of the crystal with the strongest diffraction for each reflection. The final goal is to correlate features seen in reflection profiles captured with fine phi slicing to those seen in the topography images. With this development macromolecular topography finally comes into the digital age.

Preparation of micro/nano-structure superhydrophobic film on aluminum plates using galvanic corrosion method.

PubMed

Wu, Ruomei; Chao, Guang Hua; Jiang, Haiyun; Pan, Anqiang; Chen, Hong; Yuan, Zhiqing; Liu, Qilong

2013-10-01

A simple and novel approach has been developed to obtain a microporous film with compound nanoparticles on the surface of aluminum alloy substrate using the galvanic corrosion method. The wettability of the surface changes from hydrophilicity to superhydrophobicity after chemical modification with stearic acid (SA). The water contact angle (WCA) and sliding angle (WSA) of superhydrophobic aluminum alloy surface (SAAS) are 154 degrees and 9 degrees, respectively. The roughness of the aluminum substrate increases after the oxidation reaction. The porous aluminum matrix surface is covered with irregularly shaped holes with a mean radius of about 15 microm, similar to the surface papillae of natural Lotus leaf, with villus-like nanoparticles array on pore surfaces. The superhydrophobic property is attributed to this special surface morphology and low surface energy SA. X-ray powder diffraction (XRD) pattern and Energy Dispersive X-Ray Spectroscopy (EDS) spectrum indicate that Al2O3, Al(OH)3 and AIO(OH) has been formed on the surface of aluminum substrate after the oxidation reaction. The Raman spectra indicate that C-H bond from SA and the Al-O are formed on the SAAS. The as-formed SAAS has good stability.

1-Pentyl-3-(4-methoxy-1-naphthoyl)indole and 2-(2-methoxy-phenyl)-1-(1-pentyl-1 H-indol-3-yl)-ethanone: X-ray structures and computational studies

NASA Astrophysics Data System (ADS)

Nycz, Jacek E.; Malecki, Grzegorz; Zawiazalec, Marcin; Pazdziorek, Tadeusz; Skop, Patrycja

2010-12-01

1-Pentyl-3-(4-methoxy-1-naphthoyl)indole (shortly named JWH-081) ( 1) and 2-(2-methoxy-phenyl)-1-(1-pentyl-1 H-indol-3-yl)-ethanone (shortly named JWH-250) ( 2), are examples of cannabinoids which were characterized by FTIR, UV-Vis, multinuclear NMR spectroscopy and single crystal X-ray diffraction method. The geometries of the studied compounds were optimized in singlet states using the density functional theory (DFT) method with B3LYP functional. Electronic spectra were calculated by TDDFT method. In general, the predicted bond lengths and angles are in a good agreement with the values based on the X-ray crystal structure data.

Measuring Three-Dimensional Strain and Structural Defects in a Single InGaAs Nanowire Using Coherent X-ray Multiangle Bragg Projection Ptychography

DOE PAGES

Hill, Megan O.; Calvo-Almazan, Irene; Allain, Marc; ...

2018-01-08

III - As nanowires are candidates for near-infrared light emitters and detectors that can be directly integrated onto silicon. However, nanoscale to microscale variations in structure, composition, and strain within a given nanowire, as well as variations between nanowires, pose challenges to correlating microstructure with device performance. In this work, we utilize coherent nanofocused X-rays to characterize stacking defects and strain in a single InGaAs nanowire supported on Si. By reconstructing diffraction patterns from the 2110 Bragg peak, we show that the lattice orientation varies along the length of the wire, while the strain field along the cross-section is largelymore » unaffected, leaving the band structure unperturbed. Diffraction patterns from the 0110 Bragg peak are reproducibly reconstructed to create three-dimensional images of stacking defects and associated lattice strains, revealing sharp planar boundaries between different crystal phases of wurtzite (WZ) structure that contribute to charge carrier scattering. Phase retrieval is made possible by developing multiangle Bragg projection ptychography (maBPP) to accommodate coherent nanodiffraction patterns measured at arbitrary overlapping positions at multiple angles about a Bragg peak, eliminating the need for scan registration at different angles. The penetrating nature of X-ray radiation, together with the relaxed constraints of maBPP, will enable the in operando imaging of nanowire devices.« less

Production of thick uniform-coating films containing rectorite on nanofibers through the use of an automated coating machine.

PubMed

Wu, Yang; Li, Xueyong; Shi, Xiaowen; Zhan, Yingfei; Tu, Hu; Du, Yumin; Deng, Hongbing; Jiang, Linbin

2017-01-01

When an efficient automated coating machine is used to process layer-by-layer (LBL) deposited nanofibrous mats, it causes an obvious planar effect on the surface of the mats, which can be eliminated through ultimate immersion. During this process, chitosan (CS) - rectorite (REC) intercalated composite films are built on the surface of cellulose acetate (CA) nanofibrous mats by a coating machine. Then, the immersion process is utilized to allow positively charged CS or CS-REC intercalated composites to uniformly assemble on the surface of negatively charged CA nanofibers. An investigation into the morphology of the resultant scaffolds confirms that the uniquely small pore size, high specific surface area and typically three-dimensional (3D) structure of nanofibrous mats remain present. The results of Fourier transform infrared (FT-IR) and X-ray photoelectron spectroscopy (XPS) indicate that it is feasible to assemble nanofibrous mats using a coating machine. The intercalated structure of CS-REC is confirmed by the results of small-angle X-ray diffraction (SAXRD) and wide-angle X-ray diffraction (WAXRD). The results of the cell experiment and antibacterial test demonstrate that the addition of REC not only has little impact on the cytocompatibility of the mats but also enhances their ability to inhibit bacteria. Copyright © 2016 Elsevier B.V. All rights reserved.

Measuring Three-Dimensional Strain and Structural Defects in a Single InGaAs Nanowire Using Coherent X-ray Multiangle Bragg Projection Ptychography

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

Hill, Megan O.; Calvo-Almazan, Irene; Allain, Marc

III - As nanowires are candidates for near-infrared light emitters and detectors that can be directly integrated onto silicon. However, nanoscale to microscale variations in structure, composition, and strain within a given nanowire, as well as variations between nanowires, pose challenges to correlating microstructure with device performance. In this work, we utilize coherent nanofocused X-rays to characterize stacking defects and strain in a single InGaAs nanowire supported on Si. By reconstructing diffraction patterns from the 2110 Bragg peak, we show that the lattice orientation varies along the length of the wire, while the strain field along the cross-section is largelymore » unaffected, leaving the band structure unperturbed. Diffraction patterns from the 0110 Bragg peak are reproducibly reconstructed to create three-dimensional images of stacking defects and associated lattice strains, revealing sharp planar boundaries between different crystal phases of wurtzite (WZ) structure that contribute to charge carrier scattering. Phase retrieval is made possible by developing multiangle Bragg projection ptychography (maBPP) to accommodate coherent nanodiffraction patterns measured at arbitrary overlapping positions at multiple angles about a Bragg peak, eliminating the need for scan registration at different angles. The penetrating nature of X-ray radiation, together with the relaxed constraints of maBPP, will enable the in operando imaging of nanowire devices.« less

X-ray studies of dynamic aging in an aluminum alloy subjected to severe plastic deformation

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

Sitdikov, V.D., E-mail: svil@mail.rb.ru; Laboratory for Mechanics of Bulk Nanomaterials, Saint Petersburg State University, 28 Universitetsky pr., Saint Petersburg 198504; Chizhov, P.S.

In this work, X-ray scattering methods were applied for a quantitative characterization of the microstructure of an aluminum alloy of the Al–Mg–Si system during dynamic aging realized through the high pressure torsion technique. A qualitative and quantitative phase analysis of the alloy was performed, together with Al alloy lattice parameter determination. From the reflections broadening the effective size of the coherent scattering domains and the lattice microstrain were determined in the framework of the Halder–Wagner approach. Using the method of small-angle X-ray scattering, the quantitative characteristics of the size, shape and spatial distribution of the secondary phase particles formed inmore » the Al alloy during dynamic aging were established. In order to validate the obtained results, the method of small-angle X-ray scattering was preliminarily tested on similar samples after artificial aging and compared with the results from small-angle neutron diffraction widely known in literature. - Highlights: • Spherical fcc β-Mg2Si precipitates formed in Al 6201 alloy during dynamic aging in the course of severe plastic deformation. • The size, shape and distribution of the precipitates due to artificial and dynamic aging were revealed by SAXS method. • Monoclinic needle-like β' precipitates and Al5FeSi intermetallic phase were detected in 6201 alloy after T6 treatment.« less

X-ray Photoelectron Spectroscopy (XPS), Rutherford Back Scattering (RBS) studies

NASA Technical Reports Server (NTRS)

Neely, W. C.; Bozak, M. J.; Williams, J. R.

1993-01-01

X-ray photoelectron spectroscopy (XPS), Rutherford Back Scattering (RBS) studies of each of sample received were completed. Since low angle X-ray could not be performed because of instrumentation problems, Auger spectrometry was employed instead. The results of these measurements for each of the samples is discussed in turn.

Single-pulse x-ray diffraction using polycapillary optics for in situ dynamic diffraction

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

Maddox, B. R., E-mail: maddox3@llnl.gov; Akin, M. C., E-mail: akin1@llnl.gov; Teruya, A.

2016-08-15

Diagnostic use of single-pulse x-ray diffraction (XRD) at pulsed power facilities can be challenging due to factors such as the high flux and brightness requirements for diffraction and the geometric constraints of experimental platforms. By necessity, the x-ray source is usually positioned very close, within a few inches of the sample. On dynamic compression platforms, this puts the x-ray source in the debris field. We coupled x-ray polycapillary optics to a single-shot needle-and-washer x-ray diode source using a laser-based alignment scheme to obtain high-quality x-ray diffraction using a single 16 ns x-ray pulse with the source >1 m from themore » sample. The system was tested on a Mo sample in reflection geometry using 17 keV x-rays from a Mo anode. We also identified an anode conditioning effect that increased the x-ray intensity by 180%. Quantitative measurements of the x-ray focal spot produced by the polycapillary yielded a total x-ray flux on the sample of 3.3 ± 0.5 × 10{sup 7} molybdenum Kα photons.« less

Super-resolution biomolecular crystallography with low-resolution data.

PubMed

Schröder, Gunnar F; Levitt, Michael; Brunger, Axel T

2010-04-22

X-ray diffraction plays a pivotal role in the understanding of biological systems by revealing atomic structures of proteins, nucleic acids and their complexes, with much recent interest in very large assemblies like the ribosome. As crystals of such large assemblies often diffract weakly (resolution worse than 4 A), we need methods that work at such low resolution. In macromolecular assemblies, some of the components may be known at high resolution, whereas others are unknown: current refinement methods fail as they require a high-resolution starting structure for the entire complex. Determining the structure of such complexes, which are often of key biological importance, should be possible in principle as the number of independent diffraction intensities at a resolution better than 5 A generally exceeds the number of degrees of freedom. Here we introduce a method that adds specific information from known homologous structures but allows global and local deformations of these homology models. Our approach uses the observation that local protein structure tends to be conserved as sequence and function evolve. Cross-validation with R(free) (the free R-factor) determines the optimum deformation and influence of the homology model. For test cases at 3.5-5 A resolution with known structures at high resolution, our method gives significant improvements over conventional refinement in the model as monitored by coordinate accuracy, the definition of secondary structure and the quality of electron density maps. For re-refinements of a representative set of 19 low-resolution crystal structures from the Protein Data Bank, we find similar improvements. Thus, a structure derived from low-resolution diffraction data can have quality similar to a high-resolution structure. Our method is applicable to the study of weakly diffracting crystals using X-ray micro-diffraction as well as data from new X-ray light sources. Use of homology information is not restricted to X-ray crystallography and cryo-electron microscopy: as optical imaging advances to subnanometre resolution, it can use similar tools.

Coded diffraction system in X-ray crystallography using a boolean phase coded aperture approximation

NASA Astrophysics Data System (ADS)

Pinilla, Samuel; Poveda, Juan; Arguello, Henry

2018-03-01

Phase retrieval is a problem present in many applications such as optics, astronomical imaging, computational biology and X-ray crystallography. Recent work has shown that the phase can be better recovered when the acquisition architecture includes a coded aperture, which modulates the signal before diffraction, such that the underlying signal is recovered from coded diffraction patterns. Moreover, this type of modulation effect, before the diffraction operation, can be obtained using a phase coded aperture, just after the sample under study. However, a practical implementation of a phase coded aperture in an X-ray application is not feasible, because it is computationally modeled as a matrix with complex entries which requires changing the phase of the diffracted beams. In fact, changing the phase implies finding a material that allows to deviate the direction of an X-ray beam, which can considerably increase the implementation costs. Hence, this paper describes a low cost coded X-ray diffraction system based on block-unblock coded apertures that enables phase reconstruction. The proposed system approximates the phase coded aperture with a block-unblock coded aperture by using the detour-phase method. Moreover, the SAXS/WAXS X-ray crystallography software was used to simulate the diffraction patterns of a real crystal structure called Rhombic Dodecahedron. Additionally, several simulations were carried out to analyze the performance of block-unblock approximations in recovering the phase, using the simulated diffraction patterns. Furthermore, the quality of the reconstructions was measured in terms of the Peak Signal to Noise Ratio (PSNR). Results show that the performance of the block-unblock phase coded apertures approximation decreases at most 12.5% compared with the phase coded apertures. Moreover, the quality of the reconstructions using the boolean approximations is up to 2.5 dB of PSNR less with respect to the phase coded aperture reconstructions.

X-ray absorption microtomography (microCT) and small beam diffraction mapping of sea urchin teeth.

PubMed

Stock, S R; Barss, J; Dahl, T; Veis, A; Almer, J D

2002-07-01

Two noninvasive X-ray techniques, laboratory X-ray absorption microtomography (microCT) and X-ray diffraction mapping, were used to study teeth of the sea urchin Lytechinus variegatus. MicroCT revealed low attenuation regions at near the tooth's stone part and along the carinar process-central prism boundary; this latter observation appears to be novel. The expected variation of Mg fraction x in the mineral phase (calcite, Ca(1-x)Mg(x)CO(3)) cannot account for all of the linear attenuation coefficient decrease in the two zones: this suggested that soft tissue is localized there. Transmission diffraction mapping (synchrotron X-radiation, 80.8 keV, 0.1 x 0.1mm(2) beam area, 0.1mm translation grid, image plate area detector) simultaneously probed variations in 3-D and showed that the crystal elements of the "T"-shaped tooth were very highly aligned. Diffraction patterns from the keel (adaxial web) and from the abaxial flange (containing primary plates and the stone part) differed markedly. The flange contained two populations of identically oriented crystal elements with lattice parameters corresponding to x=0.13 and x=0.32. The keel produced one set of diffraction spots corresponding to the lower x. The compositions were more or less equivalent to those determined by others for camarodont teeth, and the high Mg phase is expected to be disks of secondary mineral epitaxially related to the underlying primary mineral element. Lattice parameter gradients were not noted in the keel or flange. Taken together, the microCT and diffraction results indicated that there was a band of relatively high protein content, of up to approximately 0.25 volume fraction, in the central part of the flange and paralleling its adaxial and abaxial faces. X-ray microCT and microdiffraction data used in conjunction with protein distribution data will be crucial for understanding the properties of various biocomposites and their mechanical functions.

A comparison of glycosaminoglycan distributions, keratan sulphate sulphation patterns and collagen fibril architecture from central to peripheral regions of the bovine cornea

PubMed Central

Ho, Leona T.Y.; Harris, Anthony M.; Tanioka, Hidetoshi; Yagi, Naoto; Kinoshita, Shigeru; Caterson, Bruce; Quantock, Andrew J.; Young, Robert D.; Meek, Keith M.

2014-01-01

This study investigated changes in collagen fibril architecture and the sulphation status of keratan sulphate (KS) glycosaminoglycan (GAG) epitopes from central to peripheral corneal regions. Freshly excised adult bovine corneal tissue was examined as a function of radial position from the centre of the cornea outwards. Corneal thickness, tissue hydration, hydroxyproline content, and the total amount of sulphated GAG were all measured. High and low-sulphated epitopes of keratan sulphate were studied by immunohistochemistry and quantified by ELISA. Chondroitin sulphate (CS) and dermatan sulphate (DS) distributions were observed by immunohistochemistry following specific enzyme digestions. Electron microscopy and X-ray fibre diffraction were used to ascertain collagen fibril architecture. The bovine cornea was 1021 ± 5.42 μm thick at its outer periphery, defined as 9–12 mm from the corneal centre, compared to 844 ± 8.10 μm at the centre. The outer periphery of the cornea was marginally, but not significantly, more hydrated than the centre (H = 4.3 vs. H = 3.7), and was more abundant in hydroxyproline (0.12 vs. 0.06 mg/mg dry weight of cornea). DMMB assays indicated no change in the total amount of sulphated GAG across the cornea. Immunohistochemistry revealed the presence of both high- and low-sulphated epitopes of KS, as well as DS, throughout the cornea, and CS only in the peripheral cornea before the limbus. Quantification by ELISA, disclosed that although both high- and low-sulphated KS remained constant throughout stromal depth at different radial positions, high-sulphated epitopes remained constant from the corneal centre to outer-periphery, whereas low-sulphated epitopes increased significantly. Both small angle X-ray diffraction and TEM analysis revealed that collagen fibril diameter remained relatively constant until the outer periphery was reached, after which fibrils became more widely spaced (from small angle x-ray diffraction analysis) and of larger diameter as they approached the sclera. Depth-profiled synchrotron microbeam analyses showed that, at different radial positions from the corneal centre outwards, fibril diameter was greater superficially than in deeper stromal regions. The interfibrillar spacing was also higher at mid-depth in the stroma than it was in anterior and posterior stromal regions. Collagen fibrils in the bovine cornea exhibited a fairly consistent spacing and diameter from the corneal centre to the 12 mm radial position, after which a significant increase was seen. While the constancy of the overall sulphation levels of proteoglycans in the cornea may correlate with the fibrillar architecture, there was no correlation between the latter and the distribution of low-sulphated KS. PMID:25019467

Combined operando X-ray diffraction-electrochemical impedance spectroscopy detecting solid solution reactions of LiFePO4 in batteries.

PubMed

Hess, Michael; Sasaki, Tsuyoshi; Villevieille, Claire; Novák, Petr

2015-09-08

Lithium-ion batteries are widely used for portable applications today; however, often suffer from limited recharge rates. One reason for such limitation can be a reduced active surface area during phase separation. Here we report a technique combining high-resolution operando synchrotron X-ray diffraction coupled with electrochemical impedance spectroscopy to directly track non-equilibrium intermediate phases in lithium-ion battery materials. LiFePO4, for example, is known to undergo phase separation when cycled under low-current-density conditions. However, operando X-ray diffraction under ultra-high-rate alternating current and direct current excitation reveal a continuous but current-dependent, solid solution reaction between LiFePO4 and FePO4 which is consistent with previous experiments and calculations. In addition, the formation of a preferred phase with a composition similar to the eutectoid composition, Li0.625FePO4, is evident. Even at a low rate of 0.1C, ∼20% of the X-ray diffractogram can be attributed to non-equilibrium phases, which changes our understanding of the intercalation dynamics in LiFePO4.

Étude de la structure des alliages vitreux Ag-As2S3 par diffraction de rayons X

NASA Astrophysics Data System (ADS)

Popescu, M.; Sava, F.; Cornet, A.; Broll, N.

2002-07-01

The structure of several silver alloyed arsenic chalocgenide has been determined by X-ray diffraction. For low silver doping the disordered layer structure, characteristic to the glassy AS2S3 is retained as demonstrated by the well developed first sharp diffraction peak in the X-ray diffraction pattern. For high amount of silver introduced in the As2S3 matrix, the disoredered layer configurations disappear, as shown by the diminishing and even disappearance of the first sharp diffraction peak in the X-ray patterns. A three-dimensional structure based on Ag2S -type configuration is formed. La structure de quelques alliages sulfure d'arsenic - argent a été determinée par diffraction de rayons X. Pour de faibles dopages à l'argent on conserve la structure desordonnées caractéristique des couches atomique d'As2S3 vitreux ; ceci est prouvé par la forte intensité du premier pic étroit de diffraction. Pour des plus grandes proportions d'argent la structure de l'alliage vitreux fait apparaître des unités structurales caractéristiques du cristal d'Ag2S et la configuration atomique avec des couches desordonnées disparaît (le premier pic étroit de diffraction s'évanouit) en faisant place à une structure tridimensionelle.

Phase transformation of dental zirconia following artificial aging.

PubMed

Lucas, Thomas J; Lawson, Nathaniel C; Janowski, Gregg M; Burgess, John O

2015-10-01

Low-temperature degradation (LTD) of yttria-stabilized zirconia can produce increased surface roughness with a concomitant decrease in strength. This study determined the effectiveness of artificial aging (prolonged boiling/autoclaving) to induce LTD of Y-TZP (yttria-tetragonal zirconia-polycrystals) and used artificial aging for transformation depth progression analyses. The null hypothesis is aging techniques tested produce the same amount of transformation, transformation is not time/temperature dependent and LTD causes a constant transformation throughout the Y-TZP samples. Dental-grade Y-TZP samples were randomly divided into nine subgroups (n = 5): as received, 3.5 and 7 day boiling, 1 bar autoclave (1, 3, 5 h), and 2 bar autoclave (1, 3, 5 h). A 4-h boil treatment (n = 2) was performed post-experiment for completion of data. Transformation was measured using traditional X-ray diffraction and low-angle X-ray diffraction. The fraction of t → m transformation increased with aging time. The 3.5 day boil and 2 bar 5 h autoclave produced similar transformation results, while the 7 day boiling treatment revealed the greatest transformation. The surface layer of the aged specimen underwent the most transformation while all samples displayed decreasing transformation with depth. Surface transformation was evident, which can lead to rougher surfaces and increased wear of opposing dentition/materials. Therefore, wear studies addressing LTD of Y-TZP are needed utilizing accelerated aging. © 2014 Wiley Periodicals, Inc.

Advanced High Brilliance X-Ray Source

NASA Technical Reports Server (NTRS)

Gibson, Walter M.

1998-01-01

The possibility to dramatically increase the efficiency of laboratory based protein structure measurements through the use of polycapillary X-ray optics was investigated. This project initiated April 1, 1993 and concluded December 31, 1996 (including a no cost extension from June 31, 1996). This is a final report of the project. The basis for the project is the ability to collect X-rays from divergent electron bombardment laboratory X-ray sources and redirect them into quasiparallel or convergent (focused) beams. For example, a 0.1 radian (approx. 6 deg) portion of a divergent beam collected by a polycapillary collimator and transformed into a quasiparallel beam of 3 millradian (0.2 deg) could give a gain of 6(exp 2)/0.2(exp 2) x T for the intensity of a diffracted beam from a crystal with a 0.2 deg diffraction width. T is the transmission efficiency of the polycapillary diffraction optic, and for T=0.5, the gain would be 36/0.04 x O.5=45. In practice, the effective collection angle will depend on the source spot size, the input focal length of the optic (usually limited by the source spot-to-window distance on the x-ray tube) and the size of the crystal relative to the output diameter of the optic. The transmission efficiency, T, depends on the characteristics (fractional open area, surface roughness, shape and channel diameter) of the polycapillary optic and is typically in the range 0.2-0.4. These effects could substantially reduce the expected efficiency gain. During the course of this study, the possibility to use a weakly focused beam (0.5 deg convergence) was suggested which could give an additional 10-20 X efficiency gain for small samples . Weakly focused beams from double focusing mirrors are frequently used for macromolecular crystallography studies. Furthermore the crystals are typically oscillated by as much as 2 deg during each X-ray exposure in order to increase the reciprocal space (number of crystal planes) sampled and use of a slightly convergent beam could, in principle, provide a similar sampling benefit without oscillation. Although more problematic, because of complications in analyzing the diffraction patterns, it was also suggested that even more extreme beam convergence might be used to give another order of magnitude intensity gain and even smaller focused spot size which could make it possible to study smaller protein crystals than can be studied using standard laboratory based X-ray diffraction systems. This project represents the first systematic investigation of these possibilities. As initially proposed, the contract included requirements for design, purchase, evaluation and delivery of three polycapillary lenses to the Laboratory for Structural Biology at MSFC and demonstration of such optics at MSFC for selected protein crystal diffraction applications.

Compact energy dispersive X-ray microdiffractometer for diagnosis of neoplastic tissues

NASA Astrophysics Data System (ADS)

Sosa, C.; Malezan, A.; Poletti, M. E.; Perez, R. D.

2017-08-01

An energy dispersive X-ray microdiffractometer with capillary optics has been developed for characterizing breast cancer. The employment of low divergence capillary optics helps to reduce the setup size to a few centimeters, while providing a lateral spatial resolution of 100 μm. The system angular calibration and momentum transfer resolution were assessed by a detailed study of a polycrystalline reference material. The performance of the system was tested by means of the analysis of tissue-equivalent samples previously characterized by conventional X-ray diffraction. In addition, a simplified correction model for an appropriate comparison of the diffraction spectra was developed and validated. Finally, the system was employed to evaluate normal and neoplastic human breast samples, in order to determine their X-ray scatter signatures. The initial results indicate that the use of this compact energy dispersive X-ray microdiffractometer combined with a simplified correction procedure is able to provide additional information to breast cancer diagnosis.

Sharp chemical interface in epitaxial Fe{sub 3}O{sub 4} thin films

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

Gálvez, S.; Rubio-Zuazo, J., E-mail: rubio@esrf.fr; Salas-Colera, E.

Chemically sharp interface was obtained on single phase single oriented Fe{sub 3}O{sub 4} (001) thin film (7 nm) grown on NiO (001) substrate using oxygen assisted molecular beam epitaxy. Refinement of the atomic structure, stoichiometry, and oxygen vacancies were determined by soft and hard x-ray photoelectron spectroscopy, low energy electron diffraction and synchrotron based X-ray reflectivity, and X-ray diffraction. Our results demonstrate an epitaxial growth of the magnetite layer, perfect iron stoichiometry, absence of oxygen vacancies, and the existence of an intermixing free interface. Consistent magnetic and electrical characterizations are also shown.

Low-temperature structure transition in hexagonal LuFeO3

NASA Astrophysics Data System (ADS)

Xu, Xiaoshan; Wang, Wenbin; Wang, Xiao; Zhu, Leyi; Kim, Jong-Woo; Ryan, Phillip; Keavney, David; Ward, Thomas; Shen, Jian; Cheng, Xuemei

2014-03-01

The structural change of h-LuFeO3 films at low temperature has been studied using x-ray diffraction and x-ray absorption experiments. The results are analyzed using the displacements of three phonon modes that are related to the P63/mmc to P63cm structural transition. The data indicate that the in-plane motion of the Fe and apex oxygen are responsible for the observed anomaly in both x-ray absorption and diffraction experiments. This subtle structural transition may be an origin of the low temperature magnetic phase transition at TR=130 K. Research supported by US DOE, Office of Basic Energy Sciences, Materials Science and Engineering Division. Work at BMC is supported by NSF Career award (DMR 1053854). Work at ANL is supported by US-DOE, Office of Science, BES (No. DE-AC02-06CH11357).

Optics for coherent X-ray applications.

PubMed

Yabashi, Makina; Tono, Kensuke; Mimura, Hidekazu; Matsuyama, Satoshi; Yamauchi, Kazuto; Tanaka, Takashi; Tanaka, Hitoshi; Tamasaku, Kenji; Ohashi, Haruhiko; Goto, Shunji; Ishikawa, Tetsuya

2014-09-01

Developments of X-ray optics for full utilization of diffraction-limited storage rings (DLSRs) are presented. The expected performance of DLSRs is introduced using the design parameters of SPring-8 II. To develop optical elements applicable to manipulation of coherent X-rays, advanced technologies on precise processing and metrology were invented. With propagation-based coherent X-rays at the 1 km beamline of SPring-8, a beryllium window fabricated with the physical-vapour-deposition method was found to have ideal speckle-free properties. The elastic emission machining method was utilized for developing reflective mirrors without distortion of the wavefronts. The method was further applied to production of diffraction-limited focusing mirrors generating the smallest spot size in the sub-10 nm regime. To enable production of ultra-intense nanobeams at DLSRs, a low-vibration cooling system for a high-heat-load monochromator and advanced diagnostic systems to characterize X-ray beam properties precisely were developed. Finally, new experimental schemes for combinative nano-analysis and spectroscopy realised with novel X-ray optics are discussed.

Effect of Pressure on Valence and Structural Properties of YbFe 2 Ge 2 Heavy Fermion Compound—A Combined Inelastic X-ray Spectroscopy, X-ray Diffraction, and Theoretical Investigation

DOE PAGES

Kumar, Ravhi S.; Svane, Axel; Vaitheeswaran, Ganapathy; ...

2015-10-19

We measured the crystal structure and the Yb valence of the YbFe 2Ge 2 heavy fermion compound at room temperature and under high pressures using high-pressure powder X-ray diffraction and X-ray absorption spectroscopy via both partial fluorescence yield and resonant inelastic X-ray emission techniques. Moreover, the measurements are complemented by first-principles density functional theoretical calculations using the self-interaction corrected local spin density approximation investigating in particular the magnetic structure and the Yb valence. Finally, while the ThCr 2Si 2-type tetragonal (I4/mmm) structure is stable up to 53 GPa, the X-ray emission results show an increase of the Yb valence frommore » v = 2.72(2) at ambient pressure to v = 2.93(3) at ~9 GPa, where at low temperature a pressure-induced quantum critical state was reported.« less

X-Ray Diffraction Apparatus

NASA Technical Reports Server (NTRS)

Blake, David F. (Inventor); Bryson, Charles (Inventor); Freund, Friedmann (Inventor)

1996-01-01

An x-ray diffraction apparatus for use in analyzing the x-ray diffraction pattern of a sample is introduced. The apparatus includes a beam source for generating a collimated x-ray beam having one or more discrete x-ray energies, a holder for holding the sample to be analyzed in the path of the beam, and a charge-coupled device having an array of pixels for detecting, in one or more selected photon energy ranges, x-ray diffraction photons produced by irradiating such a sample with said beam. The CCD is coupled to an output unit which receives input information relating to the energies of photons striking each pixel in the CCD, and constructs the diffraction pattern of photons within a selected energy range striking the CCD.

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

Shin, Kyung -Wook; Karim, Karim S.

Direct conversion crystalline silicon X-ray imagers are used for low-energy X-ray photon (4-20 keV) detection in scientific research applications such as protein crystallography. In this paper, we demonstrate a novel pixel architecture that integrates a crystalline silicon X-ray detector with a thin-film transistor amorphous silicon pixel readout circuit. We describe a simplified two-mask process to fabricate a complete imaging array and present preliminary results that show the fabricated pixel to be sensitive to 5.89-keV photons from a low activity Fe-55 gamma source. Furthermore, this paper presented can expedite the development of high spatial resolution, low cost, direct conversion imagers formore » X-ray diffraction and crystallography applications.« less

Self-standing crystalline TiO2 nanotubes/CNTs heterojunction membrane: synthesis and characterization.

PubMed

Hesabi, Zohreh R; Allam, Nageh K; Dahmen, Klaus; Garmestani, Hamid; A El-Sayed, Mostafa

2011-04-01

In the present study, we report for the first time synthesis of TiO(2) nanotubes/CNTs heterojunction membrane. Chemical vapor deposition (CVD) of CNTs at 650 °C in a mixture of H(2)/He atmosphere led to in situ detachment of the anodically fabricated TiO(2) nanotube layers from the Ti substrate underneath. Morphological and structural evolution of TiO(2) nanotubes after CNTs deposition were investigated by field- emission scanning electron microscopy (FESEM), glancing angle X-ray diffraction (GAXRD), and X-ray photoelectron spectroscopy (XPS) analyses. © 2011 American Chemical Society

A CMOS-based large-area high-resolution imaging system for high-energy x-ray applications

NASA Astrophysics Data System (ADS)

Rodricks, Brian; Fowler, Boyd; Liu, Chiao; Lowes, John; Haeffner, Dean; Lienert, Ulrich; Almer, John

2008-08-01

CCDs have been the primary sensor in imaging systems for x-ray diffraction and imaging applications in recent years. CCDs have met the fundamental requirements of low noise, high-sensitivity, high dynamic range and spatial resolution necessary for these scientific applications. State-of-the-art CMOS image sensor (CIS) technology has experienced dramatic improvements recently and their performance is rivaling or surpassing that of most CCDs. The advancement of CIS technology is at an ever-accelerating pace and is driven by the multi-billion dollar consumer market. There are several advantages of CIS over traditional CCDs and other solid-state imaging devices; they include low power, high-speed operation, system-on-chip integration and lower manufacturing costs. The combination of superior imaging performance and system advantages makes CIS a good candidate for high-sensitivity imaging system development. This paper will describe a 1344 x 1212 CIS imaging system with a 19.5μm pitch optimized for x-ray scattering studies at high-energies. Fundamental metrics of linearity, dynamic range, spatial resolution, conversion gain, sensitivity are estimated. The Detective Quantum Efficiency (DQE) is also estimated. Representative x-ray diffraction images are presented. Diffraction images are compared against a CCD-based imaging system.

X-ray diffraction of solid tin to 1.2 TPa

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

Lazicki, A.; Rygg, J. R.; Coppari, F.

2015-08-12

In this study, we report direct in situ measurements of the crystal structure of tin between 0.12 and 1.2 TPa, the highest stress at which a crystal structure has ever been observed. Using angle-dispersive powder x-ray diffraction, we find that dynamically compressed Sn transforms to the body-centered-cubic (bcc) structure previously identified by ambient-temperature quasistatic-compression studies and by zero-kelvin density-functional theory predictions between 0.06 and 0.16 TPa. However, we observe no evidence for the hexagonal close-packed (hcp) phase found by those studies to be stable above 0.16 TPa. Instead, our results are consistent with bcc up to 1.2 TPa. We conjecturemore » that at high temperature bcc is stabilized relative to hcp due to differences in vibrational free energy.« less

Crystal Structure of Two V-shaped Ligands with N-Heterocycles

NASA Astrophysics Data System (ADS)

Wang, Gao-Feng; Sun, Shu-Wen; Zhang, Xiao; Sun, Shu-Gang

2017-12-01

Two V-shaped ligands with N-heterocycles, bis(4-(1 H-imidazol-1-yl) phenyl)methanone ( 1), and bis(4-(1 H-benzo[d]imidazol-1-yl)phenyl)methanone ( 2) have been synthesized and characterized by elemental analyses, IR and 1 H NMR spectroscopy. Crystal structures of 1 and 2 have been determined by X-ray diffraction. The crystal of 1 is monoclinic, sp. gr. P21/ c, Z = 4. The crystal of 2 is orthorhombic, sp. gr. Fdd2, Z = 8. X-ray diffraction analyses show that the V-shaped angles of 1 and 2 are 122.72(15)° and 120.7(4)°, respectively. Intermolecular C-H···O, C-H···N, C-H···π, and π···π interactions link the components into three-dimensional networks in the crystal structures.

Single shot speckle and coherence analysis of the hard X-ray free electron laser LCLS

DOE PAGES

Lee, Sooheyong; Roseker, W.; Gutt, C.; ...

2013-10-08

The single shot based coherence properties of hard x-ray pulses from the Linac Coherent Light Source (LCLS) were measured by analyzing coherent diffraction patterns from nano-particles and gold nanopowder. The intensity histogram of the small angle x-ray scattering ring from nano-particles reveals the fully transversely coherent nature of the LCLS beam with a number of transverse modemore » $$\\langle$$M s$$\\rangle$$ = 1.1. On the other hand, the speckle contrasts measured at a large wavevector yields information about the longitudinal coherence of the LCLS radiation after a silicon (111) monochromator. The quantitative agreement between our data and the simulation confirms a mean coherence time of 2.2 fs and a x-ray pulse duration of 29 fs. Lastly the observed reduction of the speckle contrast generated by x-rays with pulse duration longer than 30 fs indicates ultrafast dynamics taking place at an atomic length scale prior to the permanent sample damage.« less

Test and Delivery of the Chemin Mineralogical Instrument for Mars Science Laboratory

NASA Technical Reports Server (NTRS)

Blake, D. F.; Vaniman, D.; Anderson, R.; Bish, D.; Chipera, S.; Chemtob, S.; Crisp, J.; DesMarais, D. J.; Downs, R.; Feldman, S.;

Characterization of TiN/B-C-N multilayers by transmission electron microscopy, ion beam backscattering, and low angle x-ray diffraction

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

Kung, H.; Fayeulle, S.; Nastasi, M.

1997-10-01

The effects of Ar ion irradiation on the structure and stability of multilayered DC sputtered thin films of TiN/B-C-N have been studied. An increase of the bilayer repeat length to a maximum of 12.8% and departure of nitrogen from the film was observed indicating the interdiffusion between TiN and B-C-N layers. For the highest dose (5 {times} 10{sup 16} ions/cm{sup 2}) the multilayered structure partly disappears. The various mechanisms are discussed in terms of stress-driven diffusion and viscous flow of atoms.

Real-time X-ray Diffraction: Applications to Materials Characterization

NASA Technical Reports Server (NTRS)

Rosemeier, R. G.

1984-01-01

With the high speed growth of materials it becomes necessary to develop measuring systems which also have the capabilities of characterizing these materials at high speeds. One of the conventional techniques of characterizing materials was X-ray diffraction. Film, which is the oldest method of recording the X-ray diffraction phenomenon, is not quite adequate in most circumstances to record fast changing events. Even though conventional proportional counters and scintillation counters can provide the speed necessary to record these changing events, they lack the ability to provide image information which may be important in some types of experiment or production arrangements. A selected number of novel applications of using X-ray diffraction to characterize materials in real-time are discussed. Also, device characteristics of some X-ray intensifiers useful in instantaneous X-ray diffraction applications briefly presented. Real-time X-ray diffraction experiments with the incorporation of image X-ray intensification add a new dimension in the characterization of materials. The uses of real-time image intensification in laboratory and production arrangements are quite unlimited and their application depends more upon the ingenuity of the scientist or engineer.

Long Periodic Structure of a Room-Temperature Ionic Liquid by High-Pressure Small-Angle X-Ray Scattering and Wide-Angle X-Ray Scattering: 1-Decyl-3-Methylimidazolium Chloride.

PubMed

Abe, Hiroshi; Hamaya, Nozomu; Koyama, Yoshihiro; Kishimura, Hiroaki; Takekiyo, Takahiro; Yoshimura, Yukihiro; Wakabayashi, Daisuke; Funamori, Nobumasa; Matsuishi, Kiyoto

2018-04-23

The Bragg reflections of 1-decyl-3-methylimidazolium chloride ([C 10 mim][Cl]), a room-temperature ionic liquid, are observed in a lowly scattered wavevector (q) region using high-pressure (HP) small-angle X-ray scattering methods. The HP crystal of [C 10 mim][Cl] was characterized by an extremely long periodic structure. The peak position at the lowest q (1.4 nm -1 ) was different from that of the prepeak observed in the liquid state (2.3 nm -1 ). Simultaneously, Bragg reflections at high-q were detected using HP wide-angle X-ray scattering. The longest lattice constant was estimated to be 4.3 nm using structural analysis. The crystal structure of HP differed from that of the low-temperature (LT) crystal and the LT liquid crystal. With increasing pressure, Bragg reflections in the high-q component became much broader, and were accompanied by phase transition, although those in the low-q component were observed to be relatively sharp. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

The investigation of order–disorder transition process of ZSM-5 induced by spark plasma sintering

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

Wang, Liang; Wang, Lianjun, E-mail: wanglj@dhu.edu.cn; Jiang, Wan

2014-04-01

Based on the amorphization of zeolites, an order–disorder transition method was used to prepare silica glass via Spark Plasma Sintering (SPS). In order to get a better understanding about the mechanism of amorphization induced by SPS, the intermediate products in this process were prepared and characterized by different characterization techniques. X-ray diffraction and High-energy synchrotron X-ray scattering show a gradual transformation from ordered crystal to glass. Local structural changes in glass network including Si–O bond length, O–Si–O bond angle, size of rings, coordination were detected by Infrared spectroscopy and {sup 29}Si magic-angle spinning nuclear magnetic resonance (NMR) spectroscopy. Topologically ordered,more » amorphous material with a different intermediate-range structure can be obtained by precise control of intermediate process which can be expected to optimize and design material. - Graphical abstract: Low-density, ordered zeolites collapse to the rigid amorphous glass through spark plasma sintering. The intermediate-range structure formed in the process of order–disorder transition may give rise to specific property. - Highlights: • Order–disorder transition process of ZSM-5 induced by spark plasma sintering was investigated using several methods including XRD, High-energy synchrotron X-ray scattering, SAXS, IR, NMR, ect. • Order–disorder transition induced by SPS was compared with TIA and PIA. • Three stages has been divided during the whole process. • The collapse temperature range which may give rise to intermediate-range structure has been located.« less

Integrating macromolecular X-ray diffraction data with the graphical user interface iMOSFLM

PubMed Central

Powell, Harold R; Battye, T Geoff G; Kontogiannis, Luke; Johnson, Owen; Leslie, Andrew GW

2017-01-01

X-ray crystallography is the overwhelmingly dominant source of structural information for biological macromolecules, providing fundamental insights into biological function. Collection of X-ray diffraction data underlies the technique, and robust and user-friendly software to process the diffraction images makes the technique accessible to a wider range of scientists. iMosflm/MOSFLM (www.mrc-lmb.cam.ac.uk/harry/imosflm) is a software package designed to achieve this goal. The graphical user interface (GUI) version of MOSFLM (called iMosflm) is designed to guide inexperienced users through the steps of data integration, while retaining powerful features for more experienced users. Images from almost all commercially available X-ray detectors can be handled. Although the program only utilizes two-dimensional profile fitting, it can readily integrate data collected in “fine phi-slicing” mode (where the rotation angle per image is less than the crystal mosaic spread by a factor of at least 2) that is commonly employed with modern very fast readout detectors. The graphical user interface provides real-time feedback on the success of the indexing step and the progress of data processing. This feedback includes the ability to monitor detector and crystal parameter refinement and to display the average spot shape in different regions of the detector. Data scaling and merging tasks can be initiated directly from the interface. Using this protocol, a dataset of 360 images with ~2000 reflections per image can be processed in approximately four minutes. PMID:28569763

Synchrotron Radiation X-ray Diffraction Techniques Applied to Insect Flight Muscle.

PubMed

Iwamoto, Hiroyuki

2018-06-13

X-ray fiber diffraction is a powerful tool used for investigating the molecular structure of muscle and its dynamics during contraction. This technique has been successfully applied not only to skeletal and cardiac muscles of vertebrates but also to insect flight muscle. Generally, insect flight muscle has a highly ordered structure and is often capable of high-frequency oscillations. The X-ray diffraction studies on muscle have been accelerated by the advent of 3rd-generation synchrotron radiation facilities, which can generate brilliant and highly oriented X-ray beams. This review focuses on some of the novel experiments done on insect flight muscle by using synchrotron radiation X-rays. These include diffraction recordings from single myofibrils within a flight muscle fiber by using X-ray microbeams and high-speed diffraction recordings from the flight muscle during the wing-beat of live insects. These experiments have provided information about the molecular structure and dynamic function of flight muscle in unprecedented detail. Future directions of X-ray diffraction studies on muscle are also discussed.

Low-temperature high magnetic field powder x-ray diffraction setup for field-induced structural phase transition studies from 2 to 300 K and at 0 to 8-T field

NASA Astrophysics Data System (ADS)

Shahee, Aga; Sharma, Shivani; Kumar, Dhirendra; Yadav, Poonam; Bhardwaj, Preeti; Ghodke, Nandkishor; Singh, Kiran; Lalla, N. P.; Chaddah, P.

2016-10-01

A low-temperature and high magnetic field powder x-ray diffractometer (XRD) has been developed at UGC-DAE CSR (UGC: University Grant Commission, DAE: Department of Atomic Energy, and CSR: Consortium for scientific research), Indore, India. The setup has been developed around an 18 kW rotating anode x-ray source delivering Cu-Kα x-rays coming from a vertical line source. It works in a symmetric θ-2θ parallel beam geometry. It consists of a liquid helium cryostat with an 8 T split-pair Nb-Ti superconducting magnet comprising two x-ray windows each covering an angular range of 65°. This is mounted on a non-magnetic type heavy duty goniometer equipped with all necessary motions along with data collection accessories. The incident x-ray beam has been made parallel using a parabolic multilayer mirror. The scattered x-ray is detected using a NaI detector through a 0.1° acceptance solar collimator. To control the motions of the goniometer, a computer programme has been developed. The wide-angle scattering data can be collected in a range of 2°-115° of 2θ with a resolution of ˜0.1°. The whole setup is tightly shielded for the scattered x-rays using a lead hutch. The functioning of the goniometer and the artifacts arising possibly due to the effect of stray magnetic field on the goniometer motions, on the x-ray source, and on the detector have been characterized by collecting powder XRD data of a National Institute of Standards and Technology certified standard reference material LaB6 (SRM-660b) and Si powder in zero-field and in-field conditions. Occurrence of field induced structural-phase transitions has been demonstrated on various samples like Pr0.5Sr0.5MnO3, Nd0.49Sr0.51MnO3-δ and La0.175Pr0.45Ca0.375MnO3 by collecting data in zero field cool and field cool conditions.

Complementary uses of small angle X-ray scattering and X-ray crystallography.

PubMed

Pillon, Monica C; Guarné, Alba

2017-11-01

Most proteins function within networks and, therefore, protein interactions are central to protein function. Although stable macromolecular machines have been extensively studied, dynamic protein interactions remain poorly understood. Small-angle X-ray scattering probes the size, shape and dynamics of proteins in solution at low resolution and can be used to study samples in a large range of molecular weights. Therefore, it has emerged as a powerful technique to study the structure and dynamics of biomolecular systems and bridge fragmented information obtained using high-resolution techniques. Here we review how small-angle X-ray scattering can be combined with other structural biology techniques to study protein dynamics. This article is part of a Special Issue entitled: Biophysics in Canada, edited by Lewis Kay, John Baenziger, Albert Berghuis and Peter Tieleman. Copyright © 2017 Elsevier B.V. All rights reserved.

Synchrotron X-ray studies of the keel of the short-spined sea urchin Lytechinus variegatus: absorption microtomography (microCT) and small beam diffraction mapping.

PubMed

Stock, S R; Barss, J; Dahl, T; Veis, A; Almer, J D; Carlo, F

2003-05-01

In sea urchin teeth, the keel plays an important structural role, and this paper reports results of microstructural characterization of the keel of Lytechinus variegatus using two noninvasive synchrotron x-ray techniques: x-ray absorption microtomography (microCT) and x-ray diffraction mapping. MicroCT with 14 keV x-rays mapped the spatial distribution of mineral at the 1.3 microm level in a millimeter-sized fragment of a mature portion of the keel. Two rows of low absorption channels (i.e., primary channels) slightly less than 10 microm in diameter were found running linearly from the flange to the base of the keel and parallel to its sides. The primary channels paralleled the oral edge of the keel, and the microCT slices revealed a planar secondary channel leading from each primary channel to the side of the keel. The primary and secondary channels were more or less coplanar and may correspond to the soft tissue between plates of the carinar process. Transmission x-ray diffraction with 80.8 keV x-rays and a 0.1 mm beam mapped the distribution of calcite crystal orientations and the composition Ca(1-x)Mg(x)CO(3) of the calcite. Unlike the variable Mg concentration and highly curved prisms found in the keel of Paracentrotus lividus, a constant Mg content (x = 0.13) and relatively little prism curvature was found in the keel of Lytechinus variegatus.

Hartman Testing of X-Ray Telescopes

NASA Technical Reports Server (NTRS)

Saha, Timo T.; Biskasch, Michael; Zhang, William W.

2013-01-01

Hartmann testing of x-ray telescopes is a simple test method to retrieve and analyze alignment errors and low-order circumferential errors of x-ray telescopes and their components. A narrow slit is scanned along the circumference of the telescope in front of the mirror and the centroids of the images are calculated. From the centroid data, alignment errors, radius variation errors, and cone-angle variation errors can be calculated. Mean cone angle, mean radial height (average radius), and the focal length of the telescope can also be estimated if the centroid data is measured at multiple focal plane locations. In this paper we present the basic equations that are used in the analysis process. These equations can be applied to full circumference or segmented x-ray telescopes. We use the Optical Surface Analysis Code (OSAC) to model a segmented x-ray telescope and show that the derived equations and accompanying analysis retrieves the alignment errors and low order circumferential errors accurately.

I12: the Joint Engineering, Environment and Processing (JEEP) beamline at Diamond Light Source.

PubMed

Drakopoulos, Michael; Connolley, Thomas; Reinhard, Christina; Atwood, Robert; Magdysyuk, Oxana; Vo, Nghia; Hart, Michael; Connor, Leigh; Humphreys, Bob; Howell, George; Davies, Steve; Hill, Tim; Wilkin, Guy; Pedersen, Ulrik; Foster, Andrew; De Maio, Nicoletta; Basham, Mark; Yuan, Fajin; Wanelik, Kaz

2015-05-01

I12 is the Joint Engineering, Environmental and Processing (JEEP) beamline, constructed during Phase II of the Diamond Light Source. I12 is located on a short (5 m) straight section of the Diamond storage ring and uses a 4.2 T superconducting wiggler to provide polychromatic and monochromatic X-rays in the energy range 50-150 keV. The beam energy enables good penetration through large or dense samples, combined with a large beam size (1 mrad horizontally × 0.3 mrad vertically). The beam characteristics permit the study of materials and processes inside environmental chambers without unacceptable attenuation of the beam and without the need to use sample sizes which are atypically small for the process under study. X-ray techniques available to users are radiography, tomography, energy-dispersive diffraction, monochromatic and white-beam two-dimensional diffraction/scattering and small-angle X-ray scattering. Since commencing operations in November 2009, I12 has established a broad user community in materials science and processing, chemical processing, biomedical engineering, civil engineering, environmental science, palaeontology and physics.

I12: the Joint Engineering, Environment and Processing (JEEP) beamline at Diamond Light Source

PubMed Central

Drakopoulos, Michael; Connolley, Thomas; Reinhard, Christina; Atwood, Robert; Magdysyuk, Oxana; Vo, Nghia; Hart, Michael; Connor, Leigh; Humphreys, Bob; Howell, George; Davies, Steve; Hill, Tim; Wilkin, Guy; Pedersen, Ulrik; Foster, Andrew; De Maio, Nicoletta; Basham, Mark; Yuan, Fajin; Wanelik, Kaz

2015-01-01

I12 is the Joint Engineering, Environmental and Processing (JEEP) beamline, constructed during Phase II of the Diamond Light Source. I12 is located on a short (5 m) straight section of the Diamond storage ring and uses a 4.2 T superconducting wiggler to provide polychromatic and monochromatic X-rays in the energy range 50–150 keV. The beam energy enables good penetration through large or dense samples, combined with a large beam size (1 mrad horizontally × 0.3 mrad vertically). The beam characteristics permit the study of materials and processes inside environmental chambers without unacceptable attenuation of the beam and without the need to use sample sizes which are atypically small for the process under study. X-ray techniques available to users are radiography, tomography, energy-dispersive diffraction, monochromatic and white-beam two-dimensional diffraction/scattering and small-angle X-ray scattering. Since commencing operations in November 2009, I12 has established a broad user community in materials science and processing, chemical processing, biomedical engineering, civil engineering, environmental science, palaeontology and physics. PMID:25931103

Zintl Clusters as Wet-Chemical Precursors for Germanium Nanomorphologies with Tunable Composition.

PubMed

Bentlohner, Manuel M; Waibel, Markus; Zeller, Patrick; Sarkar, Kuhu; Müller-Buschbaum, Peter; Fattakhova-Rohlfing, Dina; Fässler, Thomas F

2016-02-12

[Ge9](4-) Zintl clusters are used as soluble germanium source for a bottom-up fabrication of Ge nanomorphologies such as inverse opal structures with tunable composition. The method is based on the assembly and oxidation of [Ge9 ](4-) clusters in a template mold using SiCl4 , GeCl4 , and PCl3 leading to Si and P-containing Ge phases as shown by X-ray diffraction, Raman spectroscopy, and energy-dispersive X-ray analysis. [Ge9](4-) clusters are retained using ethylenediamine (en) as a transfer medium to a mold after removal of the solvent if water is thoroughly excluded, but are oxidized to amorphous Ge in presence of water traces. (1)H NMR spectroscopy reveals the oxidative deprotonation of en by [Ge9](4-). Subsequent annealing leads to crystalline Ge. As an example for wet-chemical synthesis of complex Ge nanomorphologies, we describe the fabrication of undoped and P-doped inverse opal-structured Ge films with a rather low oxygen contents. The morphology of the films with regular volume porosity is characterized by SEM, TEM, and grazing incidence small-angle X-ray scattering. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Toward comprehensive studies of liquids at high pressures and high temperatures: Combined structure, elastic wave velocity, and viscosity measurements in the Paris-Edinburgh cell

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

Kono, Yoshio; Park, Changyong; Kenney-Benson, Curtis

2014-08-19

Techniques for measuring liquid structure, elastic wave velocity, and viscosity under high pressure have been integrated using a Paris–Edinburgh cell at Beamline 16-BM-B, HPCAT of the Advanced Photon Source. The Paris–Edinburgh press allows for compressing large volume samples (up to 2 mm in both diameter and length) up to ~7 GPa and 2000 °C. Multi-angle energy dispersive X-ray diffraction provides structure factors of liquid to a large Q of ~19 Å. Ultrasonic techniques have been developed to investigate elastic wave velocity of liquids combined with the X-ray imaging. Falling sphere viscometry, using high-speed X-ray radiography (>1000 frames/s), enables us tomore » investigate a wide range of viscosity, from those of high viscosity silicates or oxides melts to low viscosity (<1 mPa s) liquids and fluids such as liquid metals or salts. The integration of these multiple techniques has promoted comprehensive studies of structure and physical properties of liquids as well as amorphous materials at high pressures and high temperatures, making it possible to investigate correlations between structure and physical properties of liquids in situ.« less

High-pressure studies of cycloheptane up to 30 GPa

NASA Astrophysics Data System (ADS)

Ma, Chunli; Cui, Qiliang; Liu, Zhenxian

2013-06-01

High-pressure synchrotron angle dispersive x-ray diffraction, Raman scattering and infrared absorption studies have been performed on cycloheptane (C7H14) up to 30 GPa at room temperature by using diamond anvil cell techniques. The synchrotron x-ray diffraction results indicate that the liquid cyclopentane undergoes two phase transitions at around 0.5 and 1.0 GPa, respectively. Then, it gradually turns into glass state starting from 3.0 GPa. The features of the Raman scattering and infrared absorption show no significant changes with increasing pressure below 3 GPa. This implies that the two phases observed by the x-ray diffraction can be attributed to plastic phases in which the cycloheptane molecules are held in an ordered structure while the molecular orientation is disordered. Up on further compression, all Raman and infrared bands begin broadening around 3.0 GPa that provide further evidence on the transition to glass state. Our results also suggest different paths on phase transitions under isothermal compression at room temperature compare to that previously reported under isobaric cooling at ambient pressure. This work was supported by the NSF of China (91014004, 11004074,11074089), the specialized Research Fund for the Doctoral Program of Higher Education (20110061110011, 20100061120093), and the National Basic Research Program of China (2011CB808200).

Goniometer-based femtosecond X-ray diffraction of mutant 30S ribosomal subunit crystals

DOE PAGES

Dao, E. Han; Sierra, Raymond G.; Laksmono, Hartawan; ...

2015-04-30

In this work, we collected radiation-damage-free data from a set of cryo-cooled crystals for a novel 30S ribosomal subunit mutant using goniometer-based femtosecond crystallography. Crystal quality assessment for these samples was conducted at the X-ray Pump Probe end-station of the Linac Coherent Light Source (LCLS) using recently introduced goniometer-based instrumentation. These 30S subunit crystals were genetically engineered to omit a 26-residue protein, Thx, which is present in the wild-type Thermus thermophilus 30S ribosomal subunit. We are primarily interested in elucidating the contribution of this ribosomal protein to the overall 30S subunit structure. To assess the viability of this study, femtosecondmore » X-ray diffraction patterns from these crystals were recorded at the LCLS during a protein crystal screening beam time. During our data collection, we successfully observed diffraction from these difficult-to-grow 30S ribosomal subunit crystals. Most of our crystals were found to diffract to low resolution, while one crystal diffracted to 3.2 Å resolution. These data suggest the feasibility of pursuing high-resolution data collection as well as the need to improve sample preparation and handling in order to collect a complete radiation-damage-free data set using an X-ray Free Electron Laser.« less

Using acoustic levitation in synchrotron based laser pump hard x-ray probe experiments

NASA Astrophysics Data System (ADS)

Hu, Bin; Lerch, Jason; Suthar, Kamlesh; Dichiara, Anthony

Acoustic levitation provides a platform to trap and hold a small amount of material by using standing pressure waves without a container. The technique has a potential to be used for laser pump x-ray probe experiments; x-ray scattering and laser distortion from the container can be avoided, sample consumption can be minimized, and unwanted chemistry that may occur at the container interface can be avoided. The method has been used at synchrotron sources for studying protein and pharmaceutical solutions using x-ray diffraction (XRD) and small angle x-ray scattering (SAXS). However, pump-probe experiments require homogeneously excited samples, smaller than the absorption depth of the material that must be held stably at the intersection of both the laser and x-ray beams. We discuss 1) the role of oscillations in acoustic levitation and the optimal acoustic trapping conditions for x-ray/laser experiments, 2) opportunities to automate acoustic levitation for fast sample loading and manipulation, and 3) our experimental results using SAXS to monitor laser induced thermal expansion in gold nanoparticles solution. We also performed Finite Element Analysis to optimize the trapping performance and stability of droplets ranging from 0.4 mm to 2 mm. Our early x-ray/laser demonstrated the potential of the technique for time-resolved X-ray science.

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

X Li; Y Mao; H Ma

An ionic liquid (IL) 1-docosanyl-3-methylimidazolium bromide was incorporated into ultra-high molecular weight polyethylene (UHMWPE) and formed IL/UHMWPE blends by solution mixing. The structure evolution of these blends during uniaxial stretching was followed by in-situ synchrotron wide-angle X-ray diffraction (WAXD) and small-angle X-ray scattering (SAXS) techniques. During deformation at room temperature, deformation-induced phase transformation from orthorhombic to monoclinic phase was observed in both IL/UHMWPE blends and neat UHMWPE. The elongation-to-break ratios of IL/UHMWPE blends were found to increase by 2-3 times compared with that of pure UHMWPE, while the tensile strength remained about the same. In contrast, during deformation at highmore » temperature (120 C), no phase transformation was observed. However, the blend samples showed much better toughness, higher crystal orientation and higher tilting extent of lamellar structure at high strains.« less

How temperature determines formation of maghemite nanoparticles

NASA Astrophysics Data System (ADS)

Girod, Matthias; Vogel, Stefanie; Szczerba, Wojciech; Thünemann, Andreas F.

2015-04-01

We report on the formation of polymer-stabilized superparamagnetic single-core and multi-core maghemite nanoparticles. The particle formation was carried out by coprecipitation of Fe(II) and Fe(III) sulfate in a continuous aqueous process using a micromixer system. Aggregates containing 50 primary particles with sizes of 2 nm were formed at a reaction temperature of 30 °C. These particles aggregated further with time and were not stable. In contrast, stable single-core particles with a diameter of 7 nm were formed at 80 °C as revealed by small-angle X-ray scattering (SAXS) coupled in-line with the micromixer for particle characterization. X-ray diffraction and TEM confirmed the SAXS results. X-ray absorption near-edge structure spectroscopy (XANES) identified the iron oxide phase as maghemite.

Dynamical scattering in coherent hard x-ray nanobeam Bragg diffraction

NASA Astrophysics Data System (ADS)

Pateras, A.; Park, J.; Ahn, Y.; Tilka, J. A.; Holt, M. V.; Kim, H.; Mawst, L. J.; Evans, P. G.

2018-06-01

Unique intensity features arising from dynamical diffraction arise in coherent x-ray nanobeam diffraction patterns of crystals having thicknesses larger than the x-ray extinction depth or exhibiting combinations of nanoscale and mesoscale features. We demonstrate that dynamical scattering effects can be accurately predicted using an optical model combined with the Darwin theory of dynamical x-ray diffraction. The model includes the highly divergent coherent x-ray nanobeams produced by Fresnel zone plate focusing optics and accounts for primary extinction, multiple scattering, and absorption. The simulation accurately reproduces the dynamical scattering features of experimental diffraction patterns acquired from a GaAs/AlGaAs epitaxial heterostructure on a GaAs (001) substrate.

Structural ordering and interface morphology in symmetrically strained(GaIn)As/Ga(PAs) superlattices grown on off-oriented GaAs(100)

NASA Astrophysics Data System (ADS)

Giannini, C.; Tapfer, L.; Zhuang, Y.; de Caro, L.; Marschner, T.; Stolz, W.

1997-02-01

In this work we investigate the structural properties of symmetrically strained (GaIn)As/GaAs/Ga(PAs)/GaAs superlattices by means of x-ray diffraction, reciprocal-space mapping, and x-ray reflectivity. The multilayers were grown by metalorganic vapor-phase epitaxy on (001) GaAs substrates intentionally off-oriented towards one of the nearest <110> directions. High-resolution triple-crystal reciprocal-space maps recorded for different azimuth angles in the vicinity of the (004) Bragg diffraction clearly show a double periodicity of the x-ray peak intensity that can be ascribed to a lateral and a vertical periodicity occurring parallel and perpendicular to the growth surface. Moreover, from the intensity modulation of the satellite peaks, a lateral-strain gradient within the epilayer unit cell is found, varying from a tensile to a compressive strain. Thus, the substrate off-orientation promotes a lateral modulation of the layer thickness (ordered interface roughness) and of the lattice strain, giving rise to laterally ordered macrosteps. In this respect, contour maps of the specular reflected beam in the vicinity of the (000) reciprocal lattice point were recorded in order to inspect the vertical and lateral interface roughness correlation. A semiquantitative analysis of our results shows that the interface morphology and roughness is greatly influenced by the off-orientation angle and the lateral strain distribution. Two mean spatial wavelengths can be determined, one corresponding exactly to the macrostep periodicity and the other indicating a further interface waviness along the macrosteps. The same spatial periodicities were found on the surface by atomic-force-microscopy images confirming the x-ray results and revealing a strong vertical correlation of the interfaces up to the outer surface.

Structure and giant magnetoresistance of granular Co-Cu nanolayers prepared by cross-beam pulsed laser deposition

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

Jesche, A.; Stoecker, H.; Levin, A. A.

2010-01-15

A series of Co{sub x}Cu{sub 100-x} (x=0, 40-75, 100) layers with thicknesses between 13 and 55 nm were prepared on silicon substrates using cross-beam pulsed laser deposition. Wide-angle x-ray diffraction (WAXRD), transmission electron microscopy (TEM), and electrical transport measurements revealed a structure consisting of decomposed cobalt and copper grains with grain sizes of about 10 nm. The influence of cobalt content and layer thickness on the grain size is discussed. Electron diffraction indicates the presence of an intermetallic Co-Cu phase of Cu{sub 3}Au structure type. Thermal treatment at temperatures between 525 and 750 K results in the progressive decomposition ofmore » Co and Cu, with an increase of the grain sizes up to about 100 nm. This is tunable by controlling the temperature and duration of the anneal, and is directly observable in WAXRD patterns and TEM images. A careful analysis of grain size and the coherence length of the radiation used allows for an accurate interpretation of the x-ray diffraction patterns, by taking into account coherent and noncoherent scattering. The alloy films show a giant magnetoresistance of 1%-2.3% with the maximum obtained after annealing at around 725 K.« less

Coherent x-ray diffraction imaging with nanofocused illumination.

PubMed

Schroer, C G; Boye, P; Feldkamp, J M; Patommel, J; Schropp, A; Schwab, A; Stephan, S; Burghammer, M; Schöder, S; Riekel, C

2008-08-29

Coherent x-ray diffraction imaging is an x-ray microscopy technique with the potential of reaching spatial resolutions well beyond the diffraction limits of x-ray microscopes based on optics. However, the available coherent dose at modern x-ray sources is limited, setting practical bounds on the spatial resolution of the technique. By focusing the available coherent flux onto the sample, the spatial resolution can be improved for radiation-hard specimens. A small gold particle (size <100 nm) was illuminated with a hard x-ray nanobeam (E=15.25 keV, beam dimensions approximately 100 x 100 nm2) and is reconstructed from its coherent diffraction pattern. A resolution of about 5 nm is achieved in 600 s exposure time.

Crystal structure of carnidazole form II from synchrotron X-ray powder diffraction: structural comparison with form I, the hydrated form and the low energy conformations in vacuo.

PubMed

de Armas, Héctor Novoa; Peeters, Oswald M; Blaton, Norbert; Van den Mooter, Guy; De Ridder, Dirk J A; Schenk, Henk

2006-10-01

The crystal structure of carnidazole form II, O-methyl [2-(2-methyl-5-nitro-1H-imidazole-1-yl)ethyl]thiocarbamate, has been determined using synchrotron X-ray powder diffraction in combination with simulated annealing and whole profile pattern matching, and refined by the Rietveld method. For structure solution, 12 degrees of freedom were defined: one motion group and six torsions. Form II crystallizes in space group P2(1)/n, Z=4, with unit cell parameters after Rietveld refinement: a=13.915(4), b=8.095(2), c=10.649(3) A, beta=110.83(1) degrees, and V=1121.1(5) A3. The two polymorphic forms, as well as the hydrate, crystallize in the monoclinic space group P2(1)/n having four molecules in the cell. In form II, the molecules are held together by forming two infinite zig-zag chains via hydrogen bonds of the type N--H...N, the same pattern as in form I. A conformational study of carnidazole, at semiempirical PM3 level, was performed using stochastic approaches based on modification of the flexible torsion angles. The values of the torsion angles for the molecules of the two polymorphic forms and the hydrate of carnidazole are compared to those obtained from the conformational search. Form I and form II are enantiotropic polymorphic pairs this agrees with the fact that the two forms are conformational polymorphs. Copyright (c) 2006 Wiley-Liss, Inc. and the American Pharmacists Association

Study of the specific features of single-crystal boron microstructure

NASA Astrophysics Data System (ADS)

Blagov, A. E.; Vasil'ev, A. L.; Dmitriev, V. P.; Ivanova, A. G.; Kulikov, A. G.; Marchenkov, N. V.; Popov, P. A.; Presnyakov, M. Yu.; Prosekov, P. A.; Pisarevskii, Yu. V.; Targonskii, A. V.; Chernaya, T. S.; Chernyshov, D. Yu.

2017-09-01

A complex study of the structure of β-boron single crystal grown by the floating-zone method, with sizes significantly exceeding the analogs known in the literature, has been performed. The study includes X-ray diffraction analysis and X-ray diffractometry (measurement of pole figures and rocking curves), performed on both laboratory and synchrotron sources; atomic-resolution scanning transmission electron microscopy with spherical aberration correction; and energy-dispersive microanalysis. X-ray diffraction analysis using synchrotron radiation has been used to refine the β-boron structure and find impurity Si atoms. The relative variations in the unit-cell parameters a and c for the crystal bulk are found to be δ a/ a ≈ 0.4 and δ c/ c ≈ 0.1%. X-ray diffractometry has revealed that the single-crystal growth axis coincides with the [2\\bar 2013] crystallographic axis and makes an angle of 21.12° with the [0001] threefold axis. Electron microscopy data have confirmed that the sample under study is a β-boron crystal, which may contain 0.3-0.4 at % Si as an impurity. Planar defects (stacking faults and dislocations) are found. The results of additional measurements of the temperature dependence of the thermal conductivity of the crystal in the range of 50-300 K are indicative of its high structural quality.

A platform for detecting material melting from shock compression using the NIF x-ray diffraction diagnostic TARDIS

NASA Astrophysics Data System (ADS)

Wehrenberg, Christopher; Kraus, Richard; Braun, Dave; Rygg, Ryan; Coppari, Federica; Lazicki, Amy; McNaney, James; Eggert, Jon

2016-10-01

A series of experiments were performed on NIF to develop a platform to detect material melting during shock compression using x-ray diffraction. The unique pulse shaping on NIF can be utilized to directly-drive a steady shock into an ablator and material sample while simultaneously creating an x-ray source to probe the material state. Sharp diffraction lines are observed when the material is in the solid state, while broad diffuse lines are seen when in the liquid state, providing an unambiguous signal for shock driven melting. Several shots were performed in which a shock of 50-80 GPa was driven into a Pb sample while a Ge foil was used as an x-ray source probe. Laser conditions were varied to create a suitable x-ray source that provides a short, bright burst of He-alpha emission from the Ge while maintaining a low background level on the image plates contained in the TARDIS diagnostic. This work was performed under the auspices of the U.S. Department of Energy by Lawrence Livermore National Laboratory under Contract No. DE-AC52-07NA27344.

Electron backscatter diffraction as a domain analysis technique in BiFeO(3)-PbTiO(3) single crystals.

PubMed

Burnett, T L; Comyn, T P; Merson, E; Bell, A J; Mingard, K; Hegarty, T; Cain, M

2008-05-01

xBiFeO(3)-(1-x)PbTiO(3) single crystals were grown via a flux method for a range of compositions. Presented here is a study of the domain configuration in the 0.5BiFeO(3)-0.5PbTiO(3) composition using electron backscatter diffraction to demonstrate the ability of the technique to map ferroelastic domain structures at the micron and submicron scale. The micron-scale domains exhibit an angle of approximately 85 degrees between each variant, indicative of a ferroelastic domain wall in a tetragonal system with a spontaneous strain, c/a - 1 of 0.10, in excellent agreement with the lattice parameters derived from x-ray diffraction. Contrast seen in forescatter images is attributed to variations in the direction of the electrical polarization vector, providing images of ferroelectric domain patterns.

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

Self-aligned Ni-P ohmic contact scheme for silicon solar cells by electroless deposition

NASA Astrophysics Data System (ADS)

Lee, Eun Kyung; Lim, Dong Chan; Lee, Kyu Hwan; Lim, Jae-Hong

2012-08-01

We report a Ni-P metallization scheme for low resistance ohmic contacts to n-type Si for silicon solar cells. As-deposited Ni-P contacts to n-type Si showed a specific contact resistance of 6.42 × 10-4 Ω·cm2. The specific contact resistance decreased with increasing thermal annealing temperature. When the Ni-P contact was annealed at 600°C for 30 min in ambient air, the specific contact resistance was greatly decreased, to 6.37 × 10-5Ω·cm2. The improved ohmic property was attributed to the decrease in the work function due to the formation of Ni-silicides from Ni in-diffusion during the thermal annealing process. Effects of the annealing process on the electrical and crystal properties of the contacts were investigated by means of various resistivity measurements (circular transmission line method (c-TLM), 4-point probe), glancing angle x-ray diffraction (GAXRD), and x-ray photoelectron spectroscopy (XPS).

Effect of argon ion activity on the properties of Y 2O 3 thin films deposited by low pressure PACVD

NASA Astrophysics Data System (ADS)

Barve, S. A.; Jagannath; Deo, M. N.; Kishore, R.; Biswas, A.; Gantayet, L. M.; Patil, D. S.

2010-10-01

Yttrium oxide thin films are deposited by microwave electron cyclotron resonance (ECR) plasma assisted metal organic chemical vapour deposition process using an indegeneously developed Y(thd) 3 {(2,2,6,6-tetramethyl-3,5-heptanedionate)yttrium} precursor. Depositions were carried out at two different argon gas flow rates keeping precursor and oxygen gas flow rate constant. The deposited coatings are characterized by X-ray photoelectron spectroscopy (XPS), glancing angle X-ray diffraction (GIXRD) and infrared spectroscopy. Optical properties of the films are studied by spectroscopic ellipsometry. Hardness and elastic modulus of the films are measured by load depth sensing nanoindentation technique. Stability of the film and its adhesion with the substrate is inferred from the nanoscratch test. It is shown here that, the change in the argon gas flow rates changes the ionization of the gas in the microwave ECR plasma and imposes a drastic change in the characteristics like composition, structure as well as mechanical properties of the deposited film.

Preparation of nanostructured and nanosheets of MoS2 oxide using oxidation method.

PubMed

Amini, Majed; Ramazani S A, Ahmad; Faghihi, Morteza; Fattahpour, Seyyedfaridoddin

2017-11-01

Molybdenum disulfide (MoS 2 ), a two-dimensional transition metal has a 2D layered structure and has recently attracted attention due to its novel catalytic properties. In this study, MoS 2 has been successfully intercalated using chemical and physical intercalation techniques, while enhancing its surface properties. The final intercalated MoS 2 is of many interests because of its low-dimensional and potential properties in in-situ catalysis. In this research, we report different methods to intercalate the layers of MoS 2 successfully using acid-treatment, ultrasonication, oxidation and thermal shocking. The other goal of this study is to form SO bonds mainly because of expected enhanced in-situ catalytic operations. The intercalated MoS 2 is further characterized using analyses such as Fourier Transform Infrared Spectroscopy (FTIR), Raman, Contact Angle, X-ray diffraction (XRD), Field Emission Scanning Electron Microscope (FESEM), Energy Dispersive X-Ray Microanalysis (EDAX), Transmission electron microscopy (TEM), and BET. Copyright © 2017. Published by Elsevier B.V.

Understanding how the aggregation structure of starch affects its gastrointestinal digestion rate and extent.

PubMed

Chen, Pei; Wang, Kai; Kuang, Qirong; Zhou, Sumei; Wang, Dazheng; Liu, Xingxun

2016-06-01

Regulating the starch gastrointestinal digestion rate by control of its aggregation structure is an effective way, but the mechanism is still not clear. Multi-scale structure of waxy and normal wheat starches were studied by confocal laser scanning and scanning electron microscopes, as well as wide-angle and small-angle X-ray techniques in this study. In vitro digestion kinetics of those two starches and structure-digestion relationship were also discussed. Both waxy and normal starches show A-type diffraction pattern, but waxy variety shows a slightly higher crystallinity. Small-angle X-ray scattering results show that waxy wheat starch has higher scattering peak intensity (Imax) and a larger crystallinity lamellar repeat distance (Lp) compared with the normal wheat starch. We suggested that the higher digestion rate of waxy starch at initial stage is mainly due to more small-size particles, but the higher crystallinity and the larger crystalline lamellar size limit the digestion extent. Copyright © 2016 Elsevier B.V. All rights reserved.

Extracting the pair distribution function of liquids and liquid-vapor surfaces by grazing incidence x-ray diffraction mode.

PubMed

Vaknin, David; Bu, Wei; Travesset, Alex

2008-07-28

We show that the structure factor S(q) of water can be obtained from x-ray synchrotron experiments at grazing angle of incidence (in reflection mode) by using a liquid surface diffractometer. The corrections used to obtain S(q) self-consistently are described. Applying these corrections to scans at different incident beam angles (above the critical angle) collapses the measured intensities into a single master curve, without fitting parameters, which within a scale factor yields S(q). Performing the measurements below the critical angle for total reflectivity yields the structure factor of the top most layers of the water/vapor interface. Our results indicate water restructuring at the vapor/water interface. We also introduce a new approach to extract g(r), the pair distribution function (PDF), by expressing the PDF as a linear sum of error functions whose parameters are refined by applying a nonlinear least square fit method. This approach enables a straightforward determination of the inherent uncertainties in the PDF. Implications of our results to previously measured and theoretical predictions of the PDF are also discussed.

Modeling the intermolecular interactions: molecular structure of N-3-hydroxyphenyl-4-methoxybenzamide.

PubMed

Karabulut, Sedat; Namli, Hilmi; Kurtaran, Raif; Yildirim, Leyla Tatar; Leszczynski, Jerzy

2014-03-01

The title compound, N-3-hydroxyphenyl-4-methoxybenzamide (3) was prepared by the acylation reaction of 3-aminophenol (1) and 4-metoxybenzoylchloride (2) in THF and characterized by ¹H NMR, ¹³C NMR and elemental analysis. Molecular structure of the crystal was determined by single crystal X-ray diffraction and DFT calculations. 3 crystallizes in monoclinic P2₁/c space group. The influence of intermolecular interactions (dimerization and crystal packing) on molecular geometry has been evaluated by calculations performed for three different models; monomer (3), dimer (4) and dimer with added unit cell contacts (5). Molecular structure of 3, 4 and 5 was optimized by applying B3LYP method with 6-31G+(d,p) basis set in gas phase and compared with X-ray crystallographic data including bond lengths, bond angles and selected dihedral angles. It has been concluded that although the crystal packing and dimerization have a minor effect on bond lengths and angles, however, these interactions are important for the dihedral angles and the rotational conformation of aromatic rings. Copyright © 2013 Elsevier Inc. All rights reserved.

Biological imaging by soft X-ray diffraction microscopy

NASA Astrophysics Data System (ADS)

Shapiro, David

We have developed a microscope for soft x-ray diffraction imaging of dry or frozen hydrated biological specimens. This lensless imaging system does not suffer from the resolution or specimen thickness limitations that other short wavelength microscopes experience. The microscope, currently situated at beamline 9.0.1 of the Advanced Light Source, can collect diffraction data to 12 nm resolution with 750 eV photons and 17 nm resolution with 520 eV photons. The specimen can be rotated with a precision goniometer through an angle of 160 degrees allowing for the collection of nearly complete three-dimensional diffraction data. The microscope is fully computer controlled through a graphical user interface and a scripting language automates the collection of both two-dimensional and three-dimensional data. Diffraction data from a freeze-dried dwarf yeast cell, Saccharomyces cerevisiae carrying the CLN3-1 mutation, was collected to 12 run resolution from 8 specimen orientations spanning a total rotation of 8 degrees. The diffraction data was phased using the difference map algorithm and the reconstructions provide real space images of the cell to 30 nm resolution from each of the orientations. The agreement of the different reconstructions provides confidence in the recovered, and previously unknown, structure and indicates the three dimensionality of the cell. This work represents the first imaging of the natural complex refractive contrast from a whole unstained cell by the diffraction microscopy method and has achieved a resolution superior to lens based x-ray tomographic reconstructions of similar specimens. Studies of the effects of exposure to large radiation doses were also carried out. It was determined that the freeze-dried cell suffers from an initial collapse, which is followed by a uniform, but slow, shrinkage. This structural damage to the cell is not accompanied by a diminished ability to see small features in the specimen. Preliminary measurements on frozen-hydrated yeast indicate that the frozen specimens do not exhibit these changes even with doses as high as 5 x 109 Gray.

Unraveling double stranded alpha-helical coiled coils: an x-ray diffraction study on hard alpha-keratin fibers.

PubMed

Kreplak, L; Doucet, J; Briki, F

2001-04-15

Transformations of proteins secondary and tertiary structures are generally studied in globular proteins in solution. In fibrous proteins, such as hard alpha-keratin, that contain long and well-defined double stranded alpha-helical coiled coil domains, such study can be directly done on the native fibrous tissue. In order to assess the structural behavior of the coiled coil domains under an axial mechanical stress, wide angle x-ray scattering and small angle x-ray scattering experiments have been carried out on stretched horse hair fibers at relative humidity around 30%. Our observations of the three major axial spacings as a function of the applied macroscopic strain have shown two rates. Up to 4% macroscopic strain the coiled coils were slightly distorted but retained their overall conformation. Above 4% the proportion of coiled coil domains progressively decreased. The main and new result of our study is the observation of the transition from alpha-helical coiled coils to disordered chains instead of the alpha-helical coiled coil to beta-sheet transition that occurs in wet fibers.

Comparative analysis of ex-situ and operando X-ray diffraction experiments for lithium insertion materials

NASA Astrophysics Data System (ADS)

Brant, William R.; Li, Dan; Gu, Qinfen; Schmid, Siegbert

2016-01-01

A comparative study of ex-situ and operando X-ray diffraction techniques using the fast lithium ion conductor Li0.18Sr0.66Ti0.5Nb0.5O3 is presented. Ex-situ analysis of synchrotron X-ray diffraction data suggests that a single phase material exists for all discharges to as low as 0.422 V. For samples discharged to 1 V or lower, i.e. with higher lithium content, it is possible to determine the lithium position from the X-ray data. However, operando X-ray diffraction from a coin cell reveals that a kinetically driven two phase region occurs during battery cycling below 1 V. Through monitoring the change in unit cell dimension during electrochemical cycling the dynamics of lithium insertion are explored. A reduction in the rate of unit cell expansion of 22(2)% part way through the first discharge and 13(1)% during the second discharge is observed. This reduction may be caused by a drop in lithium diffusion into the bulk material for higher lithium contents. A more significant change is a jump in the unit cell expansion by 60(2)% once the lithium content exceeds one lithium ion per vacant site. It is suggested that this jump is caused by damping of octahedral rotations, thus establishing a link between lithium content and octahedral rotations.

Dose-Dependent Effects of CeO2 on Microstructure and Antibacterial Property of Plasma-Sprayed TiO2 Coatings for Orthopedic Application

NASA Astrophysics Data System (ADS)

Zhao, Xiaobing; Liu, Gaopeng; Zheng, Hai; Cao, Huiliang; Liu, Xuanyong

2015-02-01

Titanium and its alloys have been used extensively for orthopedic and dental implants. Although these devices have achieved high rates of success, two major complications may be encountered: the lack of osseointegration and the biomaterial-related infection. Accordingly, cerium oxide (CeO2)-doped titanium oxide (TiO2) materials were coated on titanium by an atmospheric plasma spraying (APS) technique. The phase structures, morphologies, and surface chemical states of the obtained coatings were characterized by x-ray diffraction, scanning electron microscopy, and x-ray photoelectron spectroscopy techniques. The in vitro antibacterial and cytocompatibility of the materials were studied with Staphylococcus aureus ( S. aureus, ATCC25923) and osteoblast precursor cell line MC3T3-E1. The results indicated that the addition of CeO2 shifts slightly the diffraction peaks of TiO2 matrix to low angles but does not change its rutile phase structure. In addition, the CeO2/TiO2 composite coatings possess dose-dependent corrosion resistance and antimicrobial properties. And doping of 10 wt.% CeO2 exhibits the highest activity against S. aureus, improved corrosion resistance, and competitive cytocompatibility, which argues a promising option for balancing the osteogenetic and antibacterial properties of titanium implants.

Improved Cytotoxic Effect of Doxorubicin by Its Combination with Sclareol in Solid Lipid Nanoparticle Suspension.

PubMed

Oliveira, Mariana Silva; Lima, Bruno Henrique Santiago; Goulart, Gisele Assis Castro; Mussi, Samuel Vidal; Borges, Gabriel Silva Marques; Oréfice, Rodrigo Lambert; Ferreira, Lucas Antônio Miranda

2018-08-01

This work aims to develop, characterize, and evaluate the anticancer activity of solid lipid nanoparticles (SLN) containing doxorubicin (DOX), an antitumoral from the antracycline class, and sclareol (SC), a lipophilic labdene diterpene (SLN-DOX-SC). The SLN were characterized by Differential Scanning Calorimetry (DSC), X-ray Diffraction (XRD), Small Angle X-ray Diffraction (SAXS), in vitro release, transmission electron microscopy, and polarized light microscopy. Evaluation of cell viability was performed in two cell cultures: MCF-7 (human breast cancer) and 4T1 (murine breast cancer). The SLN showed a size in the range of 128 nm, negative zeta potential, DOX encapsulation efficiency (EE) of 99%, and drug loading (DL) of 66 mg/g. Characterization of the formulation by DSC, XRD, and SAXS revealed the presence of DOX inside the nanoparticles of SLN and suggested increased expulsion/release of this drug when associated with SC. The release profiles revealed that the SLN-DOX-SC showed controlled release of DOX at pH 7.4 with enhanced drug release at low pH, useful for cancer treatment. The SLN-DOX-SC demonstrated to be more effective than the free DOX against 4T1 cells. So, the developed SLN efficiently encapsulate DOX and SC and show good potential as an alternative for cancer treatment.

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.

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.

Local terahertz field enhancement for time-resolved x-ray diffraction

DOE PAGES

Kozina, M.; Pancaldi, M.; Bernhard, C.; ...

2017-02-20

We report local field strength enhancement of single-cycle terahertz (THz) pulses in an ultrafast time-resolved x-ray diffraction experiment. We show that patterning the sample with gold microstructures increases the THz field without changing the THz pulse shape or drastically affecting the quality of the x-ray diffraction pattern. Lastly, we find a five-fold increase in THz-induced x-ray diffraction intensity change in the presence of microstructures on a SrTiO 3 thin-film sample.

Local terahertz field enhancement for time-resolved x-ray diffraction

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

Kozina, M.; Pancaldi, M.; Bernhard, C.

We report local field strength enhancement of single-cycle terahertz (THz) pulses in an ultrafast time-resolved x-ray diffraction experiment. We show that patterning the sample with gold microstructures increases the THz field without changing the THz pulse shape or drastically affecting the quality of the x-ray diffraction pattern. Lastly, we find a five-fold increase in THz-induced x-ray diffraction intensity change in the presence of microstructures on a SrTiO 3 thin-film sample.

Simulation study of an X-ray diffraction system for breast tumor detection

NASA Astrophysics Data System (ADS)

Marticke, F.; Montémont, G.; Paulus, C.; Michel, O.; Mars, J. I.; Verger, L.

2017-09-01

X-ray diffraction (XRD) is a powerful technique used to determine the molecular structure of biological tissues. In breast tissues for example, the scattering signatures of dense fibroglandular tissue and carcinoma have been shown to be significantly different. In this study, XRD was used as a second control level when conventional mammography results were unclear, for instance because of overly high breast density. A system optimized for this issue, called multifocal XRD, was developed combining energy dispersive spectral information at different scattering angles. This system allows depth-imaging in one go but needs an x,y-direction scan to image the region conventional mammography identified as suspect. The scan-time for about 10 cm3 with an incident flux of about 4 . 8 ṡ 107 photons per second would be around 2 s. For this study, breast phantoms with and without cancerous nodule were simulated to assess the separation power of the method and to determine the radiation dose required to obtain nearly ideal separation. For tumors situated in the center of the breast, the required dose was only about 0.3 mGy, even for breasts with high density. The tumor position was shown to have a low impact on detectability provided it remained in a zone where the system was sufficiently sensitive. The influence of incident spectrum maximum energy was also studied. The required dose remained very low with any of the incident spectra tested. Finally, an image slice was reconstructed in the x-direction and showed that the system can detect the presence of a small tumor (4 mm). Hence, XRD is a very promising tool to reduce the number of unnecessary invasive breast biopsies.

Low-Q peak in X-ray patterns of choline-phenylalanine and -homophenylalanine: A combined effect of chain and stacking

NASA Astrophysics Data System (ADS)

Campetella, Marco; Martino, Delia Chillura; Scarpellini, Eleonora; Gontrani, Lorenzo

2016-09-01

In this contribution we report for the first time the X-ray patterns of choline-phenylalanine and choline-homophenylalanine ionic liquids. The presence of a low Q peak in both systems is another evidence that a long alkyl chain is not always needed to establish a nanodomain segregation in the liquid sufficient to be revealed by the diffraction experiment. These new data are compared with the diffraction patterns and the theoretical calculations of other choline-aminoacid ionic liquids recently reported. A significant role might be played by the stacking interactions between aromatic rings.

Experiments with phase transitions at very high pressure

NASA Technical Reports Server (NTRS)

Spain, I. L.

1984-01-01

A diamond anvil cell is described which was developed for studying hydrogen and other materials to pressure above 100 PGa, including measurements at low temperature. The benefits of X-ray diffraction using synchrotron radiation and using a fixed anode source are examined as well as the optimization of X-ray diffraction at low temperature. A Ge diode detector was incorporated into apparatus for measuring optical absorption, reflectance, and fluorescence in order to enable luminescence studies and Raman spectra were obtained. Results of experiments on Si, Ge, GaP, InAs, hydrogen, benzene, nitrogen, graphite, and the superconductor CeCu2Si2 are given.

Grain boundary misorientations and percolative current paths in high-{ital J}{sub {ital c}} powder-in-tube (Bi,Pb){sub 2}Sr{sub 3}Ca{sub 3}Cu{sub 3}O{sub {ital x}}

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

Goyal, A.; Specht, E.D.; Kroeger, D.M.

1995-05-22

Grain orientations and grain boundary misorientations in high-{ital J}{sub {ital c}}, powder-in-tube (PIT) (Bi,Pb){sub 2}Sr{sub 2}Ca{sub 2}Cu{sub 3}O{sub {ital x}} (Bi-2223) were determined using electron backscatter Kikuchi diffraction and x-ray microdiffraction. Data collected from over 113 spatially correlated grains, resulting in 227 grain boundaries, show that over 40% of the boundaries are {Sigma}1 or small angle (less than 15{degree}). In addition, 8% of the boundaries are within the Brandon criterion for CSLs (sigma larger than 1 and less than 50). Grain boundary ``texture maps`` derived from the electron microscope image and orientation data reveal the presence of percolative paths betweenmore » low energy boundaries.« less

Thermal x-ray diffraction and near-field phase contrast imaging

NASA Astrophysics Data System (ADS)

Li, Zheng; Classen, Anton; Peng, Tao; Medvedev, Nikita; Wang, Fenglin; Chapman, Henry N.; Shih, Yanhua

2017-10-01

Using higher-order coherence of thermal light sources, the resolution power of standard x-ray imaging techniques can be enhanced. In this work, we applied the higher-order measurement to far-field x-ray diffraction and near-field phase contrast imaging (PCI), in order to achieve superresolution in x-ray diffraction and obtain enhanced intensity contrast in PCI. The cost of implementing such schemes is minimal compared to the methods that achieve similar effects by using entangled x-ray photon pairs.

Thermal x-ray diffraction and near-field phase contrast imaging

DOE PAGES

Li, Zheng; Classen, Anton; Peng, Tao; ...

2017-12-27

Using higher-order coherence of thermal light sources, the resolution power of standard x-ray imaging techniques can be enhanced. Here in this work, we applied the higher-order measurement to far-field x-ray diffraction and near-field phase contrast imaging (PCI), in order to achieve superresolution in x-ray diffraction and obtain enhanced intensity contrast in PCI. The cost of implementing such schemes is minimal compared to the methods that achieve similar effects by using entangled x-ray photon pairs.

The Critical Role of Thioacetamide Concentration in the Formation of ZnO/ZnS Heterostructures by Sol-Gel Process

PubMed Central

Kiatkoski Kaminski, Renata Cristina; Caetano, Bruno Leonardo; Magnani, Marina; Meneau, Florian; Rochet, Amélie; Santilli, Celso Valentim; Briois, Valérie; Bourgaux, Claudie

2018-01-01

ZnO/ZnS heterostructures have emerged as an attractive approach for tailoring the properties of particles comprising these semiconductors. They can be synthesized using low temperature sol-gel routes. The present work yields insight into the mechanisms involved in the formation of ZnO/ZnS nanostructures. ZnO colloidal suspensions, prepared by hydrolysis and condensation of a Zn acetate precursor solution, were allowed to react with an ethanolic thioacetamide solution (TAA) as sulfur source. The reactions were monitored in situ by Small Angle X-ray Scattering (SAXS) and UV-vis spectroscopy, and the final colloidal suspensions were characterized by High Resolution Transmission Electron Microscopy (HRTEM). The powders extracted at the end of the reactions were analyzed by X-ray Absorption spectroscopy (XAS) and X-ray diffraction (XRD). Depending on TAA concentration, different nanostructures were revealed. ZnO and ZnS phases were mainly obtained at low and high TAA concentrations, respectively. At intermediate TAA concentrations, we evidenced the formation of ZnO/ZnS heterostructures. ZnS formation could take place via direct crystal growth involving Zn ions remaining in solution and S ions provided by TAA and/or chemical conversion of ZnO to ZnS. The combination of all the characterization techniques was crucial to elucidate the reaction steps and the nature of the final products. PMID:29360735

Applications of a pnCCD detector coupled to columnar structure CsI(Tl) scintillator system in ultra high energy X-ray Laue diffraction

NASA Astrophysics Data System (ADS)

Shokr, M.; Schlosser, D.; Abboud, A.; Algashi, A.; Tosson, A.; Conka, T.; Hartmann, R.; Klaus, M.; Genzel, C.; Strüder, L.; Pietsch, U.

2017-12-01

Most charge coupled devices (CCDs) are made of silicon (Si) with typical active layer thicknesses of several microns. In case of a pnCCD detector the sensitive Si thickness is 450 μm. However, for silicon based detectors the quantum efficiency for hard X-rays drops significantly for photon energies above 10 keV . This drawback can be overcome by combining a pixelated silicon-based detector system with a columnar scintillator. Here we report on the characterization of a low noise, fully depleted 128×128 pixels pnCCD detector with 75×75 μm2 pixel size coupled to a 700 μm thick columnar CsI(Tl) scintillator in the photon range between 1 keV to 130 keV . The excellent performance of the detection system in the hard X-ray range is demonstrated in a Laue type X-ray diffraction experiment performed at EDDI beamline of the BESSY II synchrotron taken at a set of several GaAs single crystals irradiated by white synchrotron radiation. With the columnar structure of the scintillator, the position resolution of the whole system reaches a value of less than one pixel. Using the presented detector system and considering the functional relation between indirect and direct photon events Laue diffraction peaks with X-ray energies up to 120 keV were efficiently detected. As one of possible applications of the combined CsI-pnCCD system we demonstrate that the accuracy of X-ray structure factors extracted from Laue diffraction peaks can be significantly improved in hard X-ray range using the combined CsI(Tl)-pnCCD system compared to a bare pnCCD.

X-ray diffraction analysis of hydroxyapatite-coated in different plasma gas atmosphere on Ti and Ti-6Al-4V

PubMed Central

Kotian, Ravindra; Rao, P. Prasad; Madhyastha, Prashanthi

2017-01-01

Objective: The aim is to study the effect of plasma working gas on composition, crystallinity, and microstructure of hydroxyapatite (HA) coated on Ti and Ti-6Al-4V metal substrates. Materials and Methods: Ti and Ti-6Al-4V metal substrates were coated with HA by plasma spray using four plasma gas atmospheres of argon, argon/hydrogen, nitrogen, and nitrogen/hydrogen. The degree of crystallinity, the phases present, and microstructure of HA coating were characterized using X-ray diffraction and scanning electron microscopy. Results: Variation in crystallinity and the microstructure of HA coating on plasma gas atmosphere was observed. Micro-cracks due to thermal stresses and shift in the 2θ angle of HA compared to feedstock was seen. Conclusion: Plasma gas atmosphere has a significant influence on composition, crystallinity, and micro-cracks of HA-coated dental implants. PMID:29279668

Pressure induced structural transitions in CuSbS 2 and CuSbSe 2 thermoelectric compounds

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

Baker, Jason; Kumar, Ravhi S.; Sneed, Daniel

Here, we investigate the structural behavior of CuSbS 2 and CuSbSe 2 thermoelectric materials under high pressure conditions up to 80 GPa using angle dispersive X-ray diffraction in a diamond anvil cell (DAC). We also perform high pressure Raman spectroscopy measurements up to 16 GPa. We observed a pressure-induced structural transformation from the ambient orthorhombic structure with space group Pnma to a triclinic type structure with space group P1 beginning around 8 GPa in both samples and completing at 13 GPa and 10 GPa in CuSbS 2 and CuSbSe 2, respectively. High pressure Raman experiments complement the transitions observed bymore » high pressure X-ray diffraction (HPXRD). Finally, the transitions were found to be reversible on releasing the pressure to ambient in the DAC. The bulk modulus and compressibility of these materials are further discussed.« less

Time-resolved x-ray imaging of a laser-induced nanoplasma and its neutral residuals

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

Fluckiger, L.; Rupp, D.; Adolph, M.

The evolution of individual, large gas-phase xenon clusters, turned into a nanoplasma by a high power infrared laser pulse, is tracked from femtoseconds up to nanoseconds after laser excitation via coherent diffractive imaging, using ultra-short soft x-ray free electron laser pulses. A decline of scattering signal at high detection angles with increasing time delay indicates a softening of the cluster surface. Here we demonstrate, for the first time a representative speckle pattern of a new stage of cluster expansion for xenon clusters after a nanosecond irradiation. The analysis of the measured average speckle size and the envelope of the intensitymore » distribution reveals a mean cluster size and length scale of internal density fluctuations. Furthermore, the measured diffraction patterns were reproduced by scattering simulations which assumed that the cluster expands with pronounced internal density fluctuations hundreds of picoseconds after excitation.« less

Pressure induced structural transitions in CuSbS 2 and CuSbSe 2 thermoelectric compounds

DOE PAGES

Baker, Jason; Kumar, Ravhi S.; Sneed, Daniel; ...

2015-04-27

Here, we investigate the structural behavior of CuSbS 2 and CuSbSe 2 thermoelectric materials under high pressure conditions up to 80 GPa using angle dispersive X-ray diffraction in a diamond anvil cell (DAC). We also perform high pressure Raman spectroscopy measurements up to 16 GPa. We observed a pressure-induced structural transformation from the ambient orthorhombic structure with space group Pnma to a triclinic type structure with space group P1 beginning around 8 GPa in both samples and completing at 13 GPa and 10 GPa in CuSbS 2 and CuSbSe 2, respectively. High pressure Raman experiments complement the transitions observed bymore » high pressure X-ray diffraction (HPXRD). Finally, the transitions were found to be reversible on releasing the pressure to ambient in the DAC. The bulk modulus and compressibility of these materials are further discussed.« less

Boron monosulfide: Equation of state and pressure-induced phase transition

NASA Astrophysics Data System (ADS)

Cherednichenko, K. A.; Kruglov, I. A.; Oganov, A. R.; Le Godec, Y.; Mezouar, M.; Solozhenko, V. L.

2018-04-01

Quasi-hydrostatic compression of rhombohedral boron monosulfide (r-BS) has been studied up to 50 GPa at room temperature using diamond-anvil cells and angle-dispersive synchrotron X-ray diffraction. A fit of the experimental P-V data to the Vinet equation of state yields the bulk modulus B0 of 42.2(1.4) GPa and its first pressure derivative B0' of 7.6(2) that are in excellent agreement with our ab initio calculations. Formation of a new high-pressure phase of boron monosulfide (hp-BS) has been observed above 35 GPa. According to ab initio evolutionary crystal structure predictions combined with Rietveld refinement of high-pressure X-ray diffraction data, the structure of hp-BS has trigonal symmetry and belongs to the space group P-3m1. As it follows from the electron density of state calculations, the phase transformation is accompanied by an insulator-metal transition.

Reaction layer formation at the graphite/copper-chromium alloy interface

NASA Technical Reports Server (NTRS)

Devincent, Sandra M.; Michal, Gary M.

1992-01-01

Sessile drop tests were used to obtain information about copper chromium alloys that suitably wet graphite. Characterization of graphite/copper-chromium alloy interfaces subjected to elevated temperatures were conducted using scanning electron micrography, energy dispersive spectroscopy, auger electron spectroscopy, and x ray diffraction analyses. These analyses indicate that during sessile drop tests conducted at 1130 C for one hour, copper alloys containing greater than 0.98 percent chromium form continuous reaction layers of approximately 10 micron thickness. The reaction layers adhere to the graphite surface. The copper wets the reaction layer to form a contact angle of 60 degrees or less. X ray diffraction results indicate that the reaction layer is chromium carbide. The kinetics of reaction layer formation were modelled in terms of bulk diffusion mechanisms. Reaction layer thickness is controlled initially by the diffusion of Cr out of Cu alloy and later by the diffusion of C through chromium carbide.

Time-resolved x-ray imaging of a laser-induced nanoplasma and its neutral residuals

DOE PAGES

Fluckiger, L.; Rupp, D.; Adolph, M.; ...

2016-04-13

The evolution of individual, large gas-phase xenon clusters, turned into a nanoplasma by a high power infrared laser pulse, is tracked from femtoseconds up to nanoseconds after laser excitation via coherent diffractive imaging, using ultra-short soft x-ray free electron laser pulses. A decline of scattering signal at high detection angles with increasing time delay indicates a softening of the cluster surface. Here we demonstrate, for the first time a representative speckle pattern of a new stage of cluster expansion for xenon clusters after a nanosecond irradiation. The analysis of the measured average speckle size and the envelope of the intensitymore » distribution reveals a mean cluster size and length scale of internal density fluctuations. Furthermore, the measured diffraction patterns were reproduced by scattering simulations which assumed that the cluster expands with pronounced internal density fluctuations hundreds of picoseconds after excitation.« less

Reaction layer formation at the graphite/copper-chromium alloy interface

NASA Technical Reports Server (NTRS)

Devincent, Sandra M.; Michal, Gary M.

1993-01-01

Sessile drop tests were used to obtain information about copper chromium alloys that suitably wet graphite. Characterization of graphite/copper-chromium alloy interfaces subjected to elevated temperatures were conducted using scanning electron micrography, energy dispersive spectroscopy, Auger electron spectroscopy, and X-ray diffraction analyses. These analyses indicate that during sessile drop tests conducted at 1130 C for one hour, copper alloys containing greater than 0.98 percent chromium form continuous reaction layers of approximately 10 micron thickness. The reaction layers adhere to the graphite surface. The copper wets the reaction layer to form a contact angle of 60 degrees or less. X-ray diffraction results indicate that the reaction layer is chromium carbide. The kinetics of reaction layer formation were modelled in terms of bulk diffusion mechanisms. Reaction layer thickness is controlled initially by the diffusion of Cr out of Cu alloy and later by the diffusion of C through chromium carbide.

Automated X-Ray Diffraction of Irradiated Materials

DOE PAGES

Rodman, John; Lin, Yuewei; Sprouster, David; ...

2017-10-26

Synchrotron-based X-ray diffraction (XRD) and small-angle Xray scattering (SAXS) characterization techniques used on unirradiated and irradiated reactor pressure vessel steels yield large amounts of data. Machine learning techniques, including PCA, offer a novel method of analyzing and visualizing these large data sets in order to determine the effects of chemistry and irradiation conditions on the formation of radiation induced precipitates. In order to run analysis on these data sets, preprocessing must be carried out to convert the data to a usable format and mask the 2-D detector images to account for experimental variations. Once the data has been preprocessed, itmore » can be organized and visualized using principal component analysis (PCA), multi-dimensional scaling, and k-means clustering. In conclusion, from these techniques, it is shown that sample chemistry has a notable effect on the formation of the radiation induced precipitates in reactor pressure vessel steels.« less

An image focusing means by using an opaque object to diffract x-rays

DOEpatents

Sommargren, Gary E.; Weaver, H. Joseph

1991-01-01

The invention provides a method and apparatus for focusing and imaging x-rays. An opaque sphere is used as a diffractive imaging element to diffract x-rays from an object so that the divergent x-ray wavefronts are transformed into convergent wavefronts and are brought to focus to form an image of the object with a large depth of field.

NMR crystallography of α-poly(L-lactide).

PubMed

Pawlak, Tomasz; Jaworska, Magdalena; Potrzebowski, Marek J

2013-03-07

A complementary approach that combines NMR measurements, analysis of X-ray and neutron powder diffraction data and advanced quantum mechanical calculations was employed to study the α-polymorph of L-polylactide. Such a strategy, which is known as NMR crystallography, to the best of our knowledge, is used here for the first time for the fine refinement of the crystal structure of a synthetic polymer. The GIPAW method was used to compute the NMR shielding parameters for the different models, which included the α-PLLA structure obtained by 2-dimensional wide-angle X-ray diffraction (WAXD) at -150 °C (model M1) and at 25 °C (model M2), neutron diffraction (WAND) measurements (model M3) and the fully optimized geometry of the PLLA chains in the unit cell with defined size (model M4). The influence of changes in the chain conformation on the (13)C σ(ii) NMR shielding parameters is shown. The correlation between the σ(ii) and δ(ii) values for the M1-M4 models revealed that the M4 model provided the best fit. Moreover, a comparison of the experimental (13)C NMR spectra with the spectra calculated using the M1-M4 models strongly supports the data for the M4 model. The GIPAW method, via verification using NMR measurements, was shown to be capable of the fine refinement of the crystal structures of polymers when coarse X-ray diffraction data for powdered samples are available.

Soft X-Ray Diffraction Microscopy of a Frozen Hydrated Yeast Cell

DOE PAGES

Huang, Xiaojing; Nelson, Johanna; Kirz, Janos; ...

2009-11-01

We report the first image of an intact, frozen hydrated eukaryotic cell using x-ray diffraction microscopy, or coherent x-ray diffraction imaging. By plunge freezing the specimen in liquid ethane and maintaining it below -170 °C, artifacts due to dehydration, ice crystallization, and radiation damage are greatly reduced. In this example, coherent diffraction data using 520 eV x rays were recorded and reconstructed to reveal a budding yeast cell at a resolution better than 25 nm. This demonstration represents an important step towards high resolution imaging of cells in their natural, hydrated state, without limitations imposed by x-ray optics.

Pressure-induced structural transformations of the Zintl phase sodium silicide

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

Cabrera, Raul Quesada; Salamat, Ashkan; Barkalov, Oleg I.

The high-pressure behaviour of NaSi has been studied using Raman spectroscopy and angle-dispersive synchrotron X-ray diffraction to observe the onset of structural phase transformations and potential oligomerisation into anionic Si nanoclusters with extended dimensionality. Our studies reveal a first structural transformation occurring at 8-10 GPa, followed by irreversible amorphisation above 15 GPa, suggesting the formation of Si-Si bonds with oxidation of the Si{sup -} species and reduction of Na{sup +} to metallic sodium. We have combined our experimental studies with DFT calculations to assist in the analysis of the structural behaviour of NaSi at high pressure. - Abstract: The high-pressuremore » behaviour of NaSi has been studied using Raman spectroscopy and angle-dispersive synchrotron X-ray diffraction. Our studies reveal a first structural transformation occurring at 8-10 GPa, followed by irreversible amorphisation, suggesting the formation of Si-Si bonds with oxidation of the Si{sup -} species and reduction of Na{sup +} to metallic sodium. We have combined our experimental studies with DFT calculations to assist in the analysis of the structural behaviour of NaSi at high pressure. Display Omitted« less

Thorough small-angle X-ray scattering analysis of the instability of liquid micro-jets in air.

PubMed

Marmiroli, Benedetta; Cacho-Nerin, Fernando; Sartori, Barbara; Pérez, Javier; Amenitsch, Heinz

2014-01-01

Liquid jets are of interest, both for their industrial relevance and for scientific applications (more important, in particular for X-rays, after the advent of free-electron lasers that require liquid jets as sample carrier). Instability mechanisms have been described theoretically and by numerical simulation, but confirmed by few experimental techniques. In fact, these are mainly based on cameras, which is limited by the imaging resolution, and on light scattering, which is hindered by absorption, reflection, Mie scattering and multiple scattering due to complex air/liquid interfaces during jet break-up. In this communication it is demonstrated that synchrotron small-angle X-ray scattering (SAXS) can give quantitative information on liquid jet dynamics at the nanoscale, by detecting time-dependent morphology and break-up length. Jets ejected from circular tubes of different diameters (100-450 µm) and speeds (0.7-21 m s(-1)) have been explored to cover the Rayleigh and first wind-induced regimes. Various solvents (water, ethanol, 2-propanol) and their mixtures have been examined. The determination of the liquid jet behaviour becomes essential, as it provides background data in subsequent studies of chemical and biological reactions using SAXS or X-ray diffraction based on synchrotron radiation and free-electron lasers.

Cadmium effect on structural properties of Cu{sub 2}Zn{sub 1-x}Cd{sub x}SnS{sub 4} quinternary alloys nanostructures

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

Ibraheam, A. S.; Al-Douri, Y., E-mail: yaldouri@yahoo.com; Hashim, U.

The study report novel sensing plat of extended quinternart materials, Cu{sub 2}Zn{sub 1-x}d{sub x}SnS{sub 4} quinternary alloy nanostructures were fabricated onto oxidized silicon substrate by sol-gel method and characterized were synthesized by X-ray diffraction (XRD). The XRD peaks were shifted towered the lower angle side with increasing cadmium content. The practical size average of the Cu{sub 2}Zn{sub 1-x}d{sub x}SnS{sub 4} quinternary alloy nanostructures between 34.55 to 63.30 nm.

Optics for coherent X-ray applications

PubMed Central

Yabashi, Makina; Tono, Kensuke; Mimura, Hidekazu; Matsuyama, Satoshi; Yamauchi, Kazuto; Tanaka, Takashi; Tanaka, Hitoshi; Tamasaku, Kenji; Ohashi, Haruhiko; Goto, Shunji; Ishikawa, Tetsuya

2014-01-01

Developments of X-ray optics for full utilization of diffraction-limited storage rings (DLSRs) are presented. The expected performance of DLSRs is introduced using the design parameters of SPring-8 II. To develop optical elements applicable to manipulation of coherent X-rays, advanced technologies on precise processing and metrology were invented. With propagation-based coherent X-rays at the 1 km beamline of SPring-8, a beryllium window fabricated with the physical-vapour-deposition method was found to have ideal speckle-free properties. The elastic emission machining method was utilized for developing reflective mirrors without distortion of the wavefronts. The method was further applied to production of diffraction-limited focusing mirrors generating the smallest spot size in the sub-10 nm regime. To enable production of ultra-intense nanobeams at DLSRs, a low-vibration cooling system for a high-heat-load monochromator and advanced diagnostic systems to characterize X-ray beam properties precisely were developed. Finally, new experimental schemes for combinative nano-analysis and spectroscopy realised with novel X-ray optics are discussed. PMID:25177986

Synthesis and properties of nanocrystalline copper indium oxide thin films deposited by Rf magnetron sputtering.

PubMed

Singh, Mandeep; Singh, V N; Mehta, B R

2008-08-01

Nanocrystalline copper indium oxide (CuInO2) thin films with particle size ranging from 25 nm to 71 nm have been synthesized from a composite target using reactive Rf magnetron sputtering technique. X-ray photoelectron spectroscopy (XPS) combined with glancing angle X-ray diffraction (GAXRD) analysis confirmed the presence of delafossite CuInO2 phase in these films. The optical absorption studies show the presence of two direct band gaps at 3.3 and 4.3 eV, respectively. The resistance versus temperature measurements show thermally activated hopping with activation energy of 0.84 eV to be the conduction mechanism.

Topological Insulators and Superconductors for Innovative Devices

DTIC Science & Technology

2015-03-20

bulk-sensitive experiment with hard x ray or low-energy photons.) This demon- strates that the bulk band gap can be enhanced by taking advantage of the...crystallinity in X - ray Laue analysis, and their detailed transport properties are described in the Supplementary Information. ARPES measurements were...high quality of our fi lms grown at high temperatures, including ultrathin ones, is evident from the X - ray diffraction patterns shown in Figure 2 d

Controllable stearic acid crystal induced high hydrophobicity on cellulose film surface.

PubMed

He, Meng; Xu, Min; Zhang, Lina

2013-02-01

A novel, highly hydrophobic cellulose composite film (RCS) with biodegradability was fabricated via solvent-vaporized controllable crystallization of stearic acid in the porous structure of cellulose films (RC). The interface structure and properties of the composite films were investigated with wide-angle X-ray diffraction (WAXD), scanning electron microscopy (SEM), differential scanning calorimetry (DSC), FT-IR, solid-state (13)C NMR, water uptake, tensile testing, water contact angle, and biodegradation tests. The results indicated that the RCS films exhibited high hydrophobicity (water contact angle achieved to 145°), better mechanical properties in the humid state and lower water uptake ratio than RC. Interestingly, the stearic acid crystallization was induced by the pore wall of the cellulose matrix to form a micronano binary structure, resulting in a rough surface. The rough surface with a hierarchical structure containing micronanospace on the RCS film surface could trap abundant air, leading to the high hydrophobicity. Moreover, the RCS films were flexible, biodegradable, and low-cost, showing potential applications in biodegradable water-proof packaging.

Negative thermal expansion and magnetoelastic coupling in the breathing pyrochlore lattice material LiGaCr4S8

NASA Astrophysics Data System (ADS)

Pokharel, G.; May, A. F.; Parker, D. S.; Calder, S.; Ehlers, G.; Huq, A.; Kimber, S. A. J.; Arachchige, H. Suriya; Poudel, L.; McGuire, M. A.; Mandrus, D.; Christianson, A. D.

2018-04-01

The physical properties of the spinel LiGaCr4S8 have been studied with neutron diffraction, x-ray diffraction, magnetic susceptibility, and heat capacity measurements. The neutron diffraction and synchrotron x-ray diffraction data reveal negative thermal expansion (NTE) below 111(4) K. The magnetic susceptibility deviates from Curie-Weiss behavior with the onset of NTE. At low temperature a broad peak in the magnetic susceptibility at 10.3(3) K is accompanied by the return of normal thermal expansion. First-principles calculations find a strong coupling between the lattice and the simulated magnetic ground state. These results indicate strong magnetoelastic coupling in LiGaCr4S8 .

Application of focused-beam flat-sample method to synchrotron powder X-ray diffraction with anomalous scattering effect

NASA Astrophysics Data System (ADS)

Tanaka, M.; Katsuya, Y.; Matsushita, Y.

2013-03-01

The focused-beam flat-sample method (FFM), which is a method for high-resolution and rapid synchrotron X-ray powder diffraction measurements by combination of beam focusing optics, a flat shape sample and an area detector, was applied for diffraction experiments with anomalous scattering effect. The advantages of FFM for anomalous diffraction were absorption correction without approximation, rapid data collection by an area detector and good signal-to-noise ratio data by focusing optics. In the X-ray diffraction experiments of CoFe2O4 and Fe3O4 (By FFM) using X-rays near the Fe K absorption edge, the anomalous scattering effect between Fe/Co or Fe2+/Fe3+ can be clearly detected, due to the change of diffraction intensity. The change of observed diffraction intensity as the incident X-ray energy was consistent with the calculation. The FFM is expected to be a method for anomalous powder diffraction.

Rietveld analysis using powder diffraction data with anomalous scattering effect obtained by focused beam flat sample method

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

Tanaka, Masahiko, E-mail: masahiko@spring8.or.jp; Katsuya, Yoshio, E-mail: katsuya@spring8.or.jp; Sakata, Osami, E-mail: SAKATA.Osami@nims.go.jp

2016-07-27

Focused-beam flat-sample method (FFM) is a new trial for synchrotron powder diffraction method, which is a combination of beam focusing optics, flat shape powder sample and area detectors. The method has advantages for X-ray diffraction experiments applying anomalous scattering effect (anomalous diffraction), because of 1. Absorption correction without approximation, 2. High intensity X-rays of focused incident beams and high signal noise ratio of diffracted X-rays 3. Rapid data collection with area detectors. We applied the FFM to anomalous diffraction experiments and collected synchrotron X-ray powder diffraction data of CoFe{sub 2}O{sub 4} (inverse spinel structure) using X-rays near Fe K absorptionmore » edge, which can distinguish Co and Fe by anomalous scattering effect. We conducted Rietveld analyses with the obtained powder diffraction data and successfully determined the distribution of Co and Fe ions in CoFe{sub 2}O{sub 4} crystal structure.« less

Measurement of illite particle thickness using a direct Fourier transform of small-angle X-ray scattering data

USGS Publications Warehouse

Shang, Chao; Rice, James A.; Eberl, Dennis D.; Lin, Jar-Shyong

2003-01-01

It has been suggested that interstratified illite-smectite (I-S) minerals are composed of aggregates of fundamental particles. Many attempts have been made to measure the thickness of such fundamental particles, but each of the methods used suffers from its own limitations and uncertainties. Small-angle X-ray scattering (SAXS) can be used to measure the thickness of particles that scatter X-rays coherently. We used SAXS to study suspensions of Na-rectorite and other illites with varying proportions of smectite. The scattering intensity (I) was recorded as a function of the scattering vector, q = (4 /) sin(/2), where  is the X-ray wavelength and  is the scattering angle. The experimental data were treated with a direct Fourier transform to obtain the pair distance distribution function (PDDF) that was then used to determine the thickness of illite particles. The Guinier and Porod extrapolations were used to obtain the scattering intensity beyond the experimental q, and the effects of such extrapolations on the PDDF were examined. The thickness of independent rectorite particles (used as a reference mineral) is 18.3 Å. The SAXS results are compared with those obtained by X-ray diffraction peak broadening methods. It was found that the power-law exponent (α) obtained by fitting the data in the region of q = 0.1-0.6 nm-1 to the power law (I = I0q-α) is a linear function of illite particle thickness. Therefore, illite particle thickness could be predicted by the linear relationship as long as the thickness is within the limit where α <4.0.

X-ray lasers for structural and dynamic biology

NASA Astrophysics Data System (ADS)

Spence, J. C. H.; Weierstall, U.; Chapman, H. N.

2012-10-01

Research opportunities and techniques are reviewed for the application of hard x-ray pulsed free-electron lasers (XFEL) to structural biology. These include the imaging of protein nanocrystals, single particles such as viruses, pump-probe experiments for time-resolved nanocrystallography, and snapshot wide-angle x-ray scattering (WAXS) from molecules in solution. The use of femtosecond exposure times, rather than freezing of samples, as a means of minimizing radiation damage is shown to open up new opportunities for the molecular imaging of biochemical reactions at room temperature in solution. This is possible using a ‘diffract-and-destroy’ mode in which the incident pulse terminates before radiation damage begins. Methods for delivering hundreds of hydrated bioparticles per second (in random orientations) to a pulsed x-ray beam are described. New data analysis approaches are outlined for the correlated fluctuations in fast WAXS, for protein nanocrystals just a few molecules on a side, and for the continuous x-ray scattering from a single virus. Methods for determining the orientation of a molecule from its diffraction pattern are reviewed. Methods for the preparation of protein nanocrystals are also reviewed. New opportunities for solving the phase problem for XFEL data are outlined. A summary of the latest results is given, which now extend to atomic resolution for nanocrystals. Possibilities for time-resolved chemistry using fast WAXS (solution scattering) from mixtures is reviewed, toward the general goal of making molecular movies of biochemical processes.

In situ synchrotron X-ray diffraction study on epitaxial-growth dynamics of III–V semiconductors

NASA Astrophysics Data System (ADS)

Takahasi, Masamitu

2018-05-01

The application of in situ synchrotron X-ray diffraction (XRD) to the molecular-beam epitaxial (MBE) growth of III–V semiconductors is overviewed along with backgrounds of the diffraction theory and instrumentation. X-rays are sensitive not only to the surface of growing films but also to buried interfacial structures because of their large penetration depth. Moreover, a spatial coherence length up to µm order makes X-rays widely applicable to the characterization of low-dimensional structures, such as quantum dots and wires. In situ XRD studies during growth were performed using an X-ray diffractometer, which was combined with an MBE chamber. X-ray reciprocal space mapping at a speed matching a typical growth rate was achieved using intense X-rays available from a synchrotron light source and an area detector. The importance of measuring the three-dimensional distribution of XRD intensity in a reciprocal space map is demonstrated for the MBE growth of two-, one-, and zero-dimensional structures. A large amount of information about the growth process of two-dimensional InGaAs/GaAs(001) epitaxial films has been provided by three-dimensional X-ray reciprocal mappings, including the anisotropic strain relaxation, the compositional inhomogeneity, and the evolution of surface and interfacial roughness. For one-dimensional GaAs nanowires grown in a Au-catalyzed vapor-liquid–solid mode, the relationship between the diameter of the nanowires and the formation of polytypes has been suggested on the basis of in situ XRD measurements. In situ three-dimensional X-ray reciprocal space mapping is also shown to be useful for determining the lateral and vertical sizes of self-assembled InAs/GaAs(001) quantum dots as well as their internal strain distributions during growth.

X-ray evaluation of SEM technique for determining the crystallography of echinoid skeletons.

PubMed

Dillaman, R M; Hart, H V

1981-01-01

Coronal plates of the sea urchin Strongylocentrotus purpuratus have a microstructure typified by smooth textured trabeculae. When plates were decorated with calcite crystals each rhombohedron had the same orientation regardless of its location on the plate. When the sample was oriented so that the three edges of the rhombohedron formed equal 120 degrees angles and the three crystal faces appeared to form equal angles with the plane of the photograph, the c-axis of the plate paralleled the electron beam and the three a-axes were 30 degrees counterclockwise from the edges. These a-axes were then related to a plate edge recorded in a low magnification micrograph. Directions of the a-axes of each plate were also measured using a back-reflection Laue x-ray diffraction camera. A comparison of a-axes measured by the two techniques showed an average difference of 3 degrees, indicating that decorated crystal grew in crystallographic continuity with the plate. Assuming this relationship remains constant, the decoration technique appears to be an accurate and efficient method for evaluating the crystallography of echinoid skeletal units. Analysis of a polar plot of a-axes for 11 plates indicated that the a-axes were not randomly oriented; however, definitive relationships must await more extensive investigations.

Effects of interfaces on the thermal conductivity in Si/Si0.75Ge0.25 multilayer with varying Au layers

NASA Astrophysics Data System (ADS)

Hu, Yangsen; Wu, Zhenghua; Ye, Fengjie; Hu, Zhiyu

2018-02-01

The manoeuvre of thermal transport property across multilayer films with inserted metal layers through controlling the metal-nonmetal interfaces is of fundamental interest. In this work, amorphous Si/Si0.75Ge0.25 multilayer films inserted with varying Au layers were fabricated by magnetron sputtering. The structure and sharp interface of multilayers films were characterized by low angle x-ray diffraction (LAXRD), grazing incidence small angle x-ray scattering (GISAXS) and scanning electron microscopy (SEM). A differential 3ω method was applied to measure the effective thermal conductivity. The measurements show that thermal conductivity has changed as varying Au layers. Thermal conductivity increased from 0.94 to 1.31 Wm-1K-1 while Si0.75Ge0.25 layer was replaced by different Au layers, which was attributed to the strong electron-phonon coupling and interface thermal resistance in a metal-nonmetal multilayered system. Theoretical calculation combined with experimental results indicate that the thermal conductivity of the multilayer film could be facilely controlled by introducing different number of nanoconstructed metal-nonmetal interfaces, which provide a more insightful understanding of the thermal transport manipulation mechanism of the thin film system with inserting metal layers.

Effects of 1 MeV electrons on the deformation mechanisms of polyethylene/carbon nanotube composites

NASA Astrophysics Data System (ADS)

Yang, Jianqun; Zhang, Xiaodong; Liu, Chaoming; Li, Xingji; Li, Hongxia; Ma, Guoliang; Tian, Feng

2017-10-01

Polymer nano-composites, especially in polyethylene (PE)/carbon nanotube (CNT) composites can be employed as radiation shielding and structural materials in space. When the PE/CNT composites are used in space, it is easy to suffer from radiation damage caused by charged particles. However, few studies about deformation mechanisms of the composites exposed to electron become available so far. In this paper, mutiwalled carbon nanotubes (MWCNTs) were incorporated into low density polyethylene (LDPE) with MWCNT loadings concentrations of 0.1 wt%. The structural evolution during uniaxial tensile deformation of the LDPE/0.1% MWCNT composites before and after 1 MeV electrons were investigated by means of a small angle X-ray scattering (SAXS) and wide angle X-ray diffraction (WAXD). Experimental results show that 1 MeV electrons obviously increase the ultimate tensile strength of the LDPE/MWCNT composites. From SAXS and WAXD analyses, it is shown that 1 MeV electrons inhibit the disintegration and the rotation of the lamellae, and slow down the formation of the new crystals. It is concluded that the intense interaction between MWCNTs and LDPE matrix and the crosslinking strengthening generated by 1 MeV electrons is the dominant reason for the changes of the deformation behaviors of LDPE.

Injected ion energy dependence of SiC film deposited by low-energy SiC3H9+ ion beam produced from hexamethyldisilane

NASA Astrophysics Data System (ADS)

Yoshimura, Satoru; Sugimoto, Satoshi; Takeuchi, Takae; Murai, Kensuke; Kiuchi, Masato

2018-04-01

We mass-selected SiC3H9+ ions from various fragments produced through the decomposition of hexamethyldisilane, and finally produced low-energy SiC3H9+ ion beams. The ion beams were injected into Si(1 0 0) substrates and the dependence of deposited films on injected ion energy was then investigated. Injected ion energies were 20, 100, or 200 eV. Films obtained were investigated with X-ray diffraction, X-ray photoelectron spectroscopy, and Raman spectroscopy. X-ray diffraction and X-ray photoelectron spectroscopy of the substrates obtained following the injection of 20 eV ions demonstrated the occurrence of silicon carbide film (3C-SiC) deposition. On the other hand, Raman spectroscopy showed that the films deposited by the injection of 100 or 200 eV ions included 3C-SiC plus diamond-like carbon. Ion beam deposition using hexamethyldisilane-derived 20 eV SiC3H9+ ions is an efficient technique for 3C-SiC film formation on Si substrates.

Effect of high intensity ultrasound on the mesostructure of hydrated zirconia

NASA Astrophysics Data System (ADS)

Kopitsa, G. P.; Baranchikov, A. E.; Ivanova, O. S.; Yapryntsev, A. D.; Grigoriev, S. V.; Pranzas, P. Klaus; Ivanov, V. K.

2012-02-01

We report structural changes in amorphous hydrated zirconia caused by high intensity ultrasonic treatment studied by means of small-angle neutron scattering (SANS) and X-ray diffraction (XRD). It was established that sonication affects the mesostructure of ZrO2×xH2O gels (i.e. decreases their homogeneity, increases surface fractal dimension and the size of monomer particles). Ultrasound induced structural changes in hydrated zirconia governs its thermal behaviour, namely decreases the rate of tetragonal to monoclinic zirconia phase transition.

Invited Review Article: Development of crystal lenses for energetic photons

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

Smither, Robert K.

2014-08-15

This paper follows the development of crystal diffraction lenses designed to focus energetic photons. It begins with the search for a solution to the astrophysics problem of how to detect weak astrophysics sources of gamma rays and x-rays. This led to the basic designs for a lens and to the understanding of basic limitations of lens design. The discussion of the development of crystal diffraction lenses is divided into two parts: lenses using crystals with mosaic structure, and lenses that use crystals with curved crystal planes. This second group divides into two sub-groups: (1) Curved crystals that are used tomore » increase the acceptance angle of the diffraction of a monochromatic beam and to increase the energy bandwidth of the diffraction. (2) Curved crystals used to focus gamma ray beams. The paper describes how these two types of crystals affect the design of the corresponding crystal lenses in different fields: astrophysics, medical imaging, detection of weak, distant, gamma-ray sources, etc. The designs of crystal lenses for these applications are given in enough detail to allow the reader to design a lens for his own application.« less

Synthesis Of Noble Metal Nanoparticle Composite Glasses Using Low Energy Ion Beam Mixing

NASA Astrophysics Data System (ADS)

Varma, Ranjana S.; Kothari, D. C.; Mahadkar, A. G.; Kulkarni, N. A.; Kanjilal, D.; Kumar, P.

2010-12-01

Carbon coated thin films of Cu or Au on fused silica glasses have been irradiated using 100 keV Ar+ ions at different fluences ranging from 1×1013 to 1×1016 ion/cm2. In this article, we explore a route to form noble metal nanoparticles in amorphous glass matrices without post irradiation annealing using low energy ion beam mixing where nuclear energy loss process is dominant. Optical and structural properties were studied using UV-Vis-NIR absorbance spectroscopy and Glancing angle X-ray Diffraction (GXRD). Results showed that Cu and Au nanoparticles are formed at higher fluence of 1×1016 ion/cm2 used in this work without annealing. The diameters of metal nanoparticles obtained from UV-Vis NIR and GXRD are in agreement.

Corrosion resistance of high-Cr oxide dispersion strengthened ferritic steels in super-critical pressurized water

NASA Astrophysics Data System (ADS)

Cho, H. S.; Kimura, A.

2007-08-01

The effects of alloying elements, such as Cr and Al, on corrosion resistance in super critical pressurized water (SCPW) have been investigated to develop corrosion resistant oxide-dispersion-strengthened (ODS) steels. Corrosion tests were performed in a SCPW (783 K, 25 MPa) environment. Weight gain was measured after exposure to the SCPW, and then oxide layers were analyzed by low angle X-ray diffraction and SEM microscopy. The weight gains of all high-Cr ODS steels are smaller than an austenitic stainless steel (SUS316L). More uniform and thinner oxidation layers were observed on the ODS steels after corrosion compared to those on 9Cr martensitic steel and SUS316L.

Amorphous silicon carbide coatings for extreme ultraviolet optics

NASA Technical Reports Server (NTRS)

Kortright, J. B.; Windt, David L.

1988-01-01

Amorphous silicon carbide films formed by sputtering techniques are shown to have high reflectance in the extreme ultraviolet spectral region. X-ray scattering verifies that the atomic arrangements in these films are amorphous, while Auger electron spectroscopy and Rutherford backscattering spectroscopy show that the films have composition close to stoichiometric SiC, although slightly C-rich, with low impurity levels. Reflectance vs incidence angle measurements from 24 to 1216 A were used to derive optical constants of this material, which are presented here. Additionally, the measured extreme ultraviolet efficiency of a diffraction grating overcoated with sputtered amorphous silicon carbide is presented, demonstrating the feasibility of using these films as coatings for EUV optics.

Dynamical effects in Bragg coherent x-ray diffraction imaging of finite crystals

NASA Astrophysics Data System (ADS)

Shabalin, A. G.; Yefanov, O. M.; Nosik, V. L.; Bushuev, V. A.; Vartanyants, I. A.

2017-08-01

We present simulations of Bragg coherent x-ray diffractive imaging (CXDI) data from finite crystals in the frame of the dynamical theory of x-ray diffraction. The developed approach is based on a numerical solution of modified Takagi-Taupin equations and can be applied for modeling of a broad range of x-ray diffraction experiments with finite three-dimensional crystals of arbitrary shape also in the presence of strain. We performed simulations for nanocrystals of a cubic and hemispherical shape of different sizes and provided a detailed analysis of artifacts in the Bragg CXDI reconstructions introduced by the dynamical diffraction. Based on our theoretical analysis we developed an analytical procedure to treat effects of refraction and absorption in the reconstruction. Our results elucidate limitations for the kinematical approach in the Bragg CXDI and suggest a natural criterion to distinguish between kinematical and dynamical cases in coherent x-ray diffraction on a finite crystal.

Beam splitting of low-contrast binary gratings under second Bragg angle incidence.

PubMed

Zheng, Jiangjun; Zhou, Changhe; Wang, Bo; Feng, Jijun

2008-05-01

Beam splitting of low-contrast rectangular gratings under second Bragg angle incidence is studied. The grating period is between lambda and 2lambda. The diffraction behaviors of the three transmitted propagating orders are illustrated by analyzing the first three propagating grating modes. From a simplified modal approach, the design conditions of gratings as a high-efficiency element with most of its energy concentrated in the -2nd transmitted order (~90%) and of gratings as a 1 x 2 beam splitter with a total efficiency over 90% are derived. The grating parameters for achieving exactly the splitting pattern by use of rigorous coupled-wave analysis verified the design method. A 1 x 3 beam splitter is also demonstrated. Moreover, the polarization-dependent diffraction behaviors are investigated, which suggest the possibility of designing polarization-selective elements under such a configuration. The proposed concept of using the second Bragg angle should be helpful for developing new grating-based devices.

Mesoscale evolution of voids and microstructural changes in HMX-based explosives during heating through the β-δ phase transition

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

Willey, Trevor M., E-mail: willey1@llnl.gov; Lauderbach, Lisa; Gagliardi, Franco

HMX-based explosives LX-10 and PBX-9501 were heated through the β-δ phase transition. Ultra-small angle x-ray scattering (USAXS) and molecular diffraction were simultaneously recorded as the HMX was heated. Mesoscale voids and structure dramatically change promptly with the β-δ phase transition, rather than with other thermal effects. Also, x-ray induced damage, observed in the USAXS, occurs more readily at elevated temperatures; as such, the dose was reduced to mitigate this effect. Optical microscopy performed during a similar heating cycle gives an indication of changes on longer length scales, while x-ray microtomography, performed before and after heating, shows the character of extensivemore » microstructural damage resulting from the temperature cycle and solid-state phase transition.« less

Mesoscale evolution of voids and microstructural changes in HMX-based explosives during heating through the β-δ phase transition

DOE PAGES

Willey, Trevor M.; Lauderbach, Lisa; Gagliardi, Franco; ...

2015-08-07

HMX-based explosives LX-10 and PBX-9501 were heated through the β-δ phase transition. Ultra-small angle x-ray scattering (USAXS) and molecular diffraction were simultaneously recorded as the HMX was heated. Mesoscale voids and structure dramatically change promptly with the β-δ phase transition, rather than with other thermal effects. Also, x-ray induced damage, observed in the USAXS, occurs more readily at elevated temperatures; as such, the dose was reduced to mitigate this effect. Optical microscopy performed during a similar heating cycle gives an indication of changes on longer length scales, while x-ray microtomography, performed before and after heating, shows the character of extensivemore » microstructural damage resulting from the temperature cycle and solid-state phase transition.« less

Effect of Pd Interlayer on Electrochemical Properties of ENIG Surface Finish in 3.5 wt.% NaCl Solution

NASA Astrophysics Data System (ADS)

Nam, N. D.; Bui, Q. V.; Nhan, H. T.; Phuong, D. V.; Bian, M. Z.

2014-09-01

The corrosion resistance of a multilayered (NiP-Pd-Au) coating with various thicknesses of palladium (Pd) interlayer deposited on copper by an electroless method was investigated using electrochemical techniques including potentiodynamic polarization and electrochemical impedance spectroscopy. In addition, the surface finish was examined by x-ray diffraction analysis and scanning electron microscopy, and the contact angle of the liquid-solid interface was recorded. The corrosion resistance of the copper substrate was considerably improved by Pd interlayer addition. Increase of the thickness of the Pd interlayer enhanced the performance of the Cu-NiP-Pd-Au coating due to low porosity, high protective efficiency, high charge-transfer resistance, and contact angle. These are attributed to the diffusion of layers in the Cu-NiP-Pd-Au coating acting as a physical barrier layer, leading to the protection provided by the coating.

Energy resolution of the CdTe-XPAD detector: calibration and potential for Laue diffraction measurements on protein crystals.

PubMed

Medjoubi, Kadda; Thompson, Andrew; Bérar, Jean-François; Clemens, Jean-Claude; Delpierre, Pierre; Da Silva, Paulo; Dinkespiler, Bernard; Fourme, Roger; Gourhant, Patrick; Guimaraes, Beatriz; Hustache, Stéphanie; Idir, Mourad; Itié, Jean-Paul; Legrand, Pierre; Menneglier, Claude; Mercere, Pascal; Picca, Frederic; Samama, Jean-Pierre

2012-05-01

The XPAD3S-CdTe, a CdTe photon-counting pixel array detector, has been used to measure the energy and the intensity of the white-beam diffraction from a lysozyme crystal. A method was developed to calibrate the detector in terms of energy, allowing incident photon energy measurement to high resolution (approximately 140 eV), opening up new possibilities in energy-resolved X-ray diffraction. In order to demonstrate this, Laue diffraction experiments were performed on the bending-magnet beamline METROLOGIE at Synchrotron SOLEIL. The X-ray energy spectra of diffracted spots were deduced from the indexed Laue patterns collected with an imaging-plate detector and then measured with both the XPAD3S-CdTe and the XPAD3S-Si, a silicon photon-counting pixel array detector. The predicted and measured energy of selected diffraction spots are in good agreement, demonstrating the reliability of the calibration method. These results open up the way to direct unit-cell parameter determination and the measurement of high-quality Laue data even at low resolution. Based on the success of these measurements, potential applications in X-ray diffraction opened up by this type of technology are discussed.

Hydrogen atoms can be located accurately and precisely by x-ray crystallography.

PubMed

Woińska, Magdalena; Grabowsky, Simon; Dominiak, Paulina M; Woźniak, Krzysztof; Jayatilaka, Dylan

2016-05-01

Precise and accurate structural information on hydrogen atoms is crucial to the study of energies of interactions important for crystal engineering, materials science, medicine, and pharmacy, and to the estimation of physical and chemical properties in solids. However, hydrogen atoms only scatter x-radiation weakly, so x-rays have not been used routinely to locate them accurately. Textbooks and teaching classes still emphasize that hydrogen atoms cannot be located with x-rays close to heavy elements; instead, neutron diffraction is needed. We show that, contrary to widespread expectation, hydrogen atoms can be located very accurately using x-ray diffraction, yielding bond lengths involving hydrogen atoms (A-H) that are in agreement with results from neutron diffraction mostly within a single standard deviation. The precision of the determination is also comparable between x-ray and neutron diffraction results. This has been achieved at resolutions as low as 0.8 Å using Hirshfeld atom refinement (HAR). We have applied HAR to 81 crystal structures of organic molecules and compared the A-H bond lengths with those from neutron measurements for A-H bonds sorted into bonds of the same class. We further show in a selection of inorganic compounds that hydrogen atoms can be located in bridging positions and close to heavy transition metals accurately and precisely. We anticipate that, in the future, conventional x-radiation sources at in-house diffractometers can be used routinely for locating hydrogen atoms in small molecules accurately instead of large-scale facilities such as spallation sources or nuclear reactors.

Hydrogen atoms can be located accurately and precisely by x-ray crystallography

PubMed Central

Woińska, Magdalena; Grabowsky, Simon; Dominiak, Paulina M.; Woźniak, Krzysztof; Jayatilaka, Dylan

2016-01-01

Precise and accurate structural information on hydrogen atoms is crucial to the study of energies of interactions important for crystal engineering, materials science, medicine, and pharmacy, and to the estimation of physical and chemical properties in solids. However, hydrogen atoms only scatter x-radiation weakly, so x-rays have not been used routinely to locate them accurately. Textbooks and teaching classes still emphasize that hydrogen atoms cannot be located with x-rays close to heavy elements; instead, neutron diffraction is needed. We show that, contrary to widespread expectation, hydrogen atoms can be located very accurately using x-ray diffraction, yielding bond lengths involving hydrogen atoms (A–H) that are in agreement with results from neutron diffraction mostly within a single standard deviation. The precision of the determination is also comparable between x-ray and neutron diffraction results. This has been achieved at resolutions as low as 0.8 Å using Hirshfeld atom refinement (HAR). We have applied HAR to 81 crystal structures of organic molecules and compared the A–H bond lengths with those from neutron measurements for A–H bonds sorted into bonds of the same class. We further show in a selection of inorganic compounds that hydrogen atoms can be located in bridging positions and close to heavy transition metals accurately and precisely. We anticipate that, in the future, conventional x-radiation sources at in-house diffractometers can be used routinely for locating hydrogen atoms in small molecules accurately instead of large-scale facilities such as spallation sources or nuclear reactors. PMID:27386545

Geant4 simulations of a wide-angle x-ray focusing telescope

NASA Astrophysics Data System (ADS)

Zhao, Donghua; Zhang, Chen; Yuan, Weimin; Zhang, Shuangnan; Willingale, Richard; Ling, Zhixing

2017-06-01

The rapid development of X-ray astronomy has been made possible by widely deploying X-ray focusing telescopes on board many X-ray satellites. Geant4 is a very powerful toolkit for Monte Carlo simulations and has remarkable abilities to model complex geometrical configurations. However, the library of physical processes available in Geant4 lacks a description of the reflection of X-ray photons at a grazing incident angle which is the core physical process in the simulation of X-ray focusing telescopes. The scattering of low-energy charged particles from the mirror surfaces is another noteworthy process which is not yet incorporated into Geant4. Here we describe a Monte Carlo model of a simplified wide-angle X-ray focusing telescope adopting lobster-eye optics and a silicon detector using the Geant4 toolkit. With this model, we simulate the X-ray tracing, proton scattering and background detection. We find that: (1) the effective area obtained using Geant4 is in agreement with that obtained using Q software with an average difference of less than 3%; (2) X-rays are the dominant background source below 10 keV; (3) the sensitivity of the telescope is better by at least one order of magnitude than that of a coded mask telescope with the same physical dimensions; (4) the number of protons passing through the optics and reaching the detector by Firsov scattering is about 2.5 times that of multiple scattering for the lobster-eye telescope.

Instrument and method for X-ray diffraction, fluorescence, and crystal texture analysis without sample preparation

NASA Technical Reports Server (NTRS)

Gendreau, Keith (Inventor); Martins, Jose Vanderlei (Inventor); Arzoumanian, Zaven (Inventor)

2010-01-01

An X-ray diffraction and X-ray fluorescence instrument for analyzing samples having no sample preparation includes a X-ray source configured to output a collimated X-ray beam comprising a continuum spectrum of X-rays to a predetermined coordinate and a photon-counting X-ray imaging spectrometer disposed to receive X-rays output from an unprepared sample disposed at the predetermined coordinate upon exposure of the unprepared sample to the collimated X-ray beam. The X-ray source and the photon-counting X-ray imaging spectrometer are arranged in a reflection geometry relative to the predetermined coordinate.

Philip A. Parilla | NREL

Science.gov Websites

atomic layer deposition for applications. He also manages the majority of X-ray characterization equipment at NREL, specifically X-ray diffraction and X-ray fluorescence instrumentation. Additionally, he for EERE's Hydrogen Storage program. He is also an expert in X-ray diffraction and X-ray fluorescence

A look inside epitaxial cobalt-on-fluorite nanoparticles with three-dimensional reciprocal space mapping using GIXD, RHEED and GISAXS.

PubMed

Suturin, S M; Fedorov, V V; Korovin, A M; Valkovskiy, G A; Konnikov, S G; Tabuchi, M; Sokolov, N S

2013-08-01

In this work epitaxial growth of cobalt on CaF 2 (111), (110) and (001) surfaces has been extensively studied. It has been shown by atomic force microscopy that at selected growth conditions stand-alone faceted Co nanoparticles are formed on a fluorite surface. Grazing-incidence X-ray diffraction (GIXD) and reflection high-energy electron diffraction (RHEED) studies have revealed that the particles crystallize in the face-centered cubic lattice structure otherwise non-achievable in bulk cobalt under normal conditions. The particles were found to inherit lattice orientation from the underlying CaF 2 layer. Three-dimensional reciprocal space mapping carried out using X-ray and electron diffraction has revealed that there exist long bright 〈111〉 streaks passing through the cobalt Bragg reflections. These streaks are attributed to stacking faults formed in the crystal lattice of larger islands upon coalescence of independently nucleated smaller islands. Distinguished from the stacking fault streaks, crystal truncation rods perpendicular to the {111} and {001} particle facets have been observed. Finally, grazing-incidence small-angle X-ray scattering (GISAXS) has been applied to decouple the shape-related scattering from that induced by the crystal lattice defects. Particle faceting has been verified by modeling the GISAXS patterns. The work demonstrates the importance of three-dimensional reciprocal space mapping in the study of epitaxial nanoparticles.

A look inside epitaxial cobalt-on-fluorite nanoparticles with three-dimensional reciprocal space mapping using GIXD, RHEED and GISAXS

PubMed Central

Suturin, S. M.; Fedorov, V. V.; Korovin, A. M.; Valkovskiy, G. A.; Konnikov, S. G.; Tabuchi, M.; Sokolov, N. S.

2013-01-01

In this work epitaxial growth of cobalt on CaF2(111), (110) and (001) surfaces has been extensively studied. It has been shown by atomic force microscopy that at selected growth conditions stand-alone faceted Co nanoparticles are formed on a fluorite surface. Grazing-incidence X-ray diffraction (GIXD) and reflection high-energy electron diffraction (RHEED) studies have revealed that the particles crystallize in the face-centered cubic lattice structure otherwise non-achievable in bulk cobalt under normal conditions. The particles were found to inherit lattice orientation from the underlying CaF2 layer. Three-dimensional reciprocal space mapping carried out using X-ray and electron diffraction has revealed that there exist long bright 〈111〉 streaks passing through the cobalt Bragg reflections. These streaks are attributed to stacking faults formed in the crystal lattice of larger islands upon coalescence of independently nucleated smaller islands. Distinguished from the stacking fault streaks, crystal truncation rods perpendicular to the {111} and {001} particle facets have been observed. Finally, grazing-incidence small-angle X-ray scattering (GISAXS) has been applied to decouple the shape-related scattering from that induced by the crystal lattice defects. Particle faceting has been verified by modeling the GISAXS patterns. The work demonstrates the importance of three-dimensional reciprocal space mapping in the study of epitaxial nanoparticles. PMID:24046491

Geant4 simulations of soft proton scattering in X-ray optics. A tentative validation using laboratory measurements

NASA Astrophysics Data System (ADS)

Fioretti, Valentina; Mineo, Teresa; Bulgarelli, Andrea; Dondero, Paolo; Ivanchenko, Vladimir; Lei, Fan; Lotti, Simone; Macculi, Claudio; Mantero, Alfonso

2017-12-01

Low energy protons (< 300 keV) can enter the field of view of X-ray telescopes, scatter on their mirror surfaces at small incident angles, and deposit energy on the detector. This phenomenon can cause intense background flares at the focal plane decreasing the mission observing time (e.g. the XMM-Newton mission) or in the most extreme cases, damaging the X-ray detector. A correct modelization of the physics process responsible for the grazing angle scattering processes is mandatory to evaluate the impact of such events on the performance (e.g. observation time, sensitivity) of future X-ray telescopes as the ESA ATHENA mission. The Remizovich model describes particles reflected by solids at glancing angles in terms of the Boltzmann transport equation using the diffuse approximation and the model of continuous slowing down in energy. For the first time this solution, in the approximation of no energy losses, is implemented, verified, and qualitatively validated on top of the Geant4 release 10.2, with the possibility to add a constant energy loss to each interaction. This implementation is verified by comparing the simulated proton distribution to both the theoretical probability distribution and with independent ray-tracing simulations. Both the new scattering physics and the Coulomb scattering already built in the official Geant4 distribution are used to reproduce the latest experimental results on grazing angle proton scattering. At 250 keV multiple scattering delivers large proton angles and it is not consistent with the observation. Among the tested models, the single scattering seems to better reproduce the scattering efficiency at the three energies but energy loss obtained at small scattering angles is significantly lower than the experimental values. In general, the energy losses obtained in the experiment are higher than what obtained by the simulation. The experimental data are not completely representative of the soft proton scattering experienced by current X-ray telescopes because of the lack of measurements at low energies (< 200 keV) and small reflection angles, so we are not able to address any of the tested models as the one that can certainly reproduce the scattering behavior of low energy protons expected for the ATHENA mission. We can, however, discard multiple scattering as the model able to reproduce soft proton funnelling, and affirm that Coulomb single scattering can represent, until further measurements at lower energies are available, the best approximation of the proton scattered angular distribution at the exit of X-ray optics.

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

Simulations of X-ray diffraction of shock-compressed single-crystal tantalum with synchrotron undulator sources.

PubMed

Tang, M X; Zhang, Y Y; E, J C; Luo, S N

2018-05-01

Polychromatic synchrotron undulator X-ray sources are useful for ultrafast single-crystal diffraction under shock compression. Here, simulations of X-ray diffraction of shock-compressed single-crystal tantalum with realistic undulator sources are reported, based on large-scale molecular dynamics simulations. Purely elastic deformation, elastic-plastic two-wave structure, and severe plastic deformation under different impact velocities are explored, as well as an edge release case. Transmission-mode diffraction simulations consider crystallographic orientation, loading direction, incident beam direction, X-ray spectrum bandwidth and realistic detector size. Diffraction patterns and reciprocal space nodes are obtained from atomic configurations for different loading (elastic and plastic) and detection conditions, and interpretation of the diffraction patterns is discussed.

Simulations of X-ray diffraction of shock-compressed single-crystal tantalum with synchrotron undulator sources

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

Tang, M. X.; Zhang, Y. Y.; E, J. C.

Polychromatic synchrotron undulator X-ray sources are useful for ultrafast single-crystal diffraction under shock compression. Here, simulations of X-ray diffraction of shock-compressed single-crystal tantalum with realistic undulator sources are reported, based on large-scale molecular dynamics simulations. Purely elastic deformation, elastic–plastic two-wave structure, and severe plastic deformation under different impact velocities are explored, as well as an edge release case. Transmission-mode diffraction simulations consider crystallographic orientation, loading direction, incident beam direction, X-ray spectrum bandwidth and realistic detector size. Diffraction patterns and reciprocal space nodes are obtained from atomic configurations for different loading (elastic and plastic) and detection conditions, and interpretation of themore » diffraction patterns is discussed.« less

Coherent X-ray diffraction imaging of nanoengineered polymeric capsules

NASA Astrophysics Data System (ADS)

Erokhina, S.; Pastorino, L.; Di Lisa, D.; Kiiamov, A. G.; Faizullina, A. R.; Tayurskii, D. A.; Iannotta, S.; Erokhin, V.

2017-10-01

For the first time, nanoengineered polymeric capsules and their architecture have been studied with coherent X-ray diffraction imaging technique. The use of coherent X-ray diffraction imaging technique allowed us to analyze the samples immersed in a liquid. We report about the significant difference between polymeric capsule architectures under dry and liquid conditions.

Thick-Filament Strain and Interfilament Spacing in Passive Muscle: Effect of Titin-Based Passive Tension

PubMed Central

Irving, Thomas; Wu, Yiming; Bekyarova, Tanya; Farman, Gerrie P.; Fukuda, Norio; Granzier, Henk

2011-01-01

We studied the effect of titin-based passive tension on sarcomere structure by simultaneously measuring passive tension and low-angle x-ray diffraction patterns on passive fiber bundles from rabbit skinned psoas muscle. We used a stretch-hold-release protocol with measurement of x-ray diffraction patterns at various passive tension levels during the hold phase before and after passive stress relaxation. Measurements were performed in relaxing solution without and with dextran T-500 to compress the lattice toward physiological levels. The myofilament lattice spacing was measured in the A-band (d1,0) and Z-disk (dZ) regions of the sarcomere. The axial spacing of the thick-filament backbone was determined from the sixth myosin meridional reflection (M6) and the equilibrium positions of myosin heads from the fourth myosin layer line peak position and the I1,1/I1,0 intensity ratio. Total passive tension was measured during the x-ray experiments, and a differential extraction technique was used to determine the relations between collagen- and titin-based passive tension and sarcomere length. Within the employed range of sarcomere lengths (∼2.2–3.4 μm), titin accounted for >80% of passive tension. X-ray results indicate that titin compresses both the A-band and Z-disk lattice spacing with viscoelastic behavior when fibers are swollen after skinning, and elastic behavior when the lattice is reduced with dextran. Titin also increases the axial thick-filament spacing, M6, in an elastic manner in both the presence and absence of dextran. No changes were detected in either I1,1/I1,0 or the position of peaks on the fourth myosin layer line during passive stress relaxation. Passive tension and M6 measurements were converted to thick-filament compliance, yielding a value of ∼85 m/N, which is several-fold larger than the thick-filament compliance determined by others during the tetanic tension plateau of activated intact muscle. This difference can be explained by the fact that thick filaments are more compliant at low tension (passive muscle) than at high tension (tetanic tension). The implications of our findings are discussed. PMID:21402032

Synthesis of Thermoresponsive Amphiphilic Polyurethane Gel as a New Cell Printing Material near Body Temperature.

PubMed

Tsai, Yi-Chun; Li, Suming; Hu, Shiaw-Guang; Chang, Wen-Chi; Jeng, U-Ser; Hsu, Shan-hui

2015-12-23

Waterborne polyurethane (PU) based on poly(ε-caprolactone) (PCL) diol and a second oligodiol containing amphiphilic blocks was synthesized in this study. The microstructure was characterized by dynamic light scattering (DLS), small-angle X-ray scattering (SAXS), and rheological measurement of the PU dispersion. The surface hydrophilicity measurement, infrared spectroscopy, wide-angle X-ray diffraction, mechanical and thermal analyses were conducted in solid state. It was observed that the presence of a small amount of amphiphilic blocks in the soft segment resulted in significant changes in microstructure. When 90 mol % PCL diol and 10 mol % amphiphilic blocks of poly(l-lactide)-poly(ethylene oxide) (PLLA-PEO) diol were used as the soft segment, the synthesized PU had a water contact angle of ∼24° and degree of crystallinity of ∼14%. The dispersion had a low viscosity below room temperature. As the temperature was raised to body temperature (37 °C), the dispersion rapidly (∼170 s) underwent sol-gel transition with excellent gel modulus (G' ≈ 6.5 kPa) in 20 min. PU dispersions with a solid content of 25-30% could be easily mixed with cells in sol state, extruded by a 3D printer, and deposited layer by layer as a gel. Cells remained alive and proliferating in the printed hydrogel scaffold. We expect that the development of novel thermoresponsive PU system can be used as smart injectable hydrogel and applied as a new type of bio-3D printing ink.

Direct Observation of Active Material Concentration Gradients and Crystallinity Breakdown in LiFePO4 Electrodes During Charge/Discharge Cycling of Lithium Batteries.

PubMed

Roberts, Matthew R; Madsen, Alex; Nicklin, Chris; Rawle, Jonathan; Palmer, Michael G; Owen, John R; Hector, Andrew L

2014-04-03

The phase changes that occur during discharge of an electrode comprised of LiFePO 4 , carbon, and PTFE binder have been studied in lithium half cells by using X-ray diffraction measurements in reflection geometry. Differences in the state of charge between the front and the back of LiFePO 4 electrodes have been visualized. By modifying the X-ray incident angle the depth of penetration of the X-ray beam into the electrode was altered, allowing for the examination of any concentration gradients that were present within the electrode. At high rates of discharge the electrode side facing the current collector underwent limited lithium insertion while the electrode as a whole underwent greater than 50% of discharge. This behavior is consistent with depletion at high rate of the lithium content of the electrolyte contained in the electrode pores. Increases in the diffraction peak widths indicated a breakdown of crystallinity within the active material during cycling even during the relatively short duration of these experiments, which can also be linked to cycling at high rate.

Direct Observation of Active Material Concentration Gradients and Crystallinity Breakdown in LiFePO4 Electrodes During Charge/Discharge Cycling of Lithium Batteries

PubMed Central

2014-01-01

The phase changes that occur during discharge of an electrode comprised of LiFePO4, carbon, and PTFE binder have been studied in lithium half cells by using X-ray diffraction measurements in reflection geometry. Differences in the state of charge between the front and the back of LiFePO4 electrodes have been visualized. By modifying the X-ray incident angle the depth of penetration of the X-ray beam into the electrode was altered, allowing for the examination of any concentration gradients that were present within the electrode. At high rates of discharge the electrode side facing the current collector underwent limited lithium insertion while the electrode as a whole underwent greater than 50% of discharge. This behavior is consistent with depletion at high rate of the lithium content of the electrolyte contained in the electrode pores. Increases in the diffraction peak widths indicated a breakdown of crystallinity within the active material during cycling even during the relatively short duration of these experiments, which can also be linked to cycling at high rate. PMID:24790684

Stages in molecular beam epitaxy growth of GaAs nanowires studied by x-ray diffraction.

PubMed

Mariager, Simon O; Lauridsen, Søren L; Sørensen, Claus B; Dohn, Asmus; Willmott, Phillip R; Nygård, Jesper; Feidenhans'l, Robert

2010-03-19

GaAs nanowires were grown by molecular beam epitaxy and studied by glancing-angle x-ray diffraction during five different stages of the growth process. An entire forest of randomly positioned epitaxial nanowires was sampled simultaneously and a large variation in the Au-Ga catalyst was found. Au, AuGa, AuGa(2) and the hexagonal beta phase were all identified in several orientations and in similar amounts. The nanowires are shown to consist of regular zinc blende crystal, its twin and the hexagonal wurtzite. The evolution of the various Au-Ga catalysts and the development in the twin to the wurtzite abundance ratio indicate that the Au catalyst is saturated upon initiation of growth leading to an increased amount of wurtzite structure in the wires. A specular x-ray scan identifies the various Au-Ga alloys, three Au lattice constants and a rough interface between nanowires and catalyst. Reciprocal space maps were obtained around Au Bragg points and show the development of the Au catalyst from a distribution largely oriented with respect to the lattice to a non-uniform distribution with several well-defined lattice constants.

White-beam X-ray diffraction and radiography studies on high-boron-containing borosilicate glass at high pressures

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

Ham, Kathryn J.; Vohra, Yogesh K.; Kono, Yoshio

Multi-angle energy-dispersive X-ray diffraction studies and white-beam X-ray radiography were conducted with a cylindrically shaped (1 mm diameter and 0.7 mm high) high-boron-content borosilicate glass sample (17.6% B 2O 3) to a pressure of 13.7 GPa using a Paris-Edinburgh (PE) press at Beamline 16-BM-B, HPCAT of the Advanced Photon Source. The measured structure factor S(q) to large q = 19 Å –1 is used to determine information about the internuclear bond distances between various species of atoms within the glass sample. Sample pressure was determined with gold as a pressure standard. The sample height as measured by radiography showed anmore » overall uniaxial compression of 22.5% at 13.7 GPa with 10.6% permanent compaction after decompression to ambient conditions. The reduced pair distribution function G(r) was extracted and Si–O, O–O and Si–Si bond distances were measured as a function of pressure. Lastly, Raman spectroscopy of the pressure recovered sample as compared to starting material showed blue-shift and changes in intensity and widths of Raman bands associated with silicate and four-coordinated boron.« less

White-beam X-ray diffraction and radiography studies on high-boron-containing borosilicate glass at high pressures

DOE PAGES

Ham, Kathryn J.; Vohra, Yogesh K.; Kono, Yoshio; ...

2017-02-06

Multi-angle energy-dispersive X-ray diffraction studies and white-beam X-ray radiography were conducted with a cylindrically shaped (1 mm diameter and 0.7 mm high) high-boron-content borosilicate glass sample (17.6% B 2O 3) to a pressure of 13.7 GPa using a Paris-Edinburgh (PE) press at Beamline 16-BM-B, HPCAT of the Advanced Photon Source. The measured structure factor S(q) to large q = 19 Å –1 is used to determine information about the internuclear bond distances between various species of atoms within the glass sample. Sample pressure was determined with gold as a pressure standard. The sample height as measured by radiography showed anmore » overall uniaxial compression of 22.5% at 13.7 GPa with 10.6% permanent compaction after decompression to ambient conditions. The reduced pair distribution function G(r) was extracted and Si–O, O–O and Si–Si bond distances were measured as a function of pressure. Lastly, Raman spectroscopy of the pressure recovered sample as compared to starting material showed blue-shift and changes in intensity and widths of Raman bands associated with silicate and four-coordinated boron.« less

Universal amorphous-amorphous transition in GexSe100-x glasses under pressure

NASA Astrophysics Data System (ADS)

Yildirim, Can; Micoulaut, Matthieu; Boolchand, Punit; Kantor, Innokenty; Mathon, Olivier; Gaspard, Jean-Pierre; Irifune, Tetsuo; Raty, Jean-Yves

2016-06-01

Pressure induced structural modifications in vitreous GexSe100-x (where 10 ≤ x ≤ 25) are investigated using X-ray absorption spectroscopy (XAS) along with supplementary X-ray diffraction (XRD) experiments and ab initio molecular dynamics (AIMD) simulations. Universal changes in distances and angle distributions are observed when scaled to reduced densities. All compositions are observed to remain amorphous under pressure values up to 42 GPa. The Ge-Se interatomic distances extracted from XAS data show a two-step response to the applied pressure; a gradual decrease followed by an increase at around 15-20 GPa, depending on the composition. This increase is attributed to the metallization event that can be traced with the red shift in Ge K edge energy which is also identified by the principal peak position of the structure factor. The densification mechanisms are studied in details by means of AIMD simulations and compared to the experimental results. The evolution of bond angle distributions, interatomic distances and coordination numbers are examined and lead to similar pressure-induced structural changes for any composition.

X-Ray Structure determination of the Glycine Cleavage System Protein H of Mycobacterium tuberculosis Using An Inverse Compton Synchrotron X-Ray Source

PubMed Central

Abendroth, Jan; McCormick, Michael S.; Edwards, Thomas E.; Staker, Bart; Loewen, Roderick; Gifford, Martin; Rifkin, Jeff; Mayer, Chad; Guo, Wenjin; Zhang, Yang; Myler, Peter; Kelley, Angela; Analau, Erwin; Hewitt, Stephen Nakazawa; Napuli, Alberto J.; Kuhn, Peter; Ruth, Ronald D.; Stewart, Lance J.

2010-01-01

Structural genomics discovery projects require ready access to both X-ray and NMR instrumentation which support the collection of experimental data needed to solve large numbers of novel protein structures. The most productive X-ray crystal structure determination laboratories make extensive frequent use of tunable synchrotron X-ray light to solve novel structures by anomalous diffraction methods. This requires that frozen cryo-protected crystals be shipped to large government-run synchrotron facilities for data collection. In an effort to eliminate the need to ship crystals for data collection, we have developed the first laboratory-scale synchrotron light source capable of performing many of the state-of-the-art synchrotron applications in X-ray science. This Compact Light Source is a first-in-class device that uses inverse Compton scattering to generate X-rays of sufficient flux, tunable wavelength and beam size to allow high-resolution X-ray diffraction data collection from protein crystals. We report on benchmarking tests of X-ray diffraction data collection with hen egg white lysozyme, and the successful high-resolution X-ray structure determination of the Glycine cleavage system protein H from Mycobacterium tuberculosis using diffraction data collected with the Compact Light Source X-ray beam. PMID:20364333

When is one layer complete? Using simultaneous in-situ RHEED and x-ray reflectivity to map layer-by-layer thin-film oxide growth

NASA Astrophysics Data System (ADS)

Sullivan, M. C.; Ward, M. J.; Joress, H.; Gutierrez-Llorente, A.; White, A. E.; Woll, A.; Brock, J. D.

2014-03-01

The most popular tool for characterizing in situ layer-by-layer growth is Reflection High-Energy Electron Diffraction (RHEED). X-ray reflectivity can also be used to study layer-by-layer growth, as long as the incident angle of the x-rays is far from a Bragg peak. During layer-by-layer homoepitaxial growth, both the RHEED intensity and the reflected x-ray intensity will oscillate, and each complete oscillation indicates the addition of one layer of material. However, it is well documented, but not well understood, that the maxima in the RHEED intensity oscillations do not necessarily occur at the completion of a layer. In contrast, the maxima in the x-ray intensity oscillations do occur at the completion of a layer, thus the RHEED and x-ray oscillations are rarely in phase. We present our results on simultaneous in situ x-ray reflectivity and RHEED during layer-by-layer growth of SrTiO3 and discuss how to determine the completion of a layer for RHEED oscillations independent of the phase of the RHEED oscillation. Supported by DOE Office of Basic Energy Sciences Award DE-SC0001086, CHESS is supported by the NSF & NIH/NIGMS via NSF award DMR-0936384.

Negative thermal expansion and magnetoelastic coupling in the breathing pyrochlore lattice material LiGaCr 4 S 8

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

Pokharel, G.; May, A. F.; Parker, D. S.

In this paper, the physical properties of the spinel LiGaCr 4S 8 have been studied with neutron diffraction, x-ray diffraction, magnetic susceptibility, and heat capacity measurements. The neutron diffraction and synchrotron x-ray diffraction data reveal negative thermal expansion (NTE) below 111(4) K. The magnetic susceptibility deviates from Curie-Weiss behavior with the onset of NTE. At low temperature a broad peak in the magnetic susceptibility at 10.3(3) K is accompanied by the return of normal thermal expansion. First-principles calculations find a strong coupling between the lattice and the simulated magnetic ground state. Finally, these results indicate strong magnetoelastic coupling in LiGaCrmore » 4S 8.« less

Negative thermal expansion and magnetoelastic coupling in the breathing pyrochlore lattice material LiGaCr 4 S 8

DOE PAGES

Pokharel, G.; May, A. F.; Parker, D. S.; ...

2018-04-30

In this paper, the physical properties of the spinel LiGaCr 4S 8 have been studied with neutron diffraction, x-ray diffraction, magnetic susceptibility, and heat capacity measurements. The neutron diffraction and synchrotron x-ray diffraction data reveal negative thermal expansion (NTE) below 111(4) K. The magnetic susceptibility deviates from Curie-Weiss behavior with the onset of NTE. At low temperature a broad peak in the magnetic susceptibility at 10.3(3) K is accompanied by the return of normal thermal expansion. First-principles calculations find a strong coupling between the lattice and the simulated magnetic ground state. Finally, these results indicate strong magnetoelastic coupling in LiGaCrmore » 4S 8.« less

Anti-contamination device for cryogenic soft X-ray diffraction microscopy

DOE PAGES

Huang, Xiaojing; Miao, Huijie; Nelson, Johanna; ...

2011-05-01

Cryogenic microscopy allows one to view frozen hydrated biological and soft matter specimens with good structural preservation and a high degree of stability against radiation damage. We describe a liquid nitrogen-cooled anti-contamination device for cryogenic X-ray diffraction microscopy. The anti-contaminator greatly reduces the buildup of ice layers on the specimen due to condensation of residual water vapor in the experimental vacuum chamber. We show by coherent X-ray diffraction measurements that this leads to fivefold reduction of background scattering, which is important for far-field X-ray diffraction microscopy of biological specimens.

Incorporation of Cadmium and Nickel into Ferrite Spinel Solid Solution: X-ray Diffraction and X-ray Absorption Fine Structure Analyses.

PubMed

Su, Minhua; Liao, Changzhong; Chan, Tingshan; Shih, Kaimin; Xiao, Tangfu; Chen, Diyun; Kong, Lingjun; Song, Gang

2018-01-16

The feasibility of incorporating Cd and Ni in hematite was studied by investigating the interaction mechanism for the formation of Cd x Ni 1-x Fe 2 O 4 solid solutions (CNFs) from CdO, NiO, and α-Fe 2 O 3 . X-ray diffraction results showed that the CNFs crystallized into spinel structures with increasing lattice parameters as the Cd content in the precursors was increased. Cd 2+ ions were found to occupy the tetrahedral sites, as evidenced by Rietveld refinement and extended X-ray absorption fine structure analyses. The incorporation of Cd and Ni into ferrite spinel solid solution strongly relied on the processing parameters. The incorporation of Cd and Ni into the CNFs was greater at high x values (0.7 < x ≤ 1.0) than at low x values (0.0 ≤ x ≤ 0.7). A feasible treatment technique based on the investigated mechanism of CNF formation was developed, involving thermal treatment of waste sludge containing Cd and Ni. Both of these metals in the waste sludge were successfully incorporated into a ferrite spinel solid solution, and the concentrations of leached Cd and Ni from this solid solution were substantially reduced, stabilizing at low levels. This research offers a highly promising approach for treating the Cd and Ni content frequently encountered in electronic waste and its treatment residues.

Observation of electromigration in a Cu thin line by in situ coherent x-ray diffraction microscopy

NASA Astrophysics Data System (ADS)

Takahashi, Yukio; Nishino, Yoshinori; Furukawa, Hayato; Kubo, Hideto; Yamauchi, Kazuto; Ishikawa, Tetsuya; Matsubara, Eiichiro

2009-06-01

Electromigration (EM) in a 1-μm-thick Cu thin line was investigated by in situ coherent x-ray diffraction microscopy (CXDM). Characteristic x-ray speckle patterns due to both EM-induced voids and thermal deformation in the thin line were observed in the coherent x-ray diffraction patterns. Both parts of the voids and the deformation were successfully visualized in the images reconstructed from the diffraction patterns. This result not only represents the first demonstration of the visualization of structural changes in metallic materials by in situ CXDM but is also an important step toward studying the structural dynamics of nanomaterials using x-ray free-electron lasers in the near future.

Gas gun shock experiments with single-pulse x-ray phase contrast imaging and diffraction at the Advanced Photon Source

NASA Astrophysics Data System (ADS)

Luo, S. N.; Jensen, B. J.; Hooks, D. E.; Fezzaa, K.; Ramos, K. J.; Yeager, J. D.; Kwiatkowski, K.; Shimada, T.

2012-07-01

The highly transient nature of shock loading and pronounced microstructure effects on dynamic materials response call for in situ, temporally and spatially resolved, x-ray-based diagnostics. Third-generation synchrotron x-ray sources are advantageous for x-ray phase contrast imaging (PCI) and diffraction under dynamic loading, due to their high photon fluxes, high coherency, and high pulse repetition rates. The feasibility of bulk-scale gas gun shock experiments with dynamic x-ray PCI and diffraction measurements was investigated at the beamline 32ID-B of the Advanced Photon Source. The x-ray beam characteristics, experimental setup, x-ray diagnostics, and static and dynamic test results are described. We demonstrate ultrafast, multiframe, single-pulse PCI measurements with unprecedented temporal (<100 ps) and spatial (˜2 μm) resolutions for bulk-scale shock experiments, as well as single-pulse dynamic Laue diffraction. The results not only substantiate the potential of synchrotron-based experiments for addressing a variety of shock physics problems, but also allow us to identify the technical challenges related to image detection, x-ray source, and dynamic loading.

X-ray Diffraction Gratings for Astrophysics

NASA Astrophysics Data System (ADS)

Paerels, Frits

2010-12-01

Over the past year, we have celebrated the tenth anniversary of the Chandra and XMM-Newton X-ray observatories. Both carry powerful, novel diffraction grating spectrometers, which have opened true X-ray spectroscopy for astrophysics. I will describe the design and operation of these instruments, as the background to some of the beautiful results they have produced. But these designs do not exhaust the versatility and essential simplicity of diffraction grating spectrometers, and I will discuss applications for the International X-ray Observatory IXO.

Partially coherent X-ray wavefront propagation simulations including grazing-incidence focusing optics.

PubMed

Canestrari, Niccolo; Chubar, Oleg; Reininger, Ruben

2014-09-01

X-ray beamlines in modern synchrotron radiation sources make extensive use of grazing-incidence reflective optics, in particular Kirkpatrick-Baez elliptical mirror systems. These systems can focus the incoming X-rays down to nanometer-scale spot sizes while maintaining relatively large acceptance apertures and high flux in the focused radiation spots. In low-emittance storage rings and in free-electron lasers such systems are used with partially or even nearly fully coherent X-ray beams and often target diffraction-limited resolution. Therefore, their accurate simulation and modeling has to be performed within the framework of wave optics. Here the implementation and benchmarking of a wave-optics method for the simulation of grazing-incidence mirrors based on the local stationary-phase approximation or, in other words, the local propagation of the radiation electric field along geometrical rays, is described. The proposed method is CPU-efficient and fully compatible with the numerical methods of Fourier optics. It has been implemented in the Synchrotron Radiation Workshop (SRW) computer code and extensively tested against the geometrical ray-tracing code SHADOW. The test simulations have been performed for cases without and with diffraction at mirror apertures, including cases where the grazing-incidence mirrors can be hardly approximated by ideal lenses. Good agreement between the SRW and SHADOW simulation results is observed in the cases without diffraction. The differences between the simulation results obtained by the two codes in diffraction-dominated cases for illumination with fully or partially coherent radiation are analyzed and interpreted. The application of the new method for the simulation of wavefront propagation through a high-resolution X-ray microspectroscopy beamline at the National Synchrotron Light Source II (Brookhaven National Laboratory, USA) is demonstrated.

Amorphous boron gasket in diamond anvil cell research

NASA Astrophysics Data System (ADS)

Lin, Jung-Fu; Shu, Jinfu; Mao, Ho-kwang; Hemley, Russell J.; Shen, Guoyin

2003-11-01

Recent advances in high-pressure diamond anvil cell experiments include high-energy synchrotron x-ray techniques as well as new cell designs and gasketing procedures. The success of high-pressure experiments usually depends on a well-prepared sample, in which the gasket plays an important role. Various gasket materials such as diamond, beryllium, rhenium, and stainless steel have been used. Here we introduce amorphous boron as another gasket material in high-pressure diamond anvil cell experiments. We have applied the boron gasket for laser-heating x-ray diffraction, radial x-ray diffraction, nuclear resonant inelastic x-ray scattering, and inelastic x-ray scattering. The high shear strength of the amorphous boron maximizes the thickness of the sample chamber and increases the pressure homogeneity, improving the quality of high-pressure data. Use of amorphous boron avoids unwanted x-ray diffraction peaks and reduces the absorption of incident and x rays exiting the gasket material. The high quality of the diffraction patterns makes it possible to refine the cell parameters with powder x-ray diffraction data under high pressure and high temperature. The reactivity of boron prevents its use at high temperatures, however. When heated, boron may also react with the specimen to produce unwanted phases. The relatively porous boron starting material at ambient conditions also poses some challenges for sample preparation.

Morphology and crystallinity of ZnS nanocolumns prepared by glancing angle deposition.

PubMed

Lu, Lifang; Zhang, Fujun; Xu, Zheng; Zhao, Suling; Wang, Yongsheng

2010-03-01

ZnS films with different morphologies and nanometer structures were fabricated via high vacuum electron beam deposition by changing the oblique angle alpha between the incoming particle flux and the substrate normal. The morphology and crystallinity of ZnS nanocrystalline films prepared on the substrates at alpha = 0 degrees and 80 degrees were characterized by scanning electron microscopy (SEM), atomic force microscopy (AFM), and X-ray diffraction. These experimental results show that the ZnS nanocolumn structure was formed at the situation of alpha = 80 degrees. The incidence angle also strongly influenced the crystallinity of thin films. The most intensive diffraction peaks changed from (220) to (111) when the incidence angle was set to 0 degrees and 80 degrees. The dynamic growth process of ZnS films at alpha = 0 degrees and 80 degrees has been analyzed by shadow effect and atomic surface diffusion. The transmittance spectra of the ZnS thin films prepared at different oblique angles were measured, and the transmissivity of ZnS nanocolumn thin films was enhanced compared with ZnS thin films prepared by normal deposition in the visible light range.

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

Jones, K.M.; Al-Jassim, M.M.; Williamson, D.L.

Over the last two decades extensive studies on the optical and electrical properties of hydrogenated amorphous Si (a-Si:H) have been reported. However, less attention was given to the structural characterization of this material partly due to the insensitivity to hydrogen of structural probes such as x-rays and electron diffraction. From a recent set of experiments, results on the solubility limit of hydrogen in a special type of a-Si:H and the characterization of hydrogen induced complexes or nanobubbles has been reported. In this study, we report TEM observations of the structural morphology of hydrogen related defects that support these recent measurementsmore » obtained by secondary ion mass spectrometry (SIMS) and small-angle x-ray scattering (SAXS).« less

Effect of interparticle interactions on size determination of zirconia and silica based systems – A comparison of SAXS, DLS, BET, XRD and TEM

PubMed Central

Pabisch, Silvia; Feichtenschlager, Bernhard; Kickelbick, Guido; Peterlik, Herwig

2012-01-01

The aim of this work is a systematic comparison of size characterisation methods for two completely different model systems of oxide nanoparticles, i.e. amorphous spherical silica and anisotropic facet-shaped crystalline zirconia. Size and/or size distribution were determined in a wide range from 5 to 70 nm using small-angle X-ray scattering (SAXS), dynamic light scattering (DLS), nitrogen sorption (BET), X-ray diffraction (XRD) and transmission electron microscopy (TEM). A nearly perfect coincidence was observed only for SAXS and TEM for both types of particles. For zirconia nanoparticles considerable differences between different measurement methods were observed. PMID:22347721

Correlated oxygen displacements and phonon mode changes in LaCoO3 single crystal

NASA Astrophysics Data System (ADS)

Sikolenko, V. V.; Molodtsov, S. L.; Izquierdo, M.; Troyanchuk, I. O.; Karpinsky, D.; Tiutiunnikov, S. I.; Efimova, E.; Prabhakaran, D.; Novoselov, D.; Efimov, V.

2018-05-01

X-ray diffraction and inelastic X-ray scattering studies have been performed across the spin ( 100 K) and semiconductor-metal ( 500 K) transitions in LaCoO3 single crystals. The quadratic increase with temperature of the oxygen displacement parameters parallel and perpendicular to the Co-O bond has been correlated with softening of the TO2 and hardening of the TO1 phonon branches along the [0 ξ ξ] high symmetry direction. The latter effect can be associated with the weakening of the Co-O bond strength derived from the increase of Co-O bond length and angle as expected upon increasing the high spin state population of the system with temperature.

Multislice imaging of integrated circuits by precession X-ray ptychography.

PubMed

Shimomura, Kei; Hirose, Makoto; Takahashi, Yukio

2018-01-01

A method for nondestructively visualizing multisection nanostructures of integrated circuits by X-ray ptychography with a multislice approach is proposed. In this study, tilt-series ptychographic diffraction data sets of a two-layered circuit with a ∼1.4 µm gap at nine incident angles are collected in a wide Q range and then artifact-reduced phase images of each layer are successfully reconstructed at ∼10 nm resolution. The present method has great potential for the three-dimensional observation of flat specimens with thickness on the order of 100 µm, such as three-dimensional stacked integrated circuits based on through-silicon vias, without laborious sample preparation.

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.

Determination of the real structure of artificial and natural opals on the basis of three-dimensional reconstructions of reciprocal space

NASA Astrophysics Data System (ADS)

Eliseev, A. A.; Gorozhankin, D. F.; Napolskii, K. S.; Petukhov, A. V.; Sapoletova, N. A.; Vasilieva, A. V.; Grigoryeva, N. A.; Mistonov, A. A.; Byelov, D. V.; Bouwman, W. G.; Kvashnina, K. O.; Chernyshov, D. Yu.; Bosak, A. A.; Grigoriev, S. V.

2009-10-01

The distribution of the scattering intensity in the reciprocal space for natural and artificial opals has been reconstructed from a set of small-angle X-ray diffraction patterns. The resulting three-dimensional intensity maps are used to analyze the defect structure of opals. The structure of artificial opals can be satisfactorily described in the Wilson probability model with the prevalence of layers in the fcc environment. The diffraction patterns observed for a natural opal confirm the presence of sufficiently long unequally occupied fcc domains.

Si Lattice, Avogadro Constant, and X- and Gamma-Ray Measurements: Contributions by R.D. Deslattes

NASA Astrophysics Data System (ADS)

Kessler, Jr.

2002-04-01

The achievement of x-ray interferometry in 1965 opened the possibility of more accurately measuring the lattice spacing of a diffraction crystal on a scale directly tied to the SI system of units. The road from the possible to reality required moving objects and measuring translations with sub-atomic accuracy. The improved crystal lattice spacing determinations had a significant impact on two fundamental measurement areas: 1) the amount of substance (the mole and the associated Avogadro Constant), and 2) short wavelengths (the x- and gamma-ray regions). Progress in both areas required additional metrological advances: density and isotopic abundance measurements are needed for the Avogadro constant and small angle measurements are required for the determination of short wavelengths. The x- and gamma-ray measurements have led to more accurate wavelength standards and neutron binding energy measurements that connect gamma-ray measurements to precision atomic mass measurements, particularly the neutron mass. Richard D. Deslattes devoted much of his scientific career to this measurement program. His outstanding contributions and insights will be reviewed.

Microstructure evolution, thermal stability and fractal behavior of water vapor flow assisted in situ growth poly(vinylcarbazole)-titania quantum dots nanocomposites

NASA Astrophysics Data System (ADS)

Mombrú, Dominique; Romero, Mariano; Faccio, Ricardo; Mombrú, Alvaro W.

2017-12-01

Here, we report a novel strategy for the preparation of TiO2 quantum dots fillers prepared from alkoxide precursor via in situ water vapor flow diffusion into poly(N-vinylcarbazole) host. A detailed characterization by means of infrared and Raman spectroscopy, X-ray powder diffraction, small angle X-ray scattering and differential scanning calorimetry is reported. The growth mechanism of both crystallites and particles was mostly governed by the classical coarsening reaction limited growth and the polymer host showed no detectable chemical modifications at the interface or active participation in the growing process. The main relevance of our strategy respect to the typical sol-gel growth in solution is the possibility of the interruption of the reaction by simple stopping the water vapor flow diffusion into the polymer host thus achieving good control in the nanoparticles size. The thermal stability and fractal behavior of our nanocomposites were also studied by differential scanning calorimetry and in situ small angle X-ray scattering versus temperature. Strong correlations between modifications in the fractal behavior and glass transition or fusion processes were observed for these nanocomposites.

Probing Nucleation and Growth Behavior of Twisted Kebabs from Shish Scaffold in Sheared Polyethylene Melts by in situ X-ray Studies

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

Keum,J.; Burger, C.; Zuo, F.

2007-01-01

By utilizing synchrotron rheo-WAXD (wide-angle X-ray diffraction) and rheo-SAXS (small-angle X-ray scattering) techniques, the nucleation and growth behavior of twisted kebabs from the shear-induced shish scaffold in entangled high-density polyethylene (HDPE) melts were investigated. The evolution of the (110) reflection intensity in WAXD at the early stages of crystallization could be described by a simplified Avrami equation, while the corresponding long period of kebabs determined by SAXS was found to decrease with time. The combined SAXS and WAXD results indicate that the kebab growth in sheared HDPE melts consists of two-dimensional geometry with thermal (sporadic) nucleation. The WAXD data clearlymore » exhibited the transformations of (110) reflection from equatorial 2-arc to off-axis 4-arc and of (200) reflection from off-axis 4-arc to meridional 2-arc, which can be explained by the rotation of crystallographic a-axis around the b-axis during twisted kebab growth. This observation is also consistent with the orientation mode changes from 'Keller/Machin II' to 'intermediate' and then to 'Keller/Machin I'.« less

Investigations on the in vitro bioactivity of swift heavy oxygen ion irradiated hydroxyapatite.

PubMed

Suganthi, R V; Prakash Parthiban, S; Elayaraja, K; Girija, E K; Kulariya, P; Katharria, Y S; Singh, F; Asokan, K; Kanjilal, D; Narayana Kalkura, S

2009-12-01

The effect of swift heavy oxygen ion irradiation of hydroxyapatite on its in vitro bioactivity was studied. The irradiation experiment was performed using oxygen ions at energy of 100 MeV with 1 x 10(12) and 1 x 10(13) ions/cm2 fluence range. The irradiated samples were characterized by glancing angle X-ray diffraction (GXRD), photoluminescence spectroscopy (PL) and scanning electron microscopy (SEM). GXRD showed that irradiated samples exhibited better crystallinity. The irradiated samples revealed an increase in PL intensity. In addition, the irradiated hydroxyapatite was found to have enhanced bioactivity.

A study of the formation of amorphous calcium phosphate and hydroxyapatite on melt quenched Bioglass using surface sensitive shallow angle X-ray diffraction.

PubMed

Martin, R A; Twyman, H; Qiu, D; Knowles, J C; Newport, R J

2009-04-01

Melt quenched silicate glasses containing calcium, phosphorous and alkali metals have the ability to promote bone regeneration and to fuse to living bone. These glasses, including 45S5 Bioglass((R)) [(CaO)(26.9)(Na(2)O)(24.4)(SiO(2))(46.1)(P(2)O(5))(2.6)], are routinely used as clinical implants. Consequently there have been numerous studies on the structure of these glasses using conventional diffraction techniques. These studies have provided important information on the atomic structure of Bioglass((R)) but are of course intrinsically limited in the sense that they probe the bulk material and cannot be as sensitive to thin layers of near-surface dissolution/growth. The present study therefore uses surface sensitive shallow angle X-ray diffraction to study the formation of amorphous calcium phosphate and hydroxyapatite on Bioglass((R)) samples, pre-reacted in simulated body fluid (SBF). Unreacted Bioglass((R)) is dominated by a broad amorphous feature around 2.2 A(-1) which is characteristic of sodium calcium silicate glass. After reacting Bioglass((R)) in SBF a second broad amorphous feature evolves ~1.6 A(-1) which is attributed to amorphous calcium phosphate. This feature is evident for samples after only 4 h reacting in SBF and by 8 h the amorphous feature becomes comparable in magnitude to the background signal of the bulk Bioglass((R)). Bragg peaks characteristic of hydroxyapatite form after 1-3 days of reacting in SBF.

Hercules X-1: Spectral Variability of an X-Ray Pulsar in a Stellar Binary System. Ph.D. Thesis

NASA Technical Reports Server (NTRS)

Pravdo, S. H.

1976-01-01

A cosmic X-ray spectroscopy experiment onboard the Orbiting Solar Observatory 8 (OSO-8), observed Her x-1 continuously for approximately 8 days. Spectral-temporal correlations of the X-ray emission were obtained. The major results concern observations of: (1) iron band emission, (2) spectral hardening (increase in effective x-ray temperature) within the X-ray pulse, and (3) a transition from an X-ray low state to a high state. The spectrum obtained prior to the high state can be interpreted as reflected emission from a hot coronal gas surrounding an accretion disk, which itself shields the primary X-ray source from the line of sight during the low state. The spectral hardening within the X-ray pulse was indicative of the beaming mechanism at the neutron star surface. The hardest spectrum by pulse phase was identified with the line of sight close to the Her x-1 magnetic dipole axis, and the X-ray pencil beam become harder with decreasing angle between the line of sight and the dipole axis.

High numerical aperture multilayer Laue lenses

DOE PAGES

Morgan, Andrew J.; Prasciolu, Mauro; Andrejczuk, Andrzej; ...

2015-06-01

The ever-increasing brightness of synchrotron radiation sources demands improved X-ray optics to utilise their capability for imaging and probing biological cells, nanodevices, and functional matter on the nanometer scale with chemical sensitivity. Here we demonstrate focusing a hard X-ray beam to an 8 nm focus using a volume zone plate (also referred to as a wedged multilayer Laue lens). This lens was constructed using a new deposition technique that enabled the independent control of the angle and thickness of diffracting layers to microradian and nanometer precision, respectively. This ensured that the Bragg condition is satisfied at each point along themore » lens, leading to a high numerical aperture that is limited only by its extent. We developed a phase-shifting interferometric method based on ptychography to characterise the lens focus. The precision of the fabrication and characterisation demonstrated here provides the path to efficient X-ray optics for imaging at 1 nm resolution.« less

Transmission X-ray scattering as a probe for complex liquid-surface structures

DOE PAGES

Fukuto, Masafumi; Yang, Lin; Nykypanchuk, Dmytro; ...

2016-01-28

The need for functional materials calls for increasing complexity in self-assembly systems. As a result, the ability to probe both local structure and heterogeneities, such as phase-coexistence and domain morphologies, has become increasingly important to controlling self-assembly processes, including those at liquid surfaces. The traditional X-ray scattering methods for liquid surfaces, such as specular reflectivity and grazing-incidence diffraction, are not well suited to spatially resolving lateral heterogeneities due to large illuminated footprint. A possible alternative approach is to use scanning transmission X-ray scattering to simultaneously probe local intermolecular structures and heterogeneous domain morphologies on liquid surfaces. To test the feasibilitymore » of this approach, transmission small- and wide-angle X-ray scattering (TSAXS/TWAXS) studies of Langmuir films formed on water meniscus against a vertically immersed hydrophilic Si substrate were recently carried out. First-order diffraction rings were observed in TSAXS patterns from a monolayer of hexagonally packed gold nanoparticles and in TWAXS patterns from a monolayer of fluorinated fatty acids, both as a Langmuir monolayer on water meniscus and as a Langmuir–Blodgett monolayer on the substrate. The patterns taken at multiple spots have been analyzed to extract the shape of the meniscus surface and the ordered-monolayer coverage as a function of spot position. These results, together with continual improvement in the brightness and spot size of X-ray beams available at synchrotron facilities, support the possibility of using scanning-probe TSAXS/TWAXS to characterize heterogeneous structures at liquid surfaces.« less

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

X-Ray Diffraction and the Discovery of the Structure of DNA

ERIC Educational Resources Information Center

Crouse, David T.

2007-01-01

A method is described for teaching the analysis of X-ray diffraction of DNA through a series of steps utilizing the original methods used by James Watson, Francis Crick, Maurice Wilkins and Rosalind Franklin. The X-ray diffraction pattern led to the conclusion of the basic helical structure of DNA and its dimensions while basic chemical principles…

High Resolution X-Ray Diffraction of Macromolecules with Synchrotron Radiation

NASA Technical Reports Server (NTRS)

Stojanoff, Vivian; Boggon, Titus; Helliwell, John R.; Judge, Russell; Olczak, Alex; Snell, Edward H.; Siddons, D. Peter; Rose, M. Franklin (Technical Monitor)

2000-01-01

We recently combined synchrotron-based monochromatic X-ray diffraction topography methods with triple axis diffractometry and rocking curve measurements: high resolution X-ray diffraction imaging techniques, to better understand the quality of protein crystals. We discuss these methods in the light of results obtained on crystals grown under different conditions. These non destructive techniques are powerful tools in the characterization of the protein crystals and ultimately will allow to improve, develop, and understand protein crystal growth. High resolution X-ray diffraction imaging methods will be discussed in detail in light of recent results obtained on Hen Egg White Lysozyme crystals and other proteins.

Hard X-ray polarizer to enable simultaneous three-dimensional nanoscale imaging of magnetic structure and lattice strain

DOE PAGES

Logan, Jonathan; Harder, Ross; Li, Luxi; ...

2016-01-01

Recent progress in the development of dichroic Bragg coherent diffractive imaging, a new technique for simultaneous three-dimensional imaging of strain and magnetization at the nanoscale, is reported. This progress includes the installation of a diamond X-ray phase retarder at beamline 34-ID-C of the Advanced Photon Source. Here, the performance of the phase retarder for tuning X-ray polarization is demonstrated with temperature-dependent X-ray magnetic circular dichroism measurements on a gadolinium foil in transmission and on a Gd 5Si 2Ge 2crystal in diffraction geometry with a partially coherent, focused X-ray beam. Feasibility tests for dichroic Bragg coherent diffractive imaging are presented. Thesemore » tests include (1) using conventional Bragg coherent diffractive imaging to determine whether the phase retarder introduces aberrations using a nonmagnetic gold nanocrystal as a control sample, and (2) collecting coherent diffraction patterns of a magnetic Gd 5Si 2Ge 2nanocrystal with left- and right-circularly polarized X-rays. Future applications of dichroic Bragg coherent diffractive imaging for the correlation of strain and lattice defects with magnetic ordering and inhomogeneities are considered.« less

New developments in the Paris-Edinburgh cell program at HPCAT

NASA Astrophysics Data System (ADS)

Park, C.; Kenney-Benson, C.; Kono, Y.; Shen, G.; Yu, T.; Sakamaki, T.; Jing, Z.; Wang, Y.; Abd El Qader, M.; Baker, J.; Kumar, R.; Velisavljevic, N.

2011-12-01

The Paris-Edinburgh cell at HPCAT 16BM-B station is capable of maintaining sample pressure and temperature up to 7GPa and 2,300K for long durations more than 24 hrs for various types of materials in the molten state. Materials including rock forming minerals, metal alloys, semiconductors, and energetic organic compounds have been studied for their liquid structures and phase transition behaviors under these conditions. The sample volume ranges from 0.03 mm3 to 1.2 mm3 by adjusting the cylindrical sample diameter depending on x-ray attenuation, while the sample height available for x-ray scattering is limited to 0.4 mm due to the gap between the two co-axial WC anvils. The sample cell assembly has been optimized for x-ray transparency, chemical inertness, and thermal insulation using boron-epoxy composite gasket, hexagonal boron nitride or graphite crucible, and low density magnesia supporting the cylindrical graphite heater. For consistent measurements of liquid/amorphous and crystalline structures during melting and phase transitions, the energy-dispersive x-ray diffraction (EDXD) with multiple 2θ angles is applied, fully exploiting the bending magnet white beam spectrum provided by the Advanced Photon Source up to 120 keV energy. Fine collimation slits are applied for the diffracted beam to control the depth resolution at various diffraction angles and to minimize background scattering from the pressure media. A real-time radiography imaging system is also statically installed at the beamline for sample alignment and 2D projection volumetry applications. This combined setup is established as the routine PEC application at the station. Recently, a few new capabilities have been added: Ultrasonic velocity measurement for liquid samples having a disc shape (0.2-0.4 mm in thickness) has been successfully commissioned with the help of the radiography imaging system, which calibrates the acoustic travel distances through the sample cell assembly within 5 μm uncertainty. The white beam radiography also has been utilized in an in-situ thermoelectric property measurement for high-pressure solid phase. Electrical resistivity, thermoelectric coefficient (Seebeck coefficient), and thermal conductivity of solid phases can be simultaneously measured with a four-probe approach using inserted thermocouple wires. These new applications were made through substantial modifications of the sample assembly components as well as adding in-situ probing electrodes in- and outside of the PE anvils. These series of new instrumental developments at HPCAT opened new opportunities for in-situ studies of structure and property correlations for melts. New developments to extend the pressure and temperature capabilities while retaining the outstanding stability of the sample in molten state are ongoing.