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

[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.

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.

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.

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.

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

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.

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.

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.

A study of X-ray multiple diffraction by means of section topography.

PubMed

Kohn, V G; Smirnova, I A

2015-09-01

The results of theoretical and experimental study are presented for the question of how the X-ray multiple diffraction in a silicon single crystal influences the interference fringes of section topography for the 400 reflection in the Laue case. Two different cases of multiple diffraction are discovered for zero and very small values of the azimuthal angle for the sample in the form of a plate with the surface normal to the 001 direction. The cases are seen on the same topogram without rotation of the crystal. Accurate computer simulations of the section topogram for the case of X-ray multiple diffraction are performed for the first time. It is shown that the structure of interference fringes on the section topogram in the region of multiple diffraction becomes more complicated. It has a very sharp dependence on the azimuthal angle. The experiment is carried out using a laboratory source under conditions of low resolution over the azimuthal angle. Nevertheless, the characteristic inclination of the interference fringes on the tails of the multiple diffraction region is easily seen. This phenomenon corresponds completely to the computer simulations.

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.

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

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

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

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.

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.

X-ray diffraction gratings: Precise control of ultra-low blaze angle via anisotropic wet etching

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

Voronov, Dmitriy L.; Naulleau, Patrick; Gullikson, Eric M.

2016-07-25

Diffraction gratings are used from micron to nanometer wavelengths as dispersing elements in optical instruments. At shorter wavelengths, crystals can be used as diffracting elements, but due to the 3D nature of the interaction with light are wavelength selective rather than wavelength dispersing. There is an urgent need to extend grating technology into the x-ray domain of wavelengths from 1 to 0.1 nm, but this requires the use of gratings that have a faceted surface in which the facet angles are very small, typically less than 1°. Small facet angles are also required in the extreme ultra-violet and soft x-ray energymore » ranges in free electron laser applications, in order to reduce power density below a critical damage threshold. In this work, we demonstrate a technique based on anisotropic etching of silicon designed to produce very small angle facets with a high degree of perfection.« 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.

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.

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.

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.

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.

The measurement capabilities of cross-sectional profile of Nanoimprint template pattern using small angle x-ray scattering

NASA Astrophysics Data System (ADS)

Yamanaka, Eiji; Taniguchi, Rikiya; Itoh, Masamitsu; Omote, Kazuhiko; Ito, Yoshiyasu; Ogata, Kiyoshi; Hayashi, Naoya

2016-05-01

Nanoimprint lithography (NIL) is one of the most potential candidates for the next generation lithography for semiconductor. It will achieve the lithography with high resolution and low cost. High resolution of NIL will be determined by a high definition template. Nanoimprint lithography will faithfully transfer the pattern of NIL template to the wafer. Cross-sectional profile of the template pattern will greatly affect the resist profile on the wafer. Therefore, the management of the cross-sectional profile is essential. Grazing incidence small angle x-ray scattering (GI-SAXS) technique has been proposed as one of the method for measuring cross-sectional profile of periodic nanostructure pattern. Incident x-rays are irradiated to the sample surface with very low glancing angle. It is close to the critical angle of the total reflection of the x-ray. The scattered x-rays from the surface structure are detected on a two-dimensional detector. The observed intensity is discrete in the horizontal (2θ) direction. It is due to the periodicity of the structure, and diffraction is observed only when the diffraction condition is satisfied. In the vertical (β) direction, the diffraction intensity pattern shows interference fringes reflected to height and shape of the structure. Features of the measurement using x-ray are that the optical constant for the materials are well known, and it is possible to calculate a specific diffraction intensity pattern based on a certain model of the cross-sectional profile. The surface structure is estimated by to collate the calculated diffraction intensity pattern that sequentially while changing the model parameters with the measured diffraction intensity pattern. Furthermore, GI-SAXS technique can be measured an object in a non-destructive. It suggests the potential to be an effective tool for product quality assurance. We have developed a cross-sectional profile measurement of quartz template pattern using GI-SAXS technique. In this report, we will report the measurement capabilities of GI-SAXS technique as a cross-sectional profile measurement tool of NIL quartz template pattern.

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

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.

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.

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).

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.

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.

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.

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.

Accurate small and wide angle x-ray scattering profiles from atomic models of proteins and nucleic acids

NASA Astrophysics Data System (ADS)

Nguyen, Hung T.; Pabit, Suzette A.; Meisburger, Steve P.; Pollack, Lois; Case, David A.

2014-12-01

A new method is introduced to compute X-ray solution scattering profiles from atomic models of macromolecules. The three-dimensional version of the Reference Interaction Site Model (RISM) from liquid-state statistical mechanics is employed to compute the solvent distribution around the solute, including both water and ions. X-ray scattering profiles are computed from this distribution together with the solute geometry. We describe an efficient procedure for performing this calculation employing a Lebedev grid for the angular averaging. The intensity profiles (which involve no adjustable parameters) match experiment and molecular dynamics simulations up to wide angle for two proteins (lysozyme and myoglobin) in water, as well as the small-angle profiles for a dozen biomolecules taken from the BioIsis.net database. The RISM model is especially well-suited for studies of nucleic acids in salt solution. Use of fiber-diffraction models for the structure of duplex DNA in solution yields close agreement with the observed scattering profiles in both the small and wide angle scattering (SAXS and WAXS) regimes. In addition, computed profiles of anomalous SAXS signals (for Rb+ and Sr2+) emphasize the ionic contribution to scattering and are in reasonable agreement with experiment. In cases where an absolute calibration of the experimental data at q = 0 is available, one can extract a count of the excess number of waters and ions; computed values depend on the closure that is assumed in the solution of the Ornstein-Zernike equations, with results from the Kovalenko-Hirata closure being closest to experiment for the cases studied here.

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°.

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

Correct interpretation of diffraction properties of quartz crystals for X-ray optics applications

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

Huang, Xian-Rong; Gog, Thomas; Kim, Jungho

Quartz has hundreds of strong Bragg reflections that may offer a great number of choices for making fixed-angle X-ray analyzers and polarizers at virtually any hard X-ray energies with selectable resolution. However, quartz crystals, unlike silicon and germanium, are chiral and may thus appear in two different forms of handedness that are mirror images. Furthermore, because of the threefold rotational symmetry along thecaxis, the {h 1h 2h 3L} and {h 2h 1h 3L} Bragg reflections may have quite different Darwin bandwidth, reflectivity and angular acceptance, although they have the same Bragg angle. The design of X-ray optics from quartz crystalsmore » therefore requires unambiguous determination of the orientation, handedness and polarity of the crystals. The Laue method and single-axis diffraction technique can provide such information, but the variety of conventions used in the literature to describe quartz structures has caused widespread confusion. The current studies give detailed guidelines for design and fabrication of quartz X-ray optics, with special emphasis on the correct interpretation of Laue patterns in terms of the crystallography and diffraction properties of quartz. Meanwhile, the quartz crystals examined were confirmed by X-ray topography to have acceptably low densities of dislocations and other defects, which is the foundation for developing high-resolution quartz-based X-ray optics.« less

Use of a miniature diamond-anvil cell in high-pressure single-crystal neutron Laue diffraction

PubMed Central

Binns, Jack; Kamenev, Konstantin V.; McIntyre, Garry J.; Moggach, Stephen A.; Parsons, Simon

2016-01-01

The first high-pressure neutron diffraction study in a miniature diamond-anvil cell of a single crystal of size typical for X-ray diffraction is reported. This is made possible by modern Laue diffraction using a large solid-angle image-plate detector. An unexpected finding is that even reflections whose diffracted beams pass through the cell body are reliably observed, albeit with some attenuation. The cell body does limit the range of usable incident angles, but the crystallographic completeness for a high-symmetry unit cell is only slightly less than for a data collection without the cell. Data collections for two sizes of hexamine single crystals, with and without the pressure cell, and at 300 and 150 K, show that sample size and temperature are the most important factors that influence data quality. Despite the smaller crystal size and dominant parasitic scattering from the diamond-anvil cell, the data collected allow a full anisotropic refinement of hexamine with bond lengths and angles that agree with literature data within experimental error. This technique is shown to be suitable for low-symmetry crystals, and in these cases the transmission of diffracted beams through the cell body results in much higher completeness values than are possible with X-rays. The way is now open for joint X-ray and neutron studies on the same sample under identical conditions. PMID:27158503

Tunable hard X-ray spectrometer utilizing asymmetric planes of a quartz transmission crystal

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

Seely, John F., E-mail: seelyjf@gmail.com; Feldman, Uri; Henins, Albert

2016-05-15

A Cauchois type hard x-ray spectrometer was developed that utilizes the (301) diffraction planes at an asymmetric angle of 23.51° to the normal to the surface of a cylindrically curved quartz transmission crystal. The energy coverage is tunable by rotating the crystal and the detector arm, and spectra were recorded in the 8 keV to 20 keV range with greater than 2000 resolving power. The high resolution results from low aberrations enabled by the nearly perpendicular angle of the diffracted rays with the back surface of the crystal. By using other asymmetric planes of the same crystal and rotating tomore » selected angles, the spectrometer can operate with high resolution up to 50 keV.« less

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

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

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.

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.

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

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

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.

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.

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.

Fabrication of high-resolution x-ray diffractive optics at King's College London

NASA Astrophysics Data System (ADS)

Charalambous, Pambos S.; Anastasi, Peter A. F.; Burge, Ronald E.; Popova, Katia

1995-09-01

The fabrication of high resolution x-ray diffractive optics, and Fresnel zone plates (ZPs) in particular, is a very demanding multifaceted technological task. The commissioning of more (and brighter) synchrotron radiation sources, has increased the number of x-ray imaging beam lines world wide. The availability of cheaper and more effective laboratory x-ray sources, has further increased the number of laboratories involved in x-ray imaging. The result is an ever increasing demand for x-ray optics with a very wide range of specifications, reflecting the particular type of x-ray imaging performed at different laboratories. We have been involved in all aspects of high resolution nanofabrication for a number of years, and we have explored many different methods of lithography, which, although unorthodox, open up possibilities, and increase our flexibility for the fabrication of different diffractive optical elements, as well as other types of nanostructures. The availability of brighter x-ray sources, means that the diffraction efficiency of the ZPs is becoming of secondary importance, a trend which will continue in the future. Resolution, however, is important and will always remain so. Resolution is directly related to the accuracy af pattern generation, as well as the ability to draw fine lines. This is the area towards which we have directed most of our efforts so far.

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.

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

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

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.

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.

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.

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.

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.

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.

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.

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.

Periodic order and defects in Ni-based inverse opal-like crystals on the mesoscopic and atomic scale

NASA Astrophysics Data System (ADS)

Chumakova, A. V.; Valkovskiy, G. A.; Mistonov, A. A.; Dyadkin, V. A.; Grigoryeva, N. A.; Sapoletova, N. A.; Napolskii, K. S.; Eliseev, A. A.; Petukhov, A. V.; Grigoriev, S. V.

2014-10-01

The structure of inverse opal crystals based on nickel was probed on the mesoscopic and atomic levels by a set of complementary techniques such as scanning electron microscopy and synchrotron microradian and wide-angle diffraction. The microradian diffraction revealed the mesoscopic-scale face-centered-cubic (fcc) ordering of spherical voids in the inverse opal-like structure with unit cell dimension of 750±10nm. The diffuse scattering data were used to map defects in the fcc structure as a function of the number of layers in the Ni inverse opal-like structure. The average lateral size of mesoscopic domains is found to be independent of the number of layers. 3D reconstruction of the reciprocal space for the inverse opal crystals with different thickness provided an indirect study of original opal templates in a depth-resolved way. The microstructure and thermal response of the framework of the porous inverse opal crystal was examined using wide-angle powder x-ray diffraction. This artificial porous structure is built from nickel crystallites possessing stacking faults and dislocations peculiar for the nickel thin films.

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.

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).

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

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.

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

Polyimides with carbonyl and ether connecting groups between the aromatic rings

NASA Technical Reports Server (NTRS)

Hergenrother, Paul M. (Inventor); Havens, Stephen J. (Inventor)

1992-01-01

New polyimides have been prepared from the reaction of aromatic dianhydrides with novel aromatic diamines containing carbonyl and ether connecting groups between the aromatic rings. Several of these polyimides are shown to be semi-crystalline as evidenced by wide angle x ray diffraction and differential scanning calorimetry. Most of the polyimides form tough solvent resistant films with high tensile properties. Several of these materials can be thermally processed to form solvent and base resistant moldings.

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

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.

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)

Synthesis and structural characterization of ZnO and CuO nanoparticles supported mesoporous silica SBA-15

NASA Astrophysics Data System (ADS)

El-Nahhal, Issa M.; Salem, Jamil K.; Selmane, Mohamed; Kodeh, Fawzi S.; Ebtihan, Heba A.

2017-01-01

Zinc oxide (ZnO) and copper oxide (CuO) nanoparticles were loaded into mesoporous silica SBA-15 by post-synthesis and direct methods. The structural properties were characterized using wide and small angle X-ray diffraction (WXRD & SXRD), X-ray photoelectron spectroscopy (XPS) and N2-adsorption desorption (BET). The WXRD showed that, the loaded zinc and copper oxides were present in crystalline forms (impregnation). The mesoporosity properties of SBA-15 silica were well maintained even after the introduction of metal oxide nanoparticles. BET analysis indicate that the impregnated and condensed ZnO and CuO supported SBA-15 nanocomposites have a lower surface area than that of its parent SBA-15.

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.

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.

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.

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.

X-ray diffraction study of the caged magnetic compound DyFe 2 Zn 20 at low temperatures

NASA Astrophysics Data System (ADS)

Ohashi, M.; Ohashi, K.; Sawabu, M.; Miyagawa, M.; Maeta, K.; Isikawa, Y.

2018-05-01

We have carried out high-angle X-ray powder diffraction measurements of the caged magnetic compound DyFe2Zn20 at low temperature between 14 and 300 K. Even though a strong magnetic anisotropy exists in the magnetization and magnetic susceptibility due to strong exchange interaction between Fe and Dy, almost all X-ray powder diffraction peaks correspond to Bragg reflections of the cubic structural models not only at room temperature paramagnetic state but also at low temperature magnetic ordering state. The Debye temperature is obtained to be 227 K from the results of the volumetric thermal expansion coefficient, which is approximately coincident with that of CeRu2Zn20 (245 K) and that of pure Zn metal (235 K).

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.

Interaction of dipalmitoyl phosphatidylcholine (DPPC) liposomes and insulin

NASA Astrophysics Data System (ADS)

Mady, Mohsen M.; Elshemey, Wael M.

2011-06-01

Insulin, a peptide that has been used for decades in the treatment of diabetes, has well-defined properties and delivery requirements. Liposomes, which are lipid bilayer vesicles, have gained increasing attention as drug carriers which reduce the toxicity and increase the pharmacological activity of various drugs. The molecular interaction between (uncharged lipid) dipalmitoyl phosphatidylcholine (DPPC) liposomes and insulin has been characterized by using Fourier transform infrared spectroscopy (FTIR) and X-ray diffraction. The characteristic protein absorption band peaks, Amide I (at about 1660 cm-1) and Amide II band (at about 1546 cm-1) are potentially reduced in the liposome insulin complex. Wide-angle x-ray scattering measurements showed that the association of insulin with DPPC lipid of liposomes still maintains the characteristic DPPC diffraction peaks with almost no change in relative intensities or change in peak positions. The absence of any shift in protein peak positions after insulin being associated with DPPC liposomes indicates that insulin is successfully forming complex with DPPC liposomes with possibly no pronounced alterations in the structure of insulin molecule.

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.

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.

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

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)).

Monitoring the recrystallisation of amorphous xylitol using Raman spectroscopy and wide-angle X-ray scattering.

PubMed

Palomäki, Emmi; Ahvenainen, Patrik; Ehlers, Henrik; Svedström, Kirsi; Huotari, Simo; Yliruusi, Jouko

2016-07-11

In this paper we present a fast model system for monitoring the recrystallization of quench-cooled amorphous xylitol using Raman spectroscopy and wide-angle X-ray scattering. The use of these two methods enables comparison between surface and bulk crystallization. Non-ordered mesoporous silica micro-particles were added to the system in order to alter the rate of crystallization of the amorphous xylitol. Raman measurements showed that adding silica to the system increased the rate of surface crystallization, while X-ray measurements showed that the rate of bulk crystallization decreased. Using this model system it is possible to measure fast changes, which occur in minutes or within a few hours. Raman-spectroscopy and wide-angle X-ray scattering were found to be complementary techniques when assessing surface and bulk crystallization of amorphous xylitol. Copyright © 2016 Elsevier B.V. All rights reserved.

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.

An instrument for in situ coherent x-ray studies of metal-organic vapor phase epitaxy of III-nitrides.

PubMed

Ju, Guangxu; Highland, Matthew J; Yanguas-Gil, Angel; Thompson, Carol; Eastman, Jeffrey A; Zhou, Hua; Brennan, Sean M; Stephenson, G Brian; Fuoss, Paul H

2017-03-01

We describe an instrument that exploits the ongoing revolution in synchrotron sources, optics, and detectors to enable in situ studies of metal-organic vapor phase epitaxy (MOVPE) growth of III-nitride materials using coherent x-ray methods. The system includes high-resolution positioning of the sample and detector including full rotations, an x-ray transparent chamber wall for incident and diffracted beam access over a wide angular range, and minimal thermal sample motion, giving the sub-micron positional stability and reproducibility needed for coherent x-ray studies. The instrument enables surface x-ray photon correlation spectroscopy, microbeam diffraction, and coherent diffraction imaging of atomic-scale surface and film structure and dynamics during growth, to provide fundamental understanding of MOVPE processes.

An instrument for in situ coherent x-ray studies of metal-organic vapor phase epitaxy of III-nitrides

NASA Astrophysics Data System (ADS)

Ju, Guangxu; Highland, Matthew J.; Yanguas-Gil, Angel; Thompson, Carol; Eastman, Jeffrey A.; Zhou, Hua; Brennan, Sean M.; Stephenson, G. Brian; Fuoss, Paul H.

2017-03-01

We describe an instrument that exploits the ongoing revolution in synchrotron sources, optics, and detectors to enable in situ studies of metal-organic vapor phase epitaxy (MOVPE) growth of III-nitride materials using coherent x-ray methods. The system includes high-resolution positioning of the sample and detector including full rotations, an x-ray transparent chamber wall for incident and diffracted beam access over a wide angular range, and minimal thermal sample motion, giving the sub-micron positional stability and reproducibility needed for coherent x-ray studies. The instrument enables surface x-ray photon correlation spectroscopy, microbeam diffraction, and coherent diffraction imaging of atomic-scale surface and film structure and dynamics during growth, to provide fundamental understanding of MOVPE processes.

Modification of carbon nanotubes with fluorinated ionic liquid for improving processability of fluoro-ethylene-propylene

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

Ma, Hongyang; Chu, Benjamin; Hsiao, Benjamin S.

Fluorinated ionic liquid (F-IL), 1-(3-perfluorooctylpropyl)-3-methylimidazolium bis(perfluoroethylsufonyl)amine, had been successfully prepared and employed to modify multi-wall carbon nanotubes (MWCNTs) for improving the processability of fluoro-ethylene-propylene (FEP). The thermally decomposed temperature of F-IL was higher than 350 °C measured by thermal gravimetric analysis (TGA) which indicated that the fluorinated ionic liquid could be suitable for melting blend with FEP (blending at 290 °C) by a twin-screw extruder. Through “cation-π” interaction between the imidazolium cation of F-IL and the graphene surface of MWCNTs, MWCNTs can be modified with F-IL and used as nanofillers to improve the dispersity of MWCNTs in fluorocopolymer FEP verifiedmore » by SEM images of the FEP nanocomposite. The structural characterization and mechanical property of FEP nanocomposite during the deformation were investigated by tensile experiments and simultaneous time-resolved wide-angle X-ray diffraction (WAXD) and small-angle X-ray scattering (SAXS) techniques.« less

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.

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

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.

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.

Mechanical properties and XRD of Nafion modified by 2-hydroxyethylammonium ionic liquids

NASA Astrophysics Data System (ADS)

Garaev, V.; Pavlovica, S.; Reinholds, I.; Vaivars, G.

2013-12-01

In this work, the Nafion 112 membrane impregnated with 2-hydroxyethylammonium carboxylate ionic liquids have been investigated. The used ionic liquids were 2-hydroxyethylammonium formate [HEA]F, acetate [HEA]A and lactate [HEA]L. Prepared composite membranes Nafion/ionic liquid are characterized by mechanical testing, such as tensile test and creep test. It is found that ionic liquids decrease elastic modulus and creep compliance, but do not have significant effect on the tensile strength. Also, composite membranes were studied by wide angle X-ray diffraction. All ionic liquids shift the peak maximum to the lower angle. In this work, only biodegradable ionic liquids were used for composite preparation.

An instrument for in situ coherent x-ray studies of metal-organic vapor phase epitaxy of III-nitrides

DOE PAGES

Ju, Guangxu; Highland, Matthew J.; Yanguas-Gil, Angel; ...

2017-03-21

Here, we describe an instrument that exploits the ongoing revolution in synchrotron sources, optics, and detectors to enable in situ studies of metal-organic vapor phase epitaxy (MOVPE) growth of III-nitride materials using coherent x-ray methods. The system includes high-resolution positioning of the sample and detector including full rotations, an x-ray transparent chamber wall for incident and diffracted beam access over a wide angular range, and minimal thermal sample motion, giving the sub-micron positional stability and reproducibility needed for coherent x-ray studies. The instrument enables surface x-ray photon correlation spectroscopy, microbeam diffraction, and coherent diffraction imaging of atomic-scale surface and filmmore » structure and dynamics during growth, to provide fundamental understanding of MOVPE processes.« less

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.

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

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.

New poly(butylene succinate)/layered silicate nanocomposites: preparation and mechanical properties.

PubMed

Ray, Suprakas Sinha; Okamoto, Kazuaki; Maiti, Pralay; Okamoto, Masami

2002-04-01

New poly(butylene succinate) (PBS)/layered silicate nanocomposites have been successfully prepared by simple melt extrusion of PBS and octadecylammonium modified montmorillonite (C18-mmt) at 150 degrees C. The d-spacing of both C18-mmt and intercalated nanocomposites was investigated by wide-angle X-ray diffraction analysis. Bright-field transmission electron microscopic study showed several stacked silicate layers with random orientation in the PBS matrix. The intercalated nanocomposites exhibited remarkable improvement of mechanical properties in both solid and melt states as compared with that of PBS matrix without clay.

Structural studies of liquid Co–Sn alloys

PubMed Central

Yakymovych, A.; Shtablavyi, I.; Mudry, S.

2014-01-01

An analysis of the structure features of liquid Co–Sn alloys has been performed by means of X-ray diffraction method, viscosity coefficient analysis and computer simulation method. The X-ray diffraction investigations were carried out over a wide concentration range at the temperature 1473 K. It was found that the structure of these alloys can be described in the frame of independent X-ray scattering model. The viscosity coefficient was calculated by an excess entropy scaling and compared with experimental data. PMID:25328282

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

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

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

Environmentally induced chemical and morphological heterogeneity of zinc oxide thin films

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

Jiang, Hua; Chou, Kang Wei; Petrash, Stanislas

Zinc oxide (ZnO) thin films have been reported to suffer from degradation in electrical properties, when exposed to elevated heat and humidity, often leading to failures of electronic devices containing ZnO films. This degradation appears to be linked to water and oxygen penetration into the ZnO film. However, a direct observation in the ZnO film morphological evolution detailing structural and chemical changes has been lacking. Here, we systematically investigated the chemical and morphological heterogeneities of ZnO thin films caused by elevated heat and humidity, simulating an environmental aging. X-ray fluorescence microscopy, X-ray absorption spectroscopy, grazing incidence small angle and widemore » angle X-ray scattering, scanning electron microscopy (SEM), ultra-high-resolution SEM, and optical microscopy were carried out to examine ZnO and Al-doped ZnO thin films on two different substrates—silicon wafers and flexible polyethylene terephthalate (PET) films. In the un-doped ZnO thin film, the simulated environmental aging is resulting in pin-holes. In the Al-doped ZnO thin films, significant morphological changes occurred after the treatment, with an appearance of platelet-shaped structures that are 100–200 nm wide by 1 μm long. Synchrotron x-ray characterization further confirmed the heterogeneity in the aged Al-doped ZnO, showing the formation of anisotropic structures and disordering. X-ray diffraction and X-ray absorption spectroscopy indicated the formation of a zinc hydroxide in the aged Al-doped films. Utilizing advanced characterization methods, our studies provided information with an unprecedented level of details and revealed the chemical and morphologically heterogeneous nature of the degradation in ZnO thin films.« less

Environmentally induced chemical and morphological heterogeneity of zinc oxide thin films

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

Jiang, Hua; Chou, Kang Wei; Petrash, Stanislas

Zinc oxide (ZnO) thin films have been reported to suffer from degradation in electrical properties, when exposed to elevated heat and humidity, often leading to failures of electronic devices containing ZnO films. This degradation appears to be linked to water and oxygen penetration into the ZnO film. However, a direct observation in the ZnO film morphological evolution detailing structural and chemical changes has been lacking. Here, we systematically investigated the chemical and morphological heterogeneities of ZnO thin films caused by elevated heat and humidity, simulating an environmental aging. X-ray fluorescence microscopy, X-ray absorption spectroscopy, grazing incidence small angle and widemore » angle X-ray scattering, scanning electron microscopy (SEM), ultra-high-resolution SEM, and optical microscopy were carried out to examine ZnO and Al-doped ZnO thin films on two different substrates—silicon wafers and flexible polyethylene terephthalate (PET) films. In the un-doped ZnO thin film, the simulated environmental aging is resulting in pin-holes. In the Al-doped ZnO thin films, significant morphological changes occurred after the treatment, with an appearance of platelet-shaped structures that are 100–200 nm wide by 1μm long. Synchrotron x-ray characterization further confirmed the heterogeneity in the aged Al-doped ZnO, showing the formation of anisotropic structures and disordering. X-ray diffraction and X-ray absorption spectroscopy indicated the formation of a zinc hydroxide in the aged Al-doped films. In conclusion, utilizing advanced characterization methods, our studies provided information with an unprecedented level of details and revealed the chemical and morphologically heterogeneous nature of the degradation in ZnO thin films.« less

Environmentally induced chemical and morphological heterogeneity of zinc oxide thin films

DOE PAGES

Jiang, Hua; Chou, Kang Wei; Petrash, Stanislas; ...

2016-09-02

Zinc oxide (ZnO) thin films have been reported to suffer from degradation in electrical properties, when exposed to elevated heat and humidity, often leading to failures of electronic devices containing ZnO films. This degradation appears to be linked to water and oxygen penetration into the ZnO film. However, a direct observation in the ZnO film morphological evolution detailing structural and chemical changes has been lacking. Here, we systematically investigated the chemical and morphological heterogeneities of ZnO thin films caused by elevated heat and humidity, simulating an environmental aging. X-ray fluorescence microscopy, X-ray absorption spectroscopy, grazing incidence small angle and widemore » angle X-ray scattering, scanning electron microscopy (SEM), ultra-high-resolution SEM, and optical microscopy were carried out to examine ZnO and Al-doped ZnO thin films on two different substrates—silicon wafers and flexible polyethylene terephthalate (PET) films. In the un-doped ZnO thin film, the simulated environmental aging is resulting in pin-holes. In the Al-doped ZnO thin films, significant morphological changes occurred after the treatment, with an appearance of platelet-shaped structures that are 100–200 nm wide by 1μm long. Synchrotron x-ray characterization further confirmed the heterogeneity in the aged Al-doped ZnO, showing the formation of anisotropic structures and disordering. X-ray diffraction and X-ray absorption spectroscopy indicated the formation of a zinc hydroxide in the aged Al-doped films. In conclusion, utilizing advanced characterization methods, our studies provided information with an unprecedented level of details and revealed the chemical and morphologically heterogeneous nature of the degradation in ZnO thin films.« less

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

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 and synchrotron methods in studies of cultural heritage sites

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

Koval’chuk, M. V.; Yatsishina, E. B.; Blagov, A. E.

2016-09-15

X-ray and synchrotron methods that are most widely used in studies of cultural heritage objects (including archaeological sites)—X-ray diffraction analysis, X-ray spectroscopy, and visualization techniques— have been considered. The reported examples show high efficiency and informativeness of natural science studies when solving most diverse problems of archaeology, history, the study of art, museology, etc.

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.

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

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.

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.

First centenary of Röntgen's discovery of X-rays

NASA Astrophysics Data System (ADS)

Valkovic, V.

1996-04-01

Usually it takes a decade or even several decades, from a discovery to its practical applications. This was not the case with X-rays; they were widely applied in medical and industrial radiography within a year of their discovery in 1895 by W.C. Röntgen. Today, X-ray analysis covers a wide range of techniques and fields of applications: from deduction of atomic arrangements by observation of diffraction phenomena to measurements of trace element concentration levels, distributions and maps by measuring fluorescence, X-ray attenuation or scattering. Although the contribution of analytical applications of X-rays to the present knowledge is difficult to surpass, modern application cover a wide range of activities from three-dimensional microfabrication using synchroton radiation to collecting information from the deep space by X-ray astronomy.

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.

Combined X-ray and neutron fibre diffraction studies of biological and synthetic polymers

NASA Astrophysics Data System (ADS)

Parrot, I. M.; Urban, V.; Gardner, K. H.; Forsyth, V. T.

2005-08-01

The fibrous state is a natural one for polymer molecules which tend to assume regular helical conformations rather than the globular structures characteristic of many proteins. Fibre diffraction therefore has broad application to the study of a wide range of biological and synthetic polymers. The purpose of this paper is to illustrate the general scope of the method and in particular to demonstrate the impact of a combined approach involving both X-ray and neutron diffraction methods. While the flux of modern X-ray synchrotron radiation sources allows high quality datasets to be recorded with good resolution within a very short space of time, neutron studies can provide unique information through the ability to locate hydrogen or deuterium atoms that are often difficult or impossible to locate using X-ray methods. Furthermore, neutron fibre diffraction methods can, through the ability to selectively label specific parts of a structure, be used to highlight novel aspects of polymer structure that can not be studied using X-rays. Two examples are given. The first describes X-ray and neutron diffraction studies of conformational transitions in DNA. The second describes structural studies of the synthetic high-performance polymer poly(p-phenylene terephthalamide) (PPTA), known commercially as Kevlar® or Twaron®.

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

Structural and optical properties of glancing angle deposited TiO2 nanowires array.

PubMed

Chinnamuthu, P; Mondal, A; Singh, N K; Dhar, J C; Das, S K; Chattopadhyay, K K

2012-08-01

TiO2 nanowires (NWs) have been synthesized by glancing angle deposition technique using e-beam evaporator. The average length 490 nm and diameter 80 nm of NWs were examined by field emission-scanning electron microscopy. Transmission electron microscopy emphasized that the NWs were widely dispersed at the top. X-ray diffraction has been carried out on the TiO2 thin film (TF) and NW array. A small blue shift of 0.03 eV was observed in Photoluminescence (PL) main band emission for TiO2 NW as compared to TiO2 TF. The high temperature annealing at 980 degrees C partially removed the oxygen vacancy from the sample, which was investigated by PL and optical absorption measurements.

DIFFRACTION FROM MODEL CRYSTALS

USDA-ARS?s Scientific Manuscript database

Although calculating X-ray diffraction patterns from atomic coordinates of a crystal structure is a widely available capability, calculation from non-periodic arrays of atoms has not been widely applied to cellulose. Non-periodic arrays result from modeling studies that, even though started with at...

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.

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.

Crystallographic Characterization of Extraterrestrial Materials by Energy-Scanning X-ray Diffraction

NASA Technical Reports Server (NTRS)

Hagiya, Kenji; Mikouchi, Takashi; Ohsumi, Kazumasa; Terada, Yasuko; Yagi, Naoto; Komatsu, Mutsumi; Yamaguchi, Shoki; Hirata, Arashi; Kurokawa, Ayaka; Zolensky, Michael E. (Principal Investigator)

2016-01-01

We have continued our long-term project using X-ray diffraction to characterize a wide range of extraterrestrial samples. The stationary sample method with polychromatic X-rays is advantageous because the irradiated area of the sample is always same and fixed, meaning that all diffraction spots occur from the same area of the sample, however, unit cell parameters cannot be directly obtained by this method though they are very important for identification of mineral and for determination of crystal structures. In order to obtain the cell parameters even in the case of the sample stationary method, we apply energy scanning of a micro-beam of monochromatic SR at SPring-8.

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

Superhydrophobic surfaces allow probing of exosome self organization using X-ray scattering

NASA Astrophysics Data System (ADS)

Accardo, Angelo; Tirinato, Luca; Altamura, Davide; Sibillano, Teresa; Giannini, Cinzia; Riekel, Christian; di Fabrizio, Enzo

2013-02-01

Drops of exosome dispersions from healthy epithelial colon cell line and colorectal cancer cells were dried on a superhydrophobic PMMA substrate. The residues were studied by small- and wide-angle X-ray scattering using both a synchrotron radiation micrometric beam and a high-flux table-top X-ray source. Structural differences between healthy and cancerous cells were detected in the lamellar lattices of the exosome macro-aggregates.Drops of exosome dispersions from healthy epithelial colon cell line and colorectal cancer cells were dried on a superhydrophobic PMMA substrate. The residues were studied by small- and wide-angle X-ray scattering using both a synchrotron radiation micrometric beam and a high-flux table-top X-ray source. Structural differences between healthy and cancerous cells were detected in the lamellar lattices of the exosome macro-aggregates. Electronic supplementary information (ESI) available. See DOI: 10.1039/c3nr34032e

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

Biodegradable composites with aligned hydroxyapatite nanoneedles.

PubMed

Sun, Shih-Po; Wei, Mei; Olson, James R; Shaw, Montgomery T

2012-10-01

We prepared an anisotropic bone graft composite to mimic the hierarchical structure of the natural bone in which aligned hydroxyapatite (HA) nanocrystals deposit along collagen fibers. To approach the modulus and strength of the bone, we incorporated synthesized HA nanoneedles and melt drawn poly(L-lactic acid) fibers in our composite as reinforcing components. Their preferred orientation was induced via a modified pultrusion process. The HA orientation distribution was examined using wide angle X-ray diffraction. Micromechanical Halpin-Tsai model predictions considering the amount, shape, and orientation distribution of HA were compared, favorably, with the experimental observations. Copyright © 2012 Wiley Periodicals, Inc.

Poly(vinyl acetate)/clay nanocomposite materials for organic thin film transistor application.

PubMed

Park, B J; Sung, J H; Park, J H; Choi, J S; Choi, H J

2008-05-01

Nanocomposite materials of poly(vinyl acetate) (PVAc) and organoclay were fabricated, in order to be utilized as dielectric materials of the organic thin film transistor (OTFT). Spin coating condition of the nanocomposite solution was examined considering shear viscosity of the composite materials dissolved in chloroform. Intercalated structure of the PVAc/clay nanocomposites was characterized using both wide-angle X-ray diffraction and TEM. Fracture morphology of the composite film on silicon wafer was also observed by SEM. Dielectric constant (4.15) of the nanocomposite materials shows that the PVAc/clay nanocomposites are applicable for the gate dielectric materials.

Polyamideimides containing carbonyl and ether connecting groups

NASA Technical Reports Server (NTRS)

Havens, S. J.; Hergenrother, P. M.

1990-01-01

Polyamidenimides were prepared from the reaction of trimellitic anhydride chloride with seven diamines containing carbonyl and ether groups between the aromatic rings. Several of these polyamideimides were semicrystalline as evidenced by wide-angle X-ray diffraction and differential scanning calorimetry. Glass transition temperatures ranged between 187 and 245 C, and crystalline transition temperatures ranged between 317 and 416 C. A series of copolyamideimides from a mixture of 1,3-bis(4-aminophenoxy 4-prime-benzoyl) benzene and 1,4-bis(4-aminophenoxy 4-prime-benzoyl)benzene were similarly prepared. These copolyamideimides were semicrystalline and formed tough, solvent resistant films with good tensile properties.

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.

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.

Oriented polyvinylidene fluoride–trifluoroethylene (P(VDF–TrFE)) films by Langmuir–Blodgett deposition: A synchrotron X-ray diffraction study

DOE PAGES

Lindemann, W. R.; Philiph, R. L.; Chan, D. W. W.; ...

2015-10-07

Langmuir–Blodgett films of polyvinylidene fluoride trifluoroethylene – P(VDF–TrFE)-copolymers possess substantially improved electrocaloric and pyroelectric properties, when compared with conventionally spin-cast films. In order to rationalize this, we prepared single-layered films of P(VDF–TrFE) (70:30) using both deposition techniques. Grazing incidence wide-angle X-ray scattering (GIWAXS), reveals that Langmuir–Blodgett deposited films have a higher concentration of the ferroelectric β-phase crystals, and that these films are highly oriented with respect to the substrate. Based on these observations, we suggest alternative means of deposition, which may substantially enhance the electrocaloric effect in P(VDF–TrFE) films. As a result, this development has significant implications for the potentialmore » use of P(VDF–TrFE) in solid-state refrigeration.« less

Chemistry of surface nanostructures in lead precursor-rich PbZr0.52Ti0.48O3 sol-gel films

NASA Astrophysics Data System (ADS)

Gueye, I.; Le Rhun, G.; Gergaud, P.; Renault, O.; Defay, E.; Barrett, N.

2016-02-01

We present a study of the chemistry of the nanostructured phase at the surface of lead zirconium titanate PbZr0.52Ti0.48O3 (PZT) films synthesized by sol-gel method. In sol-gel synthesis, excess lead precursor is used to maintain the target stoichiometry. Surface nanostructures appear at 10% excess whereas 30% excess inhibits their formation. Using the surface-sensitive, quantitative X-ray photoelectron spectroscopy and glancing angle X-ray diffraction we have shown that the chemical composition of the nanostructures is ZrO1.82-1.89 rather than pyrochlore often described in the literature. The presence of a possibly discontinuous layer of wide band gap ZrO1.82-1.89 could be of importance in determining the electrical properties of PZT-based metal-insulator-metal heterostructures.

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.

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.

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.

An upgrade beamline for combined wide, small and ultra small-angle x-ray scattering at the ESRF

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

Van Vaerenbergh, Pierre; Léonardon, Joachim; Sztucki, Michael

2016-07-27

This contribution presents the main design features of the upgraded beamline ID02 (TRUSAXS). The beamline combines different small-angle X-ray scattering techniques in one unique instrument. The key component of this instrument is an evacuated (5×10{sup −3} mbar) stainless steel detector tube of length 34 m and diameter 2 m. Three different detectors (Rayonix MX170, Pilatus 300 K and FReLoN 4M) are housed inside a motorized wagon which travels along a rail system with very low parasitic lateral movements (± 0.3 mm). This system allows automatically changing the sample-to-detector distance from about 1 m to 31 m and selecting the desiredmore » detector. In addition, a wide angle detector (Rayonix LX170) is installed just above the entrance cone of the tube for optional wide-angle X-ray scattering measurements. The beamstop system enables monitoring of the X-ray beam intensity in addition to blocking the primary beam, and automated insertion of selected masks behind the primary beamstop. The focusing optics and collimation system permit to cover a scattering vector (q) range of 0.002 nm{sup −1} ≤ q ≤ 50 nm{sup −1} with one unique setting using 0.1 nm X-ray wavelength for moderate flux (5×10{sup 12} photons/sec). However, for higher flux (6x10{sup 13} photons/sec) or higher resolution (minimum q < 0.001 nm{sup −1}), focusing and collimation, respectively need to be varied. For a sample-to-detector distance of 31 m and 0.1 nm wavelength, two dimensional ultra small-angle X-ray scattering patterns can be recorded down to q≈0.001 nm{sup −1} with far superior quality as compared to one dimensional profiles obtained with a Bonse-Hart instrument.« 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.

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.

Investigating the Defect Structures in Transparent Conducting Oxides Using X-ray and Neutron Scattering Techniques

PubMed Central

González, Gabriela B.

2012-01-01

Transparent conducting oxide (TCO) materials are implemented into a wide variety of commercial devices because they possess a unique combination of high optical transparency and high electrical conductivity. Created during the processing of the TCOs, defects within the atomic-scale structure are responsible for their desirable optical and electrical properties. Therefore, studying the defect structure is essential to a better understanding of the behavior of transparent conductors. X-ray and neutron scattering techniques are powerful tools to investigate the atomic lattice structural defects in these materials. This review paper presents some of the current developments in the study of structural defects in n-type TCOs using x-ray diffraction (XRD), neutron diffraction, extended x-ray absorption fine structure (EXAFS), pair distribution functions (PDFs), and x-ray fluorescence (XRF). PMID:28817010

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.

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.

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.

Probing polymer crystallization at processing-relevant cooling rates with synchrotron radiation

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

Cavallo, Dario, E-mail: Dario.cavallo@unige.it; Portale, Giuseppe; Androsch, René

2015-12-17

Processing of polymeric materials to produce any kind of goods, from films to complex objects, involves application of flow fields on the polymer melt, accompanied or followed by its rapid cooling. Typically, polymers solidify at cooling rates which span over a wide range, from a few to hundreds of °C/s. A novel method to probe polymer crystallization at processing-relevant cooling rates is proposed. Using a custom-built quenching device, thin polymer films are ballistically cooled from the melt at rates between approximately 10 and 200 °C/s. Thanks to highly brilliant synchrotron radiation and to state-of-the-art X-ray detectors, the crystallization process ismore » followed in real-time, recording about 20 wide angle X-ray diffraction patterns per second while monitoring the instantaneous sample temperature. The method is applied to a series of industrially relevant polymers, such as isotactic polypropylene, its copolymers and virgin and nucleated polyamide-6. Their crystallization behaviour during rapid cooling is discussed, with particular attention to the occurrence of polymorphism, which deeply impact material’s properties.« less

Improving packaged food quality and safety. Part 1: synchrotron X-ray analysis.

PubMed

López-Rubio, A; Hernandez-Muñoz, P; Catala, R; Gavara, R; Lagarón, J M

2005-10-01

The objective was to demonstrate, as an example of an application, the potential of synchrotron X-ray analysis to detect morphological alterations that can occur in barrier packaging materials and structures. These changes can affect the packaging barrier characteristics when conventional food preservation treatments are applied to packaged food. The paper presents the results of a number of experiments where time-resolved combined wide-angle X-ray scattering and small-angle X-ray scattering analysis as a function of temperature and humidity were applied to ethylene-vinyl alcohol co-polymers (EVOH), polypropylene (PP)/EVOH/PP structures, aliphatic polyketone terpolymer (PK) and amorphous polyamide (aPA) materials. A comparison between conventional retorting and high-pressure processing treatments in terms of morphologic alterations are also presented for EVOH. The impact of retorting on the EVOH structure contrasts with the good behaviour of the PK during this treatment and with that of aPA. However, no significant structural changes were observed by wide-angle X-ray scattering in the EVOH structures after high-pressure processing treatment. These structural observations have also been correlated with oxygen permeability measurements that are of importance when guaranteeing the intended levels of safety and quality of packaged food.

Influence of palmitic acid and hexadecanol on the phase transition temperature and molecular packing of dipalmitoylphosphatidyl-choline monolayers at the air-water interface

NASA Astrophysics Data System (ADS)

Lee, Ka Yee C.; Gopal, Ajaykumar; von Nahmen, Anja; Zasadzinski, Joseph A.; Majewski, Jaroslaw; Smith, Gregory S.; Howes, Paul B.; Kjaer, Kristian

2002-01-01

Palmitic acid (PA) and 1-hexadecanol (HD) strongly affect the phase transition temperature and molecular packing of dipalmitoylphosphatidylcholine (DPPC) monolayers at the air-water interface. The phase behavior and morphology of mixed DPPC/PA as well as DPPC/HD monolayers were determined by pressure-area-isotherms and fluorescence microscopy. The molecular organization was probed by synchrotron grazing incidence x-ray diffraction using a liquid surface diffractometer. Addition of PA or HD to DPPC monolayers increases the temperature of the liquid-expanded to condensed phase transition. X-ray diffraction shows that DPPC forms mixed crystals both with PA and HD over a wide range of mixing ratios. At a surface pressure (π) of 40 mN/m, increasing the amount of the single chain surfactant leads to a reduction in tilt angle of the aliphatic chains from nearly 30° for pure DPPC to almost 0° in a 1:1 molar ratio of DPPC and PA or HD. At this composition we also find closest packing of the aliphatic chains. Further increase of the amount of PA or HD does not change the lattice or the tilt.

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

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.

A modified Rayleigh-Gans-Debye formula for small angle X-ray scattering by interstellar dust grains

NASA Astrophysics Data System (ADS)

Sharma, Subodh K.

2015-05-01

A widely used approximation in studies relating to small angle differential scattering cross-section of X-rays scattered by interstellar dust grains is the well known Rayleigh-Gans-Debye approximation (RGDA). The validity of this approximation, however, is limited only to X-ray energies greater than about 1 keV. At lower energies, this approximation overestimates the exact results. In this paper a modification to the RGDA is suggested. It is shown that a combination of the RGDA with Ramsauer approximation retains the formal simplicity of the RGDA and also yields good agreement with Mie computations at all X-ray energies.

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.

Reconstructive colour X-ray diffraction imaging--a novel TEDDI imaging method.

PubMed

Lazzari, Olivier; Jacques, Simon; Sochi, Taha; Barnes, Paul

2009-09-01

Tomographic Energy-Dispersive Diffraction Imaging (TEDDI) enables a unique non-destructive mapping of the interior of bulk objects, exploiting the full range of X-ray signals (diffraction, fluorescence, scattering, background) recorded. By analogy to optical imaging, a wide variety of features (structure, composition, orientation, strain) dispersed in X-ray wavelengths can be extracted and colour-coded to aid interpretation. The ultimate aim of this approach is to realise real-time high-definition colour X-ray diffraction imaging, on the timescales of seconds, so that one will be able to 'look inside' optically opaque apparatus and unravel the space/time-evolution of the materials chemistry taking place. This will impact strongly on many fields of science but there are currently two barriers to this goal: speed of data acquisition (a 2D scan currently takes minutes to hours) and loss of image definition through spatial distortion of the X-ray sampling volume. Here we present a data-collection scenario and reconstruction routine which overcomes the latter barrier and which has been successfully applied to a phantom test object and to real materials systems such as a carbonating cement block. These procedures are immediately transferable to the promising technology of multi-energy-dispersive-detector-arrays which are planned to deliver the other breakthrough, that of one-two orders of magnitude improvement in data acquisition rates, that will be needed to realise real-time high-definition colour X-ray diffraction imaging.

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).

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.

NIST Standard Reference Material 3600: Absolute Intensity Calibration Standard for Small-Angle X-ray Scattering

DOE PAGES

Allen, Andrew J.; Zhang, Fan; Kline, R. Joseph; ...

2017-03-07

The certification of a new standard reference material for small-angle scattering [NIST Standard Reference Material (SRM) 3600: Absolute Intensity Calibration Standard for Small-Angle X-ray Scattering (SAXS)], based on glassy carbon, is presented. Creation of this SRM relies on the intrinsic primary calibration capabilities of the ultra-small-angle X-ray scattering technique. This article describes how the intensity calibration has been achieved and validated in the certified Q range, Q = 0.008–0.25 Å –1, together with the purpose, use and availability of the SRM. The intensity calibration afforded by this robust and stable SRM should be applicable universally to all SAXS instruments thatmore » employ a transmission measurement geometry, working with a wide range of X-ray energies or wavelengths. As a result, the validation of the SRM SAXS intensity calibration using small-angle neutron scattering (SANS) is discussed, together with the prospects for including SANS in a future renewal certification.« less

NIST Standard Reference Material 3600: Absolute Intensity Calibration Standard for Small-Angle X-ray Scattering

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

Allen, Andrew J.; Zhang, Fan; Kline, R. Joseph

The certification of a new standard reference material for small-angle scattering [NIST Standard Reference Material (SRM) 3600: Absolute Intensity Calibration Standard for Small-Angle X-ray Scattering (SAXS)], based on glassy carbon, is presented. Creation of this SRM relies on the intrinsic primary calibration capabilities of the ultra-small-angle X-ray scattering technique. This article describes how the intensity calibration has been achieved and validated in the certified Q range, Q = 0.008–0.25 Å –1, together with the purpose, use and availability of the SRM. The intensity calibration afforded by this robust and stable SRM should be applicable universally to all SAXS instruments thatmore » employ a transmission measurement geometry, working with a wide range of X-ray energies or wavelengths. As a result, the validation of the SRM SAXS intensity calibration using small-angle neutron scattering (SANS) is discussed, together with the prospects for including SANS in a future renewal certification.« less

NIST Standard Reference Material 3600: Absolute Intensity Calibration Standard for Small-Angle X-ray Scattering.

PubMed

Allen, Andrew J; Zhang, Fan; Kline, R Joseph; Guthrie, William F; Ilavsky, Jan

2017-04-01

The certification of a new standard reference material for small-angle scattering [NIST Standard Reference Material (SRM) 3600: Absolute Intensity Calibration Standard for Small-Angle X-ray Scattering (SAXS)], based on glassy carbon, is presented. Creation of this SRM relies on the intrinsic primary calibration capabilities of the ultra-small-angle X-ray scattering technique. This article describes how the intensity calibration has been achieved and validated in the certified Q range, Q = 0.008-0.25 Å -1 , together with the purpose, use and availability of the SRM. The intensity calibration afforded by this robust and stable SRM should be applicable universally to all SAXS instruments that employ a transmission measurement geometry, working with a wide range of X-ray energies or wavelengths. The validation of the SRM SAXS intensity calibration using small-angle neutron scattering (SANS) is discussed, together with the prospects for including SANS in a future renewal certification.

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.

Angular correlations of photons from solution diffraction at a free-electron laser encode molecular structure

DOE PAGES

Mendez, Derek; Watkins, Herschel; Qiao, Shenglan; ...

2016-09-26

During X-ray exposure of a molecular solution, photons scattered from the same molecule are correlated. If molecular motion is insignificant during exposure, then differences in momentum transfer between correlated photons are direct measurements of the molecular structure. In conventional small- and wide-angle solution scattering, photon correlations are ignored. This report presents advances in a new biomolecular structural analysis technique, correlated X-ray scattering (CXS), which uses angular intensity correlations to recover hidden structural details from molecules in solution. Due to its intense rapid pulses, an X-ray free electron laser (XFEL) is an excellent tool for CXS experiments. A protocol is outlinedmore » for analysis of a CXS data set comprising a total of half a million X-ray exposures of solutions of small gold nanoparticles recorded at the Spring-8 Ångström Compact XFEL facility (SACLA). From the scattered intensities and their correlations, two populations of nanoparticle domains within the solution are distinguished: small twinned, and large probably non-twinned domains. Finally, it is shown analytically how, in a solution measurement, twinning information is only accessible via intensity correlations, demonstrating how CXS reveals atomic-level information from a disordered solution of like molecules.« less

A Curved Image-Plate Detector System for High-Resolution Synchrotron X-ray Diffraction

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

Sarin, P.; Haggerty, R; Yoon, W

2009-01-01

The developed curved image plate (CIP) is a one-dimensional detector which simultaneously records high-resolution X-ray diffraction (XRD) patterns over a 38.7 2{theta} range. In addition, an on-site reader enables rapid extraction, transfer and storage of X-ray intensity information in {le}30 s, and further qualifies this detector to study kinetic processes in materials science. The CIP detector can detect and store X-ray intensity information linearly proportional to the incident photon flux over a dynamical range of about five orders of magnitude. The linearity and uniformity of the CIP detector response is not compromised in the unsaturated regions of the image plate,more » regardless of saturation in another region. The speed of XRD data acquisition together with excellent resolution afforded by the CIP detector is unique and opens up wide possibilities in materials research accessible through X-ray diffraction. This article presents details of the basic features, operation and performance of the CIP detector along with some examples of applications, including high-temperature XRD.« less

Simultaneous small- and wide-angle scattering at high X-ray energies.

PubMed

Daniels, J E; Pontoni, D; Hoo, Rui Ping; Honkimäki, V

2010-07-01

Combined small- and wide-angle X-ray scattering (SAXS/WAXS) is a powerful technique for the study of materials at length scales ranging from atomic/molecular sizes (a few angstroms) to the mesoscopic regime ( approximately 1 nm to approximately 1 microm). A set-up to apply this technique at high X-ray energies (E > 50 keV) has been developed. Hard X-rays permit the execution of at least three classes of investigations that are significantly more difficult to perform at standard X-ray energies (8-20 keV): (i) in situ strain analysis revealing anisotropic strain behaviour both at the atomic (WAXS) as well as at the mesoscopic (SAXS) length scales, (ii) acquisition of WAXS patterns to very large q (>20 A(-1)) thus allowing atomic pair distribution function analysis (SAXS/PDF) of micro- and nano-structured materials, and (iii) utilization of complex sample environments involving thick X-ray windows and/or samples that can be penetrated only by high-energy X-rays. Using the reported set-up a time resolution of approximately two seconds was demonstrated. It is planned to further improve this time resolution in the near future.

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

Zarkevich, Nikolai A; Johnson, Duane D

Nitinol (NiTi), the most widely used shape-memory alloy, exhibits an austenite phase that has yet to be identified. The usually assumed austenitic structure is cubic B2, which has imaginary phonon modes, hence it is unstable. We suggest a stable austenitic structure that “on average” has B2 symmetry (observed by x-ray and neutron diffraction), but it exhibits finite atomic displacements from the ideal B2 sites. The proposed structure has a phonon spectrum that agrees with that from neutron scattering, has diffraction spectra in agreement with x-ray diffraction, and has an energy relative to the ground state that agrees with calorimetry data.

Portable mini-chamber for temperature dependent studies using small angle and wide angle x-ray scattering

NASA Astrophysics Data System (ADS)

Dev, Arun Singh; Kumar, Dileep; Potdar, Satish; Pandit, Pallavi; Roth, Stephan V.; Gupta, Ajay

2018-04-01

The present work describes the design and performance of a vacuum compatible portable mini chamber for temperature dependent GISAXS and GIWAXS studies of thin films and multilayer structures. The water cooled body of the chamber allows sample annealing up to 900 K using ultra high vacuum compatible (UHV) pyrolytic boron nitride heater, thus making it possible to study the temperature dependent evolution of structure and morphology of two-dimensional nanostructured materials. Due to its light weight and small size, the chamber is portable and can be accommodated at synchrotron facilities worldwide. A systematic illustration of the versatility of the chamber has been demonstrated at beamline P03, PETRA-III, DESY, Hamburg, Germany. Temperature dependent grazing incidence small angle x-ray scattering (GISAXS) and grazing incidence wide angle x-ray scattering (GIWAXS) measurements were performed on oblique angle deposited Co/Ag multilayer structure, which jointly revealed that the surface diffusion in Co columns in Co/Ag multilayer enhances by increasing temperature from RT to ˜573 K. This results in a morphology change from columnar tilted structure to densely packed morphological isotropic multilayer.

Chiral betulin-imino-chitosan hydrogels by dynamic covalent sonochemistry.

PubMed

Iftime, Manuela Maria; Marin, Luminita

2018-07-01

A series of chiral hydrogels was prepared from a homogeneous mixture of chitosan and betulinic aldehyde in different molar ratios, under the effect of ultrasound. The hydrogelation mechanism has been investigated by FTIR and CD spectroscopy, wide angle X-ray diffraction and polarized light microscopy. The morphology of hydrogels was examined by SEM. The swelling ability has been tested in three media of different pH. It was concluded that hydrogelation occurred by different pathways, closely related to the peculiarities of the chitosan-betulin systems. Circular dichroism measurements revealed chiroptical properties of the hydrogels, correlated to their content and crosslinking pathway. Copyright © 2018 Elsevier B.V. All rights reserved.

High-pressure x-ray diffraction studies on the structure of liquid silicate using a Paris-Edinburgh type large volume press.

PubMed

Yamada, Akihiro; Wang, Yanbin; Inoue, Toru; Yang, Wenge; Park, Changyong; Yu, Tony; Shen, Guoyin

2011-01-01

An experimental setup for high-pressure liquid structure studies with synchrotron x-ray diffraction using the Paris-Edinburgh press has been installed at station 16-BM-B (HPCAT) of the Advanced Photon Source, Argonne National Laboratory. By collecting energy-dispersive data with a synchrotron white beam at various 2θ angles, the present device allows us to obtain the structure factor, S(Q), over a wide range of Q ( = 4πsinθ∕λ) owing to the excellent angular accessibility up to 37° in 2θ and high energy photons well beyond 100 keV. We have successfully collected XRD data on silicate (albite, NaAlSi(3)O(8)) liquids with Q up to ∼22 Å(-1) and pressure up to 5.3 GPa and temperature 1873 K, and obtained the radial distribution function, G(r), with a reasonable resolution. The T-O bond length (where T = Al, Si), which is a fundamental measure of local structure for aluminous silicate consisting of SiO(n) and AlO(n) polyhedra (tetrahedra at 1 atm condition), was found to be slightly shortened to 1.626 Å compared to that of glass at 1 atm. The T-O-T bound angle, which is the linkage of the above polyhedra, is the most responsible for densification. The T-O-T peak in G(r) splits into two peaks, suggesting a differentiation of the bond angle at high-pressure. The present technical development demonstrates that the Paris-Edinburgh press is suitable for studies of silicate liquids under high-pressure conditions.

Shape Recovery with Concomitant Mechanical Strengthening of Amphiphilic Shape Memory Polymers in Warm Water

DOE PAGES

Zhang, Ben; DeBartolo, Janae E.; Song, Jie

2017-01-26

Maintaining adequate or enhancing mechanical properties of shape memory polymers (SMPs) after shape recovery in an aqueous environment are greatly desired for biomedical applications of SMPs as self-fitting tissue scaffolds or minimally invasive surgical implants. Here we report stable temporary shape fixing and facile shape recovery of biodegradable triblock amphiphilic SMPs containing a poly(ethylene glycol) (PEG) center block and flanking poly(lactic acid) or poly(lactic-co-glycolic acid) blocks in warm water, accompanied with concomitant enhanced mechanical strengths. Differential scanning calorimetry (DSC), wide-angle X-ray diffraction (WXRD) and small-angle X-ray scattering (SAXS) analyses revealed that the unique stiffening of the amphiphilic SMPs upon hydrationmore » was due to hydration-driven microphase separation and PEG crystallization. We further demonstrated that the chemical composition of degradable blocks in these SMPs could be tailored to affect the persistence of hydration-induced stiffening upon subsequent dehydration. These properties combined open new horizons for these amphiphilic SMPs for smart weight-bearing in vivo applications (e.g. as self-fitting intervertebral discs). In conclusion, this study also provides a new material design strategy to strengthen polymers in aqueous environment in general.« less

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.

Correlation between protein sequence similarity and x-ray diffraction quality in the protein data bank.

PubMed

Lu, Hui-Meng; Yin, Da-Chuan; Ye, Ya-Jing; Luo, Hui-Min; Geng, Li-Qiang; Li, Hai-Sheng; Guo, Wei-Hong; Shang, Peng

2009-01-01

As the most widely utilized technique to determine the 3-dimensional structure of protein molecules, X-ray crystallography can provide structure of the highest resolution among the developed techniques. The resolution obtained via X-ray crystallography is known to be influenced by many factors, such as the crystal quality, diffraction techniques, and X-ray sources, etc. In this paper, the authors found that the protein sequence could also be one of the factors. We extracted information of the resolution and the sequence of proteins from the Protein Data Bank (PDB), classified the proteins into different clusters according to the sequence similarity, and statistically analyzed the relationship between the sequence similarity and the best resolution obtained. The results showed that there was a pronounced correlation between the sequence similarity and the obtained resolution. These results indicate that protein structure itself is one variable that may affect resolution when X-ray crystallography is used.

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).

Expression, crystallization and preliminary X-ray diffraction studies of recombinant Clostridium perfringens β2-toxin

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

Gurjar, Abhijit A.; Yennawar, Neela H.; Yennawar, Hemant P.

2007-06-01

The cloning, expression, purification and crystallization of recombinant Clostridium perfringens β2-toxin is described. The crystals diffracted to 2.9 Å resolution. Clostridium perfringens is a Gram-positive sporulating anaerobic bacterium that is responsible for a wide spectrum of diseases in animals, birds and humans. The virulence of C. perfringens is associated with the production of several enterotoxins and exotoxins. β2-toxin is a 28 kDa exotoxin produced by C. perfringens. It is implicated in necrotic enteritis in animals and humans, a disease characterized by a sudden acute onset with lethal hemorrhagic mucosal ulceration. The recombinant expression, purification and crystallization of β2-toxin using themore » batch-under-oil technique are reported here. Native X-ray diffraction data were obtained to 2.9 Å resolution on a synchrotron beamline at the F2 station at Cornell High Energy Synchrotron Source (CHESS) using an ADSC Quantum-210 CCD detector. The crystals belong to space group R3, with a dimer in the asymmetric unit; the unit-cell parameters are a = b = 103.71, c = 193.48 Å, α = β = 90, γ = 120° using the hexagonal axis setting. A self-rotation function shows that the two molecules are related by a noncrystallographic twofold axis with polar angles ω = 90.0, ϕ = 210.3°.« less

Wide-angle X-ray scattering study of heat-treated PEEK and PEEK composite

NASA Technical Reports Server (NTRS)

Cebe, Peggy; Lowry, Lynn; Chung, Shirley Y.; Yavrouian, Andre; Gupta, Amitava

1987-01-01

Samples of poly(etheretherketone) (PEEK) neat resin and APC-2 carbon fiber composite were subjected to various heat treatments, and the effect of quenching and annealing treatments was studied by wide-angle X-ray scattering. It is found that high-temperature treatments may introduce disorder into neat resin and composite PEEK when followed by rapid cooling. The disorder is metastable and can revert to ordered state when the material is heated above its glass transition temperature and then cooled slowly. The disorder may result from residual thermal stresses.

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.

On the Design of Wide-Field X-ray Telescopes

NASA Technical Reports Server (NTRS)

Elsner, Ronald F.; O'Dell, Stephen L.; Ramsey, Brian D.; Weiskopf, Martin C.

2009-01-01

X-ray telescopes having a relatively wide field-of-view and spatial resolution vs. polar off-axis angle curves much flatter than the parabolic dependence characteristic of Wolter I designs are of great interest for surveys of the X-ray sky and potentially for study of the Sun s X-ray emission. We discuss the various considerations affecting the design of such telescopes, including the possible use of polynomial mirror surface prescriptions, a method of optimizing the polynomial coefficients, scaling laws for mirror segment length vs. intersection radius, the loss of on-axis spatial resolution, and the positioning of focal plane detectors.

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.

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,...

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.

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

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.

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.

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.

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.

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.

A novel high-temperature furnace for combined in situ synchrotron X-ray diffraction and infrared thermal imaging to investigate the effects of thermal gradients upon the structure of ceramic materials

PubMed Central

Robinson, James B.; Brown, Leon D.; Jervis, Rhodri; Taiwo, Oluwadamilola O.; Millichamp, Jason; Mason, Thomas J.; Neville, Tobias P.; Eastwood, David S.; Reinhard, Christina; Lee, Peter D.; Brett, Daniel J. L.; Shearing, Paul R.

2014-01-01

A new technique combining in situ X-ray diffraction using synchrotron radiation and infrared thermal imaging is reported. The technique enables the application, generation and measurement of significant thermal gradients, and furthermore allows the direct spatial correlation of thermal and crystallographic measurements. The design and implementation of a novel furnace enabling the simultaneous thermal and X-ray measurements is described. The technique is expected to have wide applicability in material science and engineering; here it has been applied to the study of solid oxide fuel cells at high temperature. PMID:25178003

Single-crystal Raman spectroscopy and X-ray crystallography at beamline X26-C of the NSLS

PubMed Central

Stoner-Ma, Deborah; Skinner, John M.; Schneider, Dieter K.; Cowan, Matt; Sweet, Robert M.; Orville, Allen M.

2011-01-01

Three-dimensional structures derived from X-ray diffraction of protein crystals provide a wealth of information. Features and interactions important for the function of macromolecules can be deduced and catalytic mechanisms postulated. Still, many questions can remain, for example regarding metal oxidation states and the interpretation of ‘mystery density’, i.e. ambiguous or unknown features within the electron density maps, especially at ∼2 Å resolutions typical of most macromolecular structures. Beamline X26-C at the National Synchrotron Light Source (NSLS), Brookhaven National Laboratory (BNL), provides researchers with the opportunity to not only determine the atomic structure of their samples but also to explore the electronic and vibrational characteristics of the sample before, during and after X-ray diffraction data collection. When samples are maintained under cryo-conditions, an opportunity to promote and follow photochemical reactions in situ as a function of X-ray exposure is also provided. Plans are in place to further expand the capabilities at beamline X26-C and to develop beamlines at NSLS-II, currently under construction at BNL, which will provide users access to a wide array of complementary spectroscopic methods in addition to high-quality X-ray diffraction data. PMID:21169688

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

X-ray Studies of Regenerated Cellulose Fibers Wet Spun from Cotton Linter Pulp in NaOH/Thiourea Aqueous Solutions

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

Chen,X.; Burger, C.; Fang, D.

Regenerated cellulose fibers were fabricated by dissolution of cotton linter pulp in NaOH (9.5 wt%) and thiourea (4.5 wt%) aqueous solution followed by wet-spinning and multi-roller drawing. The multi-roller drawing process involved three stages: coagulation (I), coagulation (II) and post-treatment (III). The crystalline structure and morphology of regenerated cellulose fiber was investigated by synchrotron wide-angle X-ray diffraction (WAXD) and small-angle X-ray scattering (SAXS) techniques. Results indicated that only the cellulose II crystal structure was found in regenerated cellulose fibers, proving that the cellulose crystals were completely transformed from cellulose I to II structure during spinning from NaOH/thiourea aqueous solution. Themore » crystallinity, orientation and crystal size at each stage were determined from the WAXD analysis. Drawing of cellulose fibers in the coagulation (II) bath (H{sub 2}SO{sub 4}/H{sub 2}O) was found to generate higher orientation and crystallinity than drawing in the post-treatment (III). Although the post-treatment process also increased crystal orientation, it led to a decrease in crystallinity with notable reduction in the anisotropic fraction. Compared with commercial rayon fibers fabricated by the viscose process, the regenerated cellulose fibers exhibited higher crystallinity but lower crystal orientation. SAXS results revealed a clear scattering maximum along the meridian direction in all regenerated cellulose fibers, indicating the formation of lamellar structure during spinning.« less

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

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.

Powder X-ray diffraction laboratory, Reston, Virginia

USGS Publications Warehouse

Piatak, Nadine M.; Dulong, Frank T.; Jackson, John C.; Folger, Helen W.

2014-01-01

The powder x-ray diffraction (XRD) laboratory is managed jointly by the Eastern Mineral and Environmental Resources and Eastern Energy Resources Science Centers. Laboratory scientists collaborate on a wide variety of research problems involving other U.S. Geological Survey (USGS) science centers and government agencies, universities, and industry. Capabilities include identification and quantification of crystalline and amorphous phases, and crystallographic and atomic structure analysis for a wide variety of sample media. Customized laboratory procedures and analyses commonly are used to characterize non-routine samples including, but not limited to, organic and inorganic components in petroleum source rocks, ore and mine waste, clay minerals, and glassy phases. Procedures can be adapted to meet a variety of research objectives.

An instrument for in situ time-resolved X-ray imaging and diffraction of laser powder bed fusion additive manufacturing processes

NASA Astrophysics Data System (ADS)

Calta, Nicholas P.; Wang, Jenny; Kiss, Andrew M.; Martin, Aiden A.; Depond, Philip J.; Guss, Gabriel M.; Thampy, Vivek; Fong, Anthony Y.; Weker, Johanna Nelson; Stone, Kevin H.; Tassone, Christopher J.; Kramer, Matthew J.; Toney, Michael F.; Van Buuren, Anthony; Matthews, Manyalibo J.

2018-05-01

In situ X-ray-based measurements of the laser powder bed fusion (LPBF) additive manufacturing process produce unique data for model validation and improved process understanding. Synchrotron X-ray imaging and diffraction provide high resolution, bulk sensitive information with sufficient sampling rates to probe melt pool dynamics as well as phase and microstructure evolution. Here, we describe a laboratory-scale LPBF test bed designed to accommodate diffraction and imaging experiments at a synchrotron X-ray source during LPBF operation. We also present experimental results using Ti-6Al-4V, a widely used aerospace alloy, as a model system. Both imaging and diffraction experiments were carried out at the Stanford Synchrotron Radiation Lightsource. Melt pool dynamics were imaged at frame rates up to 4 kHz with a ˜1.1 μm effective pixel size and revealed the formation of keyhole pores along the melt track due to vapor recoil forces. Diffraction experiments at sampling rates of 1 kHz captured phase evolution and lattice contraction during the rapid cooling present in LPBF within a ˜50 × 100 μm area. We also discuss the utility of these measurements for model validation and process improvement.

An instrument for in situ time-resolved X-ray imaging and diffraction of laser powder bed fusion additive manufacturing processes.

PubMed

Calta, Nicholas P; Wang, Jenny; Kiss, Andrew M; Martin, Aiden A; Depond, Philip J; Guss, Gabriel M; Thampy, Vivek; Fong, Anthony Y; Weker, Johanna Nelson; Stone, Kevin H; Tassone, Christopher J; Kramer, Matthew J; Toney, Michael F; Van Buuren, Anthony; Matthews, Manyalibo J

2018-05-01

In situ X-ray-based measurements of the laser powder bed fusion (LPBF) additive manufacturing process produce unique data for model validation and improved process understanding. Synchrotron X-ray imaging and diffraction provide high resolution, bulk sensitive information with sufficient sampling rates to probe melt pool dynamics as well as phase and microstructure evolution. Here, we describe a laboratory-scale LPBF test bed designed to accommodate diffraction and imaging experiments at a synchrotron X-ray source during LPBF operation. We also present experimental results using Ti-6Al-4V, a widely used aerospace alloy, as a model system. Both imaging and diffraction experiments were carried out at the Stanford Synchrotron Radiation Lightsource. Melt pool dynamics were imaged at frame rates up to 4 kHz with a ∼1.1 μm effective pixel size and revealed the formation of keyhole pores along the melt track due to vapor recoil forces. Diffraction experiments at sampling rates of 1 kHz captured phase evolution and lattice contraction during the rapid cooling present in LPBF within a ∼50 × 100 μm area. We also discuss the utility of these measurements for model validation and process improvement.

An instrument for in situ time-resolved X-ray imaging and diffraction of laser powder bed fusion additive manufacturing processes

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

Calta, Nicholas P.; Wang, Jenny; Kiss, Andrew M.

In situ X-ray-based measurements of the laser powder bed fusion (LPBF) additive manufacturing process produce unique data for model validation and improved process understanding. Synchrotron X-ray imaging and diffraction provide high resolution, bulk sensitive information with sufficient sampling rates to probe melt pool dynamics as well as phase and microstructure evolution. Here, we describe a laboratory-scale LPBF test bed designed to accommodate diffraction and imaging experiments at a synchrotron X-ray source during LPBF operation. We also present experimental results using Ti-6Al-4V, a widely used aerospace alloy, as a model system. Both imaging and diffraction experiments were carried out at themore » Stanford Synchrotron Radiation Lightsource. Melt pool dynamics were imaged at frame rates up to 4 kHz with a ~1.1 μm effective pixel size and revealed the formation of keyhole pores along the melt track due to vapor recoil forces. Diffraction experiments at sampling rates of 1 kHz captured phase evolution and lattice contraction during the rapid cooling present in LPBF within a ~50 × 100 μm area. In conclusion, we also discuss the utility of these measurements for model validation and process improvement.« less

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

PubMed

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

2015-06-16

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

An instrument for in situ time-resolved X-ray imaging and diffraction of laser powder bed fusion additive manufacturing processes

DOE PAGES

Calta, Nicholas P.; Wang, Jenny; Kiss, Andrew M.; ...

2018-05-01

In situ X-ray-based measurements of the laser powder bed fusion (LPBF) additive manufacturing process produce unique data for model validation and improved process understanding. Synchrotron X-ray imaging and diffraction provide high resolution, bulk sensitive information with sufficient sampling rates to probe melt pool dynamics as well as phase and microstructure evolution. Here, we describe a laboratory-scale LPBF test bed designed to accommodate diffraction and imaging experiments at a synchrotron X-ray source during LPBF operation. We also present experimental results using Ti-6Al-4V, a widely used aerospace alloy, as a model system. Both imaging and diffraction experiments were carried out at themore » Stanford Synchrotron Radiation Lightsource. Melt pool dynamics were imaged at frame rates up to 4 kHz with a ~1.1 μm effective pixel size and revealed the formation of keyhole pores along the melt track due to vapor recoil forces. Diffraction experiments at sampling rates of 1 kHz captured phase evolution and lattice contraction during the rapid cooling present in LPBF within a ~50 × 100 μm area. In conclusion, we also discuss the utility of these measurements for model validation and process improvement.« less

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

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

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

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

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

PubMed

Humphreys, C J

2013-01-01

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

Chemical Doping Effects in Multilayer MoS2 and its Application in Complementary Inverter.

PubMed

Yoo, Hocheon; Hong, Seongin; On, Sungmin; Ahn, Hyungju; Lee, Han-Koo; Hong, Young Ki; Kim, Sunkook; Kim, Jae-Joon

2018-06-19

Multilayer MoS2 has been gaining interests as a new semiconducting material for flexible displays, memory devices, chemical/bio sensors, and photodetectors. However, conventional multilayer MoS2 devices have exhibited limited performances due to the Schottky barrier (SB) and defects. Here, we demonstrate PDPP3T doping effects in multilayer MoS2, which results in improved electrical characteristics (~3.2X mobility compared to the baseline and a high current on/off ratio of 106). Synchrotron-based study using X-ray photoelectron spectroscopy (XPS) and grazing-incidence wide-angle X-ray diffraction (GIWAXD) provides mechanisms that align the edge-on crystallites (97.5 %) of the PDPP3T as well as a larger interaction with MoS2 that leads to dipole and charge transfer effects (at annealing temperature of 300 °C), which support the observed enhancement of the electrical characteristics. Furthermore, we demonstrate a hybrid CMOS inverter using the PDPP3T-doped MoS2 and organic DNTT transistors as n- and p-channels, respectively. The proposed hybrid inverter offers an ultra-high voltage gain of ~205 V/V.

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.

Mechanical Properties versus Morphology of Ordered Polymers. Volume III. Part I

DTIC Science & Technology

1982-08-01

measured by wide angle x-ray scattering and differential scanning calorimetry, is unrelated to the diffuse scattered intensity [62]. Cellulose acetate which...increasing void fraction, in air swollen cellulose . Comparison of the volume fraction of voids calculated from the SAXS integrated intensity with...1964). 63. P.H. Hermans, D. Heikens, and A. Weidinger, "A Quantitative Investigation on the X-Ray Small Angle Scattering of Cellulose Fibers. Part II

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

Scanning three-dimensional x-ray diffraction microscopy using a high-energy microbeam

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

Hayashi, Y., E-mail: y-hayashi@mosk.tytlabs.co.jp; Hirose, Y.; Seno, Y.

2016-07-27

A scanning three-dimensional X-ray diffraction (3DXRD) microscope apparatus with a high-energy microbeam was installed at the BL33XU Toyota beamline at SPring-8. The size of the 50 keV beam focused using Kirkpatrick-Baez mirrors was 1.3 μm wide and 1.6 μm high in full width at half maximum. The scanning 3DXRD method was tested for a cold-rolled carbon steel sheet sample. A three-dimensional orientation map with 37 {sup 3} voxels was obtained.

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

Molecular Packing of Amphiphilic Nanosheets Resolved by X-ray Scattering

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

Harutyunyan, Boris; Dannenhoffer, Adam; Kewalramani, Sumit

2016-12-29

Molecular packing in light harvesting 2D assemblies of photocatalytic materials is a critical factor for solar-to-fuel conversion efficiency. However, structure–function correlations have yet to be fully established. This is partly due to the difficulties in extracting the molecular arrangements from the complex 3D powder averaged diffraction patterns of 2D lattices, obtained via in situ wide-angle X-ray scattering. Here, we develop a scattering theory formalism and couple it with a simple geometrical model for the molecular shape of chromophore 9-methoxy-N-(sodium hexanoate)perylene-3,4-dicarboximide (MeO-PMI) used in our study. This generally applicable method fully reproduces the measured diffraction pattern including the asymmetric line shapesmore » for the Bragg reflections and yields the molecular packing arrangement within a 2D crystal structure with a remarkable degree of detail. We find an approximate edge-centered herringbone structure for the PMI fused aromatic rings and ordering of the carboxypentyl chains above and below the nanosheets. Such a packing arrangement differs from the more symmetric face-to-face orientation of the unsubstituted PMI rings. This structural difference is correlated to our measurement of the reduced catalytic performance of MeO-PMI nanosheets as compared to the mesoscopically similar unsubstituted PMI assemblies.« less

Collagen organization in the chicken cornea and structural alterations in the retinopathy, globe enlarged (rge) phenotype--an X-ray diffraction study.

PubMed

Boote, Craig; Hayes, Sally; Jones, Simon; Quantock, Andrew J; Hocking, Paul M; Inglehearn, Chris F; Ali, Manir; Meek, Keith M

2008-01-01

An investigation into the collagenous structure of the mature avian cornea is presented. Wide-angle X-ray diffraction is employed to assess collagen organization in 9-month-old chicken corneas. The central 2-4mm corneal region features a preponderance of fibrils directed along the superior-inferior and nasal-temporal orthogonal meridians. More peripherally the orientation of fibrils alters in favor of a predominantly tangential arrangement. The chicken cornea appears to be circumscribed by an annulus of fibrils that extends into the limbus. The natural arrangement of collagen in the chicken cornea is discussed in relation to corneal shape and the mechanical requirements of avian corneal accommodation. Equivalent data are also presented from age-matched blind chickens affected with the retinopathy, globe enlarged (rge) mutation, characterized by an abnormally thick and flat cornea. The data indicate considerable realignment and redistribution of collagen lamellae in the peripheral rge cornea. In contrast to normal chickens, no obvious tangential collagen alignment was evident in the periphery of rge corneas. In mammals, the presence of a limbal fibril annulus is believed to be important in corneal shape preservation. We postulate that corneal flattening in rge chickens may be related to biomechanical changes brought about by an alteration in collagen arrangement at the corneal periphery.

Chemistry and properties of poly(arylene ether benzoxazole)s

NASA Technical Reports Server (NTRS)

Smith, J. G., Jr.; Connell, J. W.; Hergenrother, P. M.

1992-01-01

Several new poly(arylene ether benzoxazole)s (PAEBs) were prepared by the nucleophilic displacement reaction of activated aromatic difluorides with two novel bis(hydroxyphenyl benzoxazole), using potassium carbonate. The 6F-containing PAEBs exhibited better solubility and higher Tgs than did the 6,6'-bis-(2-(4-hydroxyphenyl)benzoxazole)-derived polymers. Several of the 6,6'bis(2-(4-hydroxyphenyl)benzoxazole)-derived polymers exhibited crystallinity by DSC and wide-angle X-ray diffraction. Unorientated thin film properties of the 6F-containing PAEBs were comparable to those of other 6F-containing PAEBS that were previously reported. The chemistry and the physical and mechanical properties of the above polymers are discussed.

Lattice strains and load partitioning in bovine trabecular bone.

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

Akhtar, R.; Daymond, M. R.; Almer, J. D.

2012-02-01

Microdamage and failure mechanisms have been well characterized in bovine trabecular bone. However, little is known about how elastic strains develop in the apatite crystals of the trabecular struts and their relationship with different deformation mechanisms. In this study, wide-angle high-energy synchrotron X-ray diffraction has been used to determine bulk elastic strains under in situ compression. Dehydrated bone is compared to hydrated bone in terms of their response to load. During compression, load is initially borne by trabeculae aligned parallel to loading direction with non-parallel trabeculae deforming by bending. Ineffective load partitioning is noted in dehydrated bone whereas hydrated bonemore » behaves like a plastically yielding foam« less

VizieR Online Data Catalog: WATCH Solar X-Ray Burst Catalogue (Crosby+ 1998)

NASA Astrophysics Data System (ADS)

Crosby, N.; Lund, N.; Vilmer, N.; Sunyaev, R.

1998-01-01

Catalogue containing solar X-ray bursts measured by the Danish Wide Angle Telescope for Cosmic Hard X-Rays (WATCH) experiment aboard the Russian satellite GRANAT in the deca-keV energy range. Table 1 lists the periods during which solar observations with WATCH are available (WATCH ON-TIME) and where the bursts listed in the catalogue have been observed. (2 data files).

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.

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.

Microscopy of biological sample through advanced diffractive optics from visible to X-ray wavelength regime.

PubMed

Di Fabrizio, Enzo; Cojoc, Dan; Emiliani, Valentina; Cabrini, Stefano; Coppey-Moisan, Maite; Ferrari, Enrico; Garbin, Valeria; Altissimo, Matteo

2004-11-01

The aim of this report is to demonstrate a unified version of microscopy through the use of advanced diffractive optics. The unified scheme derives from the technical possibility of realizing front wave engineering in a wide range of electromagnetic spectrum. The unified treatment is realized through the design and nanofabrication of phase diffractive elements (PDE) through which wave front beam shaping is obtained. In particular, we will show applications, by using biological samples, ranging from micromanipulation using optical tweezers to X-ray differential interference contrast (DIC) microscopy combined with X-ray fluorescence. We report some details on the design and physical implementation of diffractive elements that besides focusing also perform other optical functions: beam splitting, beam intensity, and phase redistribution or mode conversion. Laser beam splitting is used for multiple trapping and independent manipulation of micro-beads surrounding a cell as an array of tweezers and for arraying and sorting microscopic size biological samples. Another application is the Gauss to Laguerre-Gauss mode conversion, which allows for trapping and transfering orbital angular momentum of light to micro-particles immersed in a fluid. These experiments are performed in an inverted optical microscope coupled with an infrared laser beam and a spatial light modulator for diffractive optics implementation. High-resolution optics, fabricated by means of e-beam lithography, are demonstrated to control the intensity and the phase of the sheared beams in x-ray DIC microscopy. DIC experiments with phase objects reveal a dramatic increase in image contrast compared to bright-field x-ray microscopy. Besides the topographic information, fluorescence allows detection of certain chemical elements (Cl, P, Sc, K) in the same setup, by changing the photon energy of the x-ray beam. (c) 2005 Wiley-Liss, Inc.

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.

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).

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

PubMed

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

2015-03-01

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

Technical Report: Understanding Functional Lyotropic Liquid Crystal Network Phase Self-Assembly and the Properties of Nanoconfined Water

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

Mahanthappa, Mahesh K; Yethiraj, Arun

Through the synergistic interplay of molecular dynamics (MD) simulations, chemical synthesis, and materials characterization by X-ray and neutron scattering techniques, this project investigated the phase behaviors of new classes of aqueous lyotropic liquid crystals (LLCs) and the properties of water nanoconfined within their pores. A portion of our studies focused on the synthesis of new classes of alkylsulfonic acid and alkylphosphonate amphiphiles, which were shown to undergo water-induced self-assembly to form a wide variety of nanostructured morphologies with unusually high degrees of long-range translational order observed by small- angle X-ray scattering (SAXS). Sample LLC morphologies that were observed include themore » lamellar (L!), tricontinuous double gyroid (G), hexagonally-packed cylinders (H), and low symmetry discontinuous micellar (I) Frank-Kasper phases. Since the G and H phases are the most promising for the development of selective ion transporting membranes for energy applications, we sought the characterize the structure and dynamics of water confined within the sub-3 nm pores of these LLCs using wide-angle neutron diffraction (WAND) and quasielastic neutron scattering (QENS) experiments performed at the Spallation Neutron Source at Oak Ridge National Laboratory. Using molecular dynamics (MD) simulations, we validated models for analyzing this QENS data to obtain water self-diffusion coefficients in LLC G and H phases of carboxylate and sulfonate surfactant LLCs as a function of the identities of their charge compensating counterions.« less

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

Enhanced Crystalline Phase Purity of CH3NH3PbI3-xClx Film for High-Efficiency Hysteresis-Free Perovskite Solar Cells.

PubMed

Yang, Yingguo; Feng, Shanglei; Xu, Weidong; Li, Meng; Li, Li; Zhang, Xingmin; Ji, Gengwu; Zhang, Xiaonan; Wang, Zhaokui; Xiong, Yimin; Cao, Liang; Sun, Baoquan; Gao, Xingyu

2017-07-12

Despite rapid successful developments toward promising perovskite solar cells (PSCs) efficiency, they often suffer significant hysteresis effects. Using synchrotron-based grazing incidence X-ray diffraction (GIXRD) with different probing depths by varying the incident angle, we found that the perovskite films consist of dual phases with a parent phase dominant in the interior and a child phase with a smaller (110) interplanar space (d (110) ) after rapid thermal annealing (RTA), which is a widely used post treatment to improve the crystallization of solution-processed perovskite films for high-performance planar PSCs. In particular, the child phase composition gradually increases with decreasing depth till it becomes the majority on the surface, which might be one of the key factors related to hysteresis in fabricated PSCs. We further improve the crystalline phase purity of the solution-processed CH 3 NH 3 PbI 3-x Cl x perovskite film (referred as g-perovskite) by using a facile gradient thermal annealing (GTA), which shows a uniformly distributed phase structure in pinhole-free morphology with less undercoordinated Pb and I ions determined by synchrotron-based GIXRD, grazing incidence small-angle X-ray scattering, scanning electron microscopy, and X-ray photoelectron spectroscopy. Regardless of device structures (conventional and inverted types), the planar heterojunction PSCs employing CH 3 NH 3 PbI 3-x Cl x g-perovskite films exhibit negligible hysteresis with a champion power conversion efficiency of 17.04% for TiO 2 -based conventional planar PSCs and 14.83% for poly(3,4-ethylenedioxythiophene:poly(styrenesulfonate) (PEDOT:PSS)-based inverted planar PSCs. Our results indicate that the crystalline phase purity in CH 3 NH 3 PbI 3-x Cl x perovskite film, especially in the surface region, plays a crucial role in determining the hysteresis effect and device performance.

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

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

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.

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.

Surface layering and melting in an ionic liquid studied by resonant soft X-ray reflectivity

PubMed Central

Mezger, Markus; Ocko, Benjamin M.; Reichert, Harald; Deutsch, Moshe

2013-01-01

The molecular-scale structure of the ionic liquid [C18mim]+[FAP]− near its free surface was studied by complementary methods. X-ray absorption spectroscopy and resonant soft X-ray reflectivity revealed a depth-decaying near-surface layering. Element-specific interfacial profiles were extracted with submolecular resolution from energy-dependent soft X-ray reflectivity data. Temperature-dependent hard X-ray reflectivity, small- and wide-angle X-ray scattering, and infrared spectroscopy uncovered an intriguing melting mechanism for the layered region, where alkyl chain melting drove a negative thermal expansion of the surface layer spacing. PMID:23431181

Surface-treated self-standing curved crystals as high-efficiency elements for X- and γ-ray optics: theory and experiment.

PubMed

Bonnini, Elisa; Buffagni, Elisa; Zappettini, Andrea; Doyle, Stephen; Ferrari, Claudio

2015-06-01

The efficiency of a Laue lens for X- and γ-ray focusing in the energy range 60-600 keV is closely linked to the diffraction efficiency of the single crystals composing the lens. A powerful focusing system is crucial for applications like medical imaging and X-ray astronomy where wide beams must be focused. Mosaic crystals with a high density, such as Cu or Au, and bent crystals with curved diffracting planes (CDPs) are considered for the realization of a focusing system for γ-rays, owing to their high diffraction efficiency in a predetermined angular range. In this work, a comparison of the efficiency of CDP crystals and Cu and Au mosaic crystals was performed on the basis of the theory of X-ray diffraction. Si, GaAs and Ge CDP crystals with optimized thicknesses and moderate radii of curvature of several tens of metres demonstrate comparable or superior performance with respect to the higher atomic number mosaic crystals generally used. In order to increase the efficiency of the lens further, a stack of several CDP crystals is proposed as an optical element. CDP crystals were obtained by a surface-damage method, and a stack of two surface-damaged bent Si crystals was prepared and tested. Rocking curves of the stack were performed with synchrotron radiation at 19 keV to check the lattice alignment: they exhibited only one diffraction peak.

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.

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.

PREFACE: Exploring surfaces and buried interfaces of functional materials by advanced x-ray and neutron techniques Exploring surfaces and buried interfaces of functional materials by advanced x-ray and neutron techniques

NASA Astrophysics Data System (ADS)

Sakurai, Kenji

2010-12-01

This special issue is devoted to describing recent applications of x-ray and neutron scattering techniques to the exploration of surfaces and buried interfaces of various functional materials. Unlike many other surface-sensitive methods, these techniques do not require ultra high vacuum, and therefore, a variety of real and complicated surfaces fall within the scope of analysis. It must be particularly emphasized that the techniques are capable of seeing even buried function interfaces as well as the surface. Furthermore, the information, which ranges from the atomic to mesoscopic scale, is highly quantitative and reproducible. The non-destructive nature of the techniques is another important advantage of using x-rays and neutrons, when compared with other atomic-scale analyses. This ensures that the same specimen can be measured by other techniques. Such features are fairly attractive when exploring multilayered materials with nanostructures (dots, tubes, wires, etc), which are finding applications in electronic, magnetic, optical and other devices. The Japan Applied Physics Society has established a group to develop the research field of studying buried function interfaces with x-rays and neutrons. As the methods can be applied to almost all types of materials, from semiconductor and electronic devices to soft materials, participants have fairly different backgrounds but share a common interest in state-of-the-art x-ray and neutron techniques and sophisticated applications. A series of workshops has been organized almost every year since 2001. Some international interactions have been continued intensively, although the community is part of a Japanese society. This special issue does not report the proceedings of the recent workshop, although all the authors are in some way involved in the activities of the above society. Initially, we intended to collect quite long overview papers, including the authors' latest and most important original results, as well as updates on recent progress and global trends in the field. We planned to cover quite a wide area of surface and buried interface science with x-rays and neutrons. Following a great deal of discussion during the editing process, we have decided to change direction. As we intend to publish similar special issues on a frequent basis, we will not insist on editing this issue as systematic and complete collections of research. Many authors decided to write an ordinary research paper rather than an article including systematic accounts. Due to this change in policy, some authors declined to contribute, and the number of papers is now just 12. However, readers will find that the special issue gives an interesting collection of new original research in surface and buried interface studies with x-rays and neutrons. The 12 papers cover the following research topics: (1) polymer analysis by diffuse scattering; (2) discussion of the electrochemical solid--liquid interface by synchrotron x-ray diffraction; (3) analysis of capped nanodots by grazing incidence small-angle x-ray scattering (GISAXS); (4) discussion of the strain distribution in silicon by high-resolution x-ray diffraction; (5) study of mesoporous structures by a combination of x-ray reflectivity and GISAXS; (6) discussion of energy-dispersive x-ray reflectometry and its applications; (7) neutron reflectivity studies on hydrogen terminated silicon interface; (8) the fabrication and performance of a special mirror for water windows; (9) depth selective analysis by total-reflection x-ray diffraction; (10) nanoparticle thin films prepared by a gas deposition technique; (11) discussion of crystal truncation rod (CTR) scattering of semiconductor nanostructures; (12) magnetic structure analysis of thin films by polarized neutron reflectivity. While not discussed in the present special issue, x-ray and neutron techniques have made great progress. The most important steps forward have been in 2D/3D real-space imaging, and realtime measurement. Advances in such technologies are bringing with them new opportunities in surface and buried interface science. In the not too distant future, we will publish a special issue or a book detailing such progress. Exploring surfaces and buried interfaces of functional materials by advanced x-ray and neutron techniques contents Lateral uniformity in chemical composition along a buried reaction front in polymers using off-specular reflectivity Kristopher A Lavery, Vivek M Prabhu, Sushil Satija and Wen-li Wu Orientation dependence of Pd growth on Au electrode surfaces M Takahasi, K Tamura, J Mizuki, T Kondo and K Uosaki A grazing incidence small-angle x-ray scattering analysis on capped Ge nanodots in layer structures Hiroshi Okuda, Masayuki Kato, Keiji Kuno, Shojiro Ochiai, Noritaka Usami, Kazuo Nakajima and Osami Sakata High resolution grazing-incidence in-plane x-ray diffraction for measuring the strain of a Si thin layer Kazuhiko Omote X-ray analysis of mesoporous silica thin films templated by Brij58 surfactant S Fall, M Kulij and A Gibaud Review of the applications of x-ray refraction and the x-ray waveguide phenomenon to estimation of film structures Kouichi Hayashi Epitaxial growth of largely mismatched crystals on H-terminated Si(111) surfaces Hidehito Asaoka Novel TiO2/ZnO multilayer mirrors at 'water-window' wavelengths fabricated by atomic layer epitaxy H Kumagai, Y Tanaka, M Murata, Y Masuda and T Shinagawa Depth-selective structural analysis of thin films using total-external-reflection x-ray diffraction Tomoaki Kawamura and Hiroo Omi Structures of Yb nanoparticle thin films grown by deposition in He and N2 gas atmospheres: AFM and x-ray reflectivity studies Martin Jerab and Kenji Sakurai Ga and As composition profiles in InP/GaInAs/InP heterostructures—x-ray CTR scattering and cross-sectional STM measurements Yoshikazu Takeda, Masao Tabuchi and Arao Nakamura Polarized neutron reflectivity study of a thermally treated MnIr/CoFe exchange bias system Naoki Awaji, Toyoo Miyajima, Shuuichi Doi and Kenji Nomura

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.

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

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.

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

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.

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.

Fourier Transforms Simplified: Computing an Infrared Spectrum from an Interferogram

ERIC Educational Resources Information Center

Hanley, Quentin S.

2012-01-01

Fourier transforms are used widely in chemistry and allied sciences. Examples include infrared, nuclear magnetic resonance, and mass spectroscopies. A thorough understanding of Fourier methods assists the understanding of microscopy, X-ray diffraction, and diffraction gratings. The theory of Fourier transforms has been presented in this "Journal",…

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.

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.

The atomic scale structure of CXV carbon: wide-angle x-ray scattering and modeling studies.

PubMed

Hawelek, L; Brodka, A; Dore, J C; Honkimaki, V; Burian, A

2013-11-13

The disordered structure of commercially available CXV activated carbon produced from finely powdered wood-based carbon has been studied using the wide-angle x-ray scattering technique, molecular dynamics and density functional theory simulations. The x-ray scattering data has been converted to the real space representation in the form of the pair correlation function via the Fourier transform. Geometry optimizations using classical molecular dynamics based on the reactive empirical bond order potential and density functional theory at the B3LYP/6-31g* level have been performed to generate nanoscale models of CXV carbon consistent with the experimental data. The final model of the structure comprises four chain-like and buckled graphitic layers containing a small percentage of four-fold coordinated atoms (sp(3) defects) in each layer. The presence of non-hexagonal rings in the atomic arrangement has been also considered.

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.

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

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

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

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.

Automated comprehensive Adolescent Idiopathic Scoliosis assessment using MVC-Net.

PubMed

Wu, Hongbo; Bailey, Chris; Rasoulinejad, Parham; Li, Shuo

2018-05-18

Automated quantitative estimation of spinal curvature is an important task for the ongoing evaluation and treatment planning of Adolescent Idiopathic Scoliosis (AIS). It solves the widely accepted disadvantage of manual Cobb angle measurement (time-consuming and unreliable) which is currently the gold standard for AIS assessment. Attempts have been made to improve the reliability of automated Cobb angle estimation. However, it is very challenging to achieve accurate and robust estimation of Cobb angles due to the need for correctly identifying all the required vertebrae in both Anterior-posterior (AP) and Lateral (LAT) view x-rays. The challenge is especially evident in LAT x-ray where occlusion of vertebrae by the ribcage occurs. We therefore propose a novel Multi-View Correlation Network (MVC-Net) architecture that can provide a fully automated end-to-end framework for spinal curvature estimation in multi-view (both AP and LAT) x-rays. The proposed MVC-Net uses our newly designed multi-view convolution layers to incorporate joint features of multi-view x-rays, which allows the network to mitigate the occlusion problem by utilizing the structural dependencies of the two views. The MVC-Net consists of three closely-linked components: (1) a series of X-modules for joint representation of spinal structure (2) a Spinal Landmark Estimator network for robust spinal landmark estimation, and (3) a Cobb Angle Estimator network for accurate Cobb Angles estimation. By utilizing an iterative multi-task training algorithm to train the Spinal Landmark Estimator and Cobb Angle Estimator in tandem, the MVC-Net leverages the multi-task relationship between landmark and angle estimation to reliably detect all the required vertebrae for accurate Cobb angles estimation. Experimental results on 526 x-ray images from 154 patients show an impressive 4.04° Circular Mean Absolute Error (CMAE) in AP Cobb angle and 4.07° CMAE in LAT Cobb angle estimation, which demonstrates the MVC-Net's capability of robust and accurate estimation of Cobb angles in multi-view x-rays. Our method therefore provides clinicians with a framework for efficient, accurate, and reliable estimation of spinal curvature for comprehensive AIS assessment. Copyright © 2018. Published by Elsevier B.V.

Mesoporous CdS via Network of Self-Assembled Nanocrystals: Synthesis, Characterization and Enhanced Photoconducting Property.

PubMed

Patra, Astam K; Banerjee, Biplab; Bhaumik, Asim

2018-01-01

Semiconduction nanoparticles are intensively studied due to their huge potential in optoelctronic applications. Here we report an efficient chemical route for hydrothermal synthesis of aggregated mesoporous cadmium sulfide (CdS) nanoparticles using supramolecular-assembly of ionic and water soluble sodium salicylate as the capping agent. The nanostructure, mesophase, optical property and photoconductivity of these mesoporous CdS materials have been characterized by using small and wide angle powder X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), N2-sorption, Raman analysis, Fourier transformed infrared (FT-IR), UV-Visible DSR spectroscopy, and photoconductivity measurement. Wide angle XRD pattern and high resolution TEM image analysis suggested that the particle size of the materials is within 10 nm and the nanoparticles are in well-crystallized cubic phase. Mesoporous CdS nanoparticles showed drastically enhanced photoelectrochemical response under visible light irradiation on entrapping a photosensitizer (dye) molecule in the interparticle spaces. Efficient synthesis strategy and the enhanced photo response in the mesoporous CdS material could facilitate the designing of other porous semiconductor oxide/sulfide and their applications in photon-to-electron conversion processes.

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.

Growth and properties of wide bandgap (MgSe)n(ZnxCd1-xSe)m short-period superlattices

NASA Astrophysics Data System (ADS)

Garcia, Thor A.; Tamargo, Maria C.

2017-12-01

We report the molecular beam epitaxy (MBE) growth and properties of (MgSe)n(ZnxCd1-x Se)m short-period superlattices(SPSLs) for potential application in II-VI devices grown on InP substrates. SPSL structures up to 1 μm thick with effective bandgaps ranging from 2.6 eV to above 3.42 eV are grown and characterized, extending the typical range possible for the ZnxCdyMg1-x-ySe random alloy beyond 3.2 eV. Additionally, ZnxCd1-xSe single and multiple quantum well structures using the SPSL barriers are also grown and investigated. The structures are characterized utilizing reflection high-energy electron diffraction, X-ray reflectance, X-ray diffraction and photoluminescence. We observed layer-by-layer growth and smoother interfaces in the QWs grown with SPSL when compared to the ZnxCdyMg1-x-ySe random alloy. The results indicate that this materials platform is a good candidate to replace the random alloy in wide bandgap device applications.

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.

Structural hysteresis in dragline spider silks induced by supercontraction: an X-ray fiber micro-diffraction study

DOE PAGES

Sampath, Sujatha; Yarger, Jeffery L.

2014-11-27

Interaction with water causes shrinkage and significant changes in the structure of spider dragline silks, which has been referred to as supercontraction in the literature. Preferred orientation or alignment of protein chains with respect to the fiber axis is extensively changed during this supercontraction process. Synchrotron X-ray micro-fiber diffraction experiments have been performed on Nephila clavipes and Argiope aurantia major and minor ampullate dragline spider fibers in the native dry, contracted (by immersion in water) and restretched (from contracted) states. Changes in the orientation of β-sheet nanocrystallites and the oriented component of the amorphous network have been determined from wide-anglemore » X-ray diffraction patterns. While both the crystalline and amorphous components lose preferred orientation on wetting with water, the nano-crystallites regain their orientation on wet-restretching, whereas the oriented amorphous components only partially regain their orientation. Dragline major ampullate silks in both the species contract more than their minor ampullate silks.« 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

Beyond simple small-angle X-ray scattering: developments in online complementary techniques and sample environments.

PubMed

Bras, Wim; Koizumi, Satoshi; Terrill, Nicholas J

2014-11-01

Small- and wide-angle X-ray scattering (SAXS, WAXS) are standard tools in materials research. The simultaneous measurement of SAXS and WAXS data in time-resolved studies has gained popularity due to the complementary information obtained. Furthermore, the combination of these data with non X-ray based techniques, via either simultaneous or independent measurements, has advanced understanding of the driving forces that lead to the structures and morphologies of materials, which in turn give rise to their properties. The simultaneous measurement of different data regimes and types, using either X-rays or neutrons, and the desire to control parameters that initiate and control structural changes have led to greater demands on sample environments. Examples of developments in technique combinations and sample environment design are discussed, together with a brief speculation about promising future developments.

Beyond simple small-angle X-ray scattering: developments in online complementary techniques and sample environments

PubMed Central

Bras, Wim; Koizumi, Satoshi; Terrill, Nicholas J

2014-01-01

Small- and wide-angle X-ray scattering (SAXS, WAXS) are standard tools in materials research. The simultaneous measurement of SAXS and WAXS data in time-resolved studies has gained popularity due to the complementary information obtained. Furthermore, the combination of these data with non X-ray based techniques, via either simultaneous or independent measurements, has advanced understanding of the driving forces that lead to the structures and morphologies of materials, which in turn give rise to their properties. The simultaneous measurement of different data regimes and types, using either X-rays or neutrons, and the desire to control parameters that initiate and control structural changes have led to greater demands on sample environments. Examples of developments in technique combinations and sample environment design are discussed, together with a brief speculation about promising future developments. PMID:25485128

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

Abe, T., E-mail: kikutani.t.aa@m.titech.ac.jp; Takarada, W., E-mail: kikutani.t.aa@m.titech.ac.jp; Kikutani, T., E-mail: kikutani.t.aa@m.titech.ac.jp

Effect of pre-annealing on stress and birefringence behavior of poly(ethylene naphthalate) (PEN) films during stretching and relaxation processes was investigated. Amorphous and non-oriented PEN films were pre-annealed under the conditions of different temperatures and periods. The pre-annealed films were stretched uniaxially or equi-biaxially and then relaxed at fixed length. It was found that pre-annealing did not cause any notable change for the initial behavior of refractive indices variation, whereas the behaviors after necking were significantly affected. Through the comparison between in-plane and out-of-plane birefringence and the analysis of wide-angle x-ray diffraction patterns of drawn films of both stretching modes, itmore » was confirmed that the orientation of naphthalene ring in the film plane was enhanced by pre-annealing.« less

Synthesis of nanodimensional TiO2 thin films.

PubMed

Thakurdesai, Madhavi; Mohanty, T; John, J; Rao, T K Gundu; Raychaudhuri, Pratap; Bhattacharyya, V; Kanjilal, D

2008-08-01

Nanodimensional TiO2 has wide application in the field of photocatalysis, photovoltaic and photochromic devices. In present investigation TiO2 thin films deposited by pulsed laser deposition method are irradiated by 100 MeV Ag ion beam to achieve growth of nanophases. The nanostructure evolution is characterized by atomic force microscopy (AFM). The phases of TiO2 formed after irradiation are identified by glancing angle X-ray diffraction and Raman spectroscopy. The particle radius estimated by AFM varies from 10-13 nm. Anatase phase of TiO2 is formed after irradiation. The blue shift observed in UV-VIS absorption spectra indicates the nanostructure formation. The shape and size of nanoparticles formed due to high electronic excitation depend upon thickness of the film.

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

Methods development for diffraction and spectroscopy studies of metalloenzymes at X-ray free-electron lasers

PubMed Central

Kern, Jan; Hattne, Johan; Tran, Rosalie; Alonso-Mori, Roberto; Laksmono, Hartawan; Gul, Sheraz; Sierra, Raymond G.; Rehanek, Jens; Erko, Alexei; Mitzner, Rolf; Wernet, Phillip; Bergmann, Uwe; Sauter, Nicholas K.; Yachandra, Vittal; Yano, Junko

2014-01-01

X-ray free-electron lasers (XFELs) open up new possibilities for X-ray crystallographic and spectroscopic studies of radiation-sensitive biological samples under close to physiological conditions. To facilitate these new X-ray sources, tailored experimental methods and data-processing protocols have to be developed. The highly radiation-sensitive photosystem II (PSII) protein complex is a prime target for XFEL experiments aiming to study the mechanism of light-induced water oxidation taking place at a Mn cluster in this complex. We developed a set of tools for the study of PSII at XFELs, including a new liquid jet based on electrofocusing, an energy dispersive von Hamos X-ray emission spectrometer for the hard X-ray range and a high-throughput soft X-ray spectrometer based on a reflection zone plate. While our immediate focus is on PSII, the methods we describe here are applicable to a wide range of metalloenzymes. These experimental developments were complemented by a new software suite, cctbx.xfel. This software suite allows for near-real-time monitoring of the experimental parameters and detector signals and the detailed analysis of the diffraction and spectroscopy data collected by us at the Linac Coherent Light Source, taking into account the specific characteristics of data measured at an XFEL. PMID:24914169

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.

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.

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

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

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.

Minimizing Experimental Setup Time and Effort at APS beamline 1-ID through Instrumentation Design

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

Benda, Erika; Almer, Jonathan; Kenesei, Peter

2016-01-01

Sector 1-ID at the APS accommodates a number of dif-ferent experimental techniques in the same spatial enve-lope of the E-hutch end station. These include high-energy small and wide angle X-ray scattering (SAXS and WAXS), high-energy diffraction microscopy (HEDM, both near and far field modes) and high-energy X-ray tomography. These techniques are frequently combined to allow the users to obtain multimodal data, often attaining 1 μm spatial resolution and <0.05º angular resolution. Furthermore, these techniques are utilized while the sam-ple is thermo-mechanically loaded to mimic real operat-ing conditions. The instrumentation required for each of these techniques and environments has been designedmore » and configured in a modular way with a focus on stability and repeatability between changeovers. This approach allows the end station to be more versatile, capable of collecting multi-modal data in-situ while reducing time and effort typically required for set up and alignment, resulting in more efficient beam time use. Key instrumentation de-sign features and layout of the end station are presented.« less

Advanced techniques for characterization of ion beam modified materials

DOE PAGES

Zhang, Yanwen; Debelle, Aurélien; Boulle, Alexandre; ...

2014-10-30

Understanding the mechanisms of damage formation in materials irradiated with energetic ions is essential for the field of ion-beam materials modification and engineering. Utilizing incident ions, electrons, photons, and positrons, various analysis techniques, including Rutherford backscattering spectrometry (RBS), electron RBS, Raman spectroscopy, high-resolution X-ray diffraction, small-angle X-ray scattering, and positron annihilation spectroscopy, are routinely used or gaining increasing attention in characterizing ion beam modified materials. The distinctive information, recent developments, and some perspectives in these techniques are reviewed in this paper. Applications of these techniques are discussed to demonstrate their unique ability for studying ion-solid interactions and the corresponding radiationmore » effects in modified depths ranging from a few nm to a few tens of μm, and to provide information on electronic and atomic structure of the materials, defect configuration and concentration, as well as phase stability, amorphization and recrystallization processes. Finally, such knowledge contributes to our fundamental understanding over a wide range of extreme conditions essential for enhancing material performance and also for design and synthesis of new materials to address a broad variety of future energy applications.« less

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

Xu, Gui-Liang; Chen, Zonghai; Zhong, Gui-Ming

Sodium-ion batteries are promising alternatives to lithium-ion batteries for large-scale applications. However, the low capacity and poor rate capability of existing anodes for sodium-ion batteries are bottlenecks for future developments. Here, we report a high performance nanostructured anode material for sodium-ion batteries that is fabricated by high energy ball milling to form black phosphorus/Ketjenblack–multiwalled carbon nanotubes (BPC) composite. With this strategy, the BPC composite with a high phosphorus content (70 wt %) could deliver a very high initial Coulombic efficiency (>90%) and high specific capacity with excellent cyclability at high rate of charge/discharge (~1700 mAh g–1 after 100 cycles atmore » 1.3 A g–1 based on the mass of P). In situ electrochemical impedance spectroscopy, synchrotron high energy X-ray diffraction, ex situ small/wide-angle X-ray scattering, high resolution transmission electronic microscopy, and nuclear magnetic resonance were further used to unravel its superior sodium storage performance. The scientific findings gained in this work are expected to serve as a guide for future design on high performance anode material for sodium-ion batteries.« less

Critical size of crystalline ZrO(2) nanoparticles synthesized in near- and supercritical water and supercritical isopropyl alcohol.

PubMed

Becker, Jacob; Hald, Peter; Bremholm, Martin; Pedersen, Jan S; Chevallier, Jacques; Iversen, Steen B; Iversen, Bo B

2008-05-01

Nanocrystalline ZrO(2) samples with narrow size distributions and mean particle sizes below 10 nm have been synthesized in a continuous flow reactor in near and supercritical water as well as supercritical isopropyl alcohol using a wide range of temperatures, pressures, concentrations and precursors. The samples were comprehensively characterized by powder X-ray diffraction (PXRD), transmission electron microscopy (TEM), and small-angle X-ray scattering (SAXS), and the influence of the synthesis parameters on the particle size, particle size distribution, shape, aggregation and crystallinity was studied. On the basis of the choice of synthesis parameters either monoclinic or tetragonal zirconia phases can be obtained. The results suggest a critical particle size of 5-6 nm for nanocrystalline monoclinic ZrO(2) under the present conditions, which is smaller than estimates reported in the literature. Thus, very small monoclinic ZrO(2) particles can be obtained using a continuous flow reactor. This is an important result with respect to improvement of the catalytic properties of nanocrystalline ZrO(2).

An Optically Isotropic Antiferroelectric Liquid Crystal (OI-AFLC) Display Mode Operating over a Wide Temperature Range using Ternary Bent-Core Liquid Crystal Mixtures

DOE PAGES

Bergquist, Leah; Zhang, Cuiyu; Ribeiro de Almeida, Roberta R.; ...

2017-02-07

Here, we report on the synthesis and characterization of bent-core liquid crystal (LC) compounds and the preparation of mixtures that provide an optically isotropic antiferroelectric (OI-AFLC) liquid crystal display mode over a very wide temperature interval and well below room temperature. From the collection of compounds synthesized during this study, we recognized that several ternary mixtures displayed a modulated SmC aP A phase down to below -40 °C and up to about 100 °C on both heating and cooling, as well as optical tilt angles in the transformed state of approximately 45° (optically isotropic state). The materials were fully characterizedmore » and their liquid crystal as well as electro-optical properties analyzed by polarized optical microscopy, differential scanning calorimetry, synchrotron X-ray diffraction, dielectric spectroscopy, and electro-optical tests.« less

An Optically Isotropic Antiferroelectric Liquid Crystal (OI-AFLC) Display Mode Operating over a Wide Temperature Range using Ternary Bent-Core Liquid Crystal Mixtures

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

Bergquist, Leah; Zhang, Cuiyu; Ribeiro de Almeida, Roberta R.

Here, we report on the synthesis and characterization of bent-core liquid crystal (LC) compounds and the preparation of mixtures that provide an optically isotropic antiferroelectric (OI-AFLC) liquid crystal display mode over a very wide temperature interval and well below room temperature. From the collection of compounds synthesized during this study, we recognized that several ternary mixtures displayed a modulated SmC aP A phase down to below -40 °C and up to about 100 °C on both heating and cooling, as well as optical tilt angles in the transformed state of approximately 45° (optically isotropic state). The materials were fully characterizedmore » and their liquid crystal as well as electro-optical properties analyzed by polarized optical microscopy, differential scanning calorimetry, synchrotron X-ray diffraction, dielectric spectroscopy, and electro-optical tests.« less

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

Cross-sectional transmission electron microscopic study of irradiation induced nano-crystallization of nickel in a W/Ni multilayer.

PubMed

Bagchi, Sharmistha; Lalla, N P

2008-06-11

The present study reports the cross-sectional transmission electron microscopic investigations of swift heavy ion-irradiation induced nano-size recrystallization of Ni in a nearly immiscible W/Ni multilayer structure. Multilayer structures (MLS) of [W(25 Å)/Ni(25 Å)](10BL) were grown on Si-(100) substrate by the ion-beam sputtering technique. The as-synthesized MLS were subjected to 120 MeV-Au(9+) ion-irradiation to a fluence of ∼5 × 10(13) ions cm(-2). Wide-angle x-ray diffraction studies of pristine as well as irradiated W/Ni multilayers show deterioration of the superlattice structure, whereas x-ray reflectivity (XRR) measurement reveals a nearly unaffected microstructure after irradiation. Analysis of the XRR data using 'Parratt's formalism' does show a significant increase of W/Ni interface roughness. Cross-sectional transmission electron microscopy (TEM) studies carried out in diffraction and imaging modes (including bright-field and dark-field imaging), show that at high irradiation dose the intralayer microstructure of Ni becomes nano-crystalline (1-2 nm). During these irradiation induced changes of the intralayer microstructure, the interlayer definition of the W and Ni layers still remains intact. The observed nano-recrystallization of Ni has been attributed to competition between low miscibility of the W/Ni interface and the ion-beam induced mixing kinetics.

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.

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).

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.

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.

Theoretical study of the properties of X-ray diffraction moiré fringes. I

PubMed Central

Yoshimura, Jun-ichi

2015-01-01

A detailed and comprehensive theoretical description of X-ray diffraction moiré fringes for a bicrystal specimen is given on the basis of a calculation by plane-wave dynamical diffraction theory. Firstly, prior to discussing the main subject of the paper, a previous article [Yoshimura (1997 ▸). Acta Cryst. A53, 810–812] on the two-dimensionality of diffraction moiré patterns is restated on a thorough calculation of the moiré interference phase. Then, the properties of moiré fringes derived from the above theory are explained for the case of a plane-wave diffraction image, where the significant effect of Pendellösung intensity oscillation on the moiré pattern when the crystal is strained is described in detail with theoretically simulated moiré images. Although such plane-wave moiré images are not widely observed in a nearly pure form, knowledge of their properties is essential for the understanding of diffraction moiré fringes in general. PMID:25970298

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.

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.

Aerodynamic levitation, supercooled liquids and glass formation

DOE PAGES

Benmore, C. J.; Weber, J. K. R.

2017-05-04

Containerless processing or ‘levitation’ is a valuable tool for the synthesis and characterization of materials, particularly at extreme temperatures and under non-equilibrium conditions. The method enables formation of novel glasses, amorphous phases, and metastable crystalline forms that are not easily accessed when nucleation and growth can readily occur at a container interface. Removing the container enables the use of a wide variety of process atmospheres to modify a materials structure and properties. In the past decade levitation methods, including acoustic, aerodynamic, electromagnetic, and electrostatic, have become well established sample environments at X-ray synchrotron and neutron sources. This article briefly reviewsmore » the methods and then focuses on the application of aerodynamic levitation to synthesize and study new materials. This is presented in conjunction with non-contact probes used to investigate the atomic structure and to measure the properties of materials at extreme temperatures. The use of aerodynamic levitation in research using small and wide-angle X-ray diffraction, XANES, and neutron scattering are discussed in the context of technique development. The use of the containerless methods to investigate thermophysical properties is also considered. We argue that structural motifs and in the liquid state can potentially lead to the fabrication of materials, whose properties would differ substantially from their well known crystalline forms.« 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.

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.

High-dynamic-range coherent diffractive imaging: ptychography using the mixed-mode pixel array detector

PubMed Central

Giewekemeyer, Klaus; Philipp, Hugh T.; Wilke, Robin N.; Aquila, Andrew; Osterhoff, Markus; Tate, Mark W.; Shanks, Katherine S.; Zozulya, Alexey V.; Salditt, Tim; Gruner, Sol M.; Mancuso, Adrian P.

2014-01-01

Coherent (X-ray) diffractive imaging (CDI) is an increasingly popular form of X-ray microscopy, mainly due to its potential to produce high-resolution images and the lack of an objective lens between the sample and its corresponding imaging detector. One challenge, however, is that very high dynamic range diffraction data must be collected to produce both quantitative and high-resolution images. In this work, hard X-ray ptychographic coherent diffractive imaging has been performed at the P10 beamline of the PETRA III synchrotron to demonstrate the potential of a very wide dynamic range imaging X-ray detector (the Mixed-Mode Pixel Array Detector, or MM-PAD). The detector is capable of single photon detection, detecting fluxes exceeding 1 × 108 8-keV photons pixel−1 s−1, and framing at 1 kHz. A ptychographic reconstruction was performed using a peak focal intensity on the order of 1 × 1010 photons µm−2 s−1 within an area of approximately 325 nm × 603 nm. This was done without need of a beam stop and with a very modest attenuation, while ‘still’ images of the empty beam far-field intensity were recorded without any attenuation. The treatment of the detector frames and CDI methodology for reconstruction of non-sensitive detector regions, partially also extending the active detector area, are described. PMID:25178008

High-dynamic-range coherent diffractive imaging: ptychography using the mixed-mode pixel array detector.

PubMed

Giewekemeyer, Klaus; Philipp, Hugh T; Wilke, Robin N; Aquila, Andrew; Osterhoff, Markus; Tate, Mark W; Shanks, Katherine S; Zozulya, Alexey V; Salditt, Tim; Gruner, Sol M; Mancuso, Adrian P

2014-09-01

Coherent (X-ray) diffractive imaging (CDI) is an increasingly popular form of X-ray microscopy, mainly due to its potential to produce high-resolution images and the lack of an objective lens between the sample and its corresponding imaging detector. One challenge, however, is that very high dynamic range diffraction data must be collected to produce both quantitative and high-resolution images. In this work, hard X-ray ptychographic coherent diffractive imaging has been performed at the P10 beamline of the PETRA III synchrotron to demonstrate the potential of a very wide dynamic range imaging X-ray detector (the Mixed-Mode Pixel Array Detector, or MM-PAD). The detector is capable of single photon detection, detecting fluxes exceeding 1 × 10(8) 8-keV photons pixel(-1) s(-1), and framing at 1 kHz. A ptychographic reconstruction was performed using a peak focal intensity on the order of 1 × 10(10) photons µm(-2) s(-1) within an area of approximately 325 nm × 603 nm. This was done without need of a beam stop and with a very modest attenuation, while `still' images of the empty beam far-field intensity were recorded without any attenuation. The treatment of the detector frames and CDI methodology for reconstruction of non-sensitive detector regions, partially also extending the active detector area, are described.

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.

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.

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.

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.

High diffraction efficiency of three-layer diffractive optics designed for wide temperature range and large incident angle.

PubMed

Mao, Shan; Cui, Qingfeng; Piao, Mingxu; Zhao, Lidong

2016-05-01

A mathematical model of diffraction efficiency and polychromatic integral diffraction efficiency affected by environment temperature change and incident angle for three-layer diffractive optics with different dispersion materials is put forward, and its effects are analyzed. Taking optical materials N-FK5 and N-SF1 as the substrates of multilayer diffractive optics, the effect on diffraction efficiency and polychromatic integral diffraction efficiency with intermediate materials POLYCARB is analyzed with environment temperature change as well as incident angle. Therefore, three-layer diffractive optics can be applied in more wide environmental temperature ranges and larger incident angles for refractive-diffractive hybrid optical systems, which can obtain better image quality. Analysis results can be used to guide the hybrid imaging optical system design for optical engineers.

Novel micro-reactor flow cell for investigation of model catalysts using in situ grazing-incidence X-ray scattering

PubMed Central

Kehres, Jan; Pedersen, Thomas; Masini, Federico; Andreasen, Jens Wenzel; Nielsen, Martin Meedom; Diaz, Ana; Nielsen, Jane Hvolbæk; Hansen, Ole

2016-01-01

The design, fabrication and performance of a novel and highly sensitive micro-reactor device for performing in situ grazing-incidence X-ray scattering experiments of model catalyst systems is presented. The design of the reaction chamber, etched in silicon on insulator (SIO), permits grazing-incidence small-angle X-ray scattering (GISAXS) in transmission through 10 µm-thick entrance and exit windows by using micro-focused beams. An additional thinning of the Pyrex glass reactor lid allows simultaneous acquisition of the grazing-incidence wide-angle X-ray scattering (GIWAXS). In situ experiments at synchrotron facilities are performed utilizing the micro-reactor and a designed transportable gas feed and analysis system. The feasibility of simultaneous in situ GISAXS/GIWAXS experiments in the novel micro-reactor flow cell was confirmed with CO oxidation over mass-selected Ru nanoparticles. PMID:26917133

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.

Side-Chain Liquid Crystalline Poly(meth)acrylates with Bent-Core Mesogens

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

Chen,X.; Tenneti, K.; Li, C.

2007-01-01

We report the design, synthesis, and characterization of side-chain liquid crystalline (LC) poly(meth)acrylates with end-on bent-core liquid crystalline (BCLC) mesogens. Both conventional free radical polymerization and atom transfer radical polymerization have been used to synthesize these liquid crystalline polymers (LCP). The resulting polymers exhibit thermotropic LC behavior. Differential scanning calorimetry, thermopolarized light microscopy, wide-angle X-ray diffraction, and small-angle X-ray scattering were used to characterize the LC structure of both monomers and polymers. The electro-optic (EO) measurement was carried out by applying a triangular wave and measuring the LC EO response. SmCP (Smectic C indicates the LC molecules are tilted withmore » respect to the layer normal; P denotes polar ordering) phases were observed for both monomers and polymers. In LC monomers, typical antiferroelectric switching was observed. In the ground state, SmCP{sub A} (A denotes antiferroelectric) was observed which switched to SmCP{sub F} (F denotes ferroelectric) upon applying an electric field. In the corresponding LCP, a unique bilayer structure was observed, which is different from the reported BCLC bilayer SmCG (G denotes generated) phase. Most of the LCPs did not switch upon applying electric field while weak AF switching was observed in a low molecular weight poly{l_brace}3'-[4-(4-n-dodecyloxybenzoyloxy)benzoyloxy]-4-(12-acryloyloxydodecyloxy)benzoyloxybiphenyl{r_brace} sample.« less

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.

Probing the structure of heterogeneous diluted materials by diffraction tomography.

PubMed

Bleuet, Pierre; Welcomme, Eléonore; Dooryhée, Eric; Susini, Jean; Hodeau, Jean-Louis; Walter, Philippe

2008-06-01

The advent of nanosciences calls for the development of local structural probes, in particular to characterize ill-ordered or heterogeneous materials. Furthermore, because materials properties are often related to their heterogeneity and the hierarchical arrangement of their structure, different structural probes covering a wide range of scales are required. X-ray diffraction is one of the prime structural methods but suffers from a relatively poor detection limit, whereas transmission electron analysis involves destructive sample preparation. Here we show the potential of coupling pencil-beam tomography with X-ray diffraction to examine unidentified phases in nanomaterials and polycrystalline materials. The demonstration is carried out on a high-pressure pellet containing several carbon phases and on a heterogeneous powder containing chalcedony and iron pigments. The present method enables a non-invasive structural refinement with a weight sensitivity of one part per thousand. It enables the extraction of the scattering patterns of amorphous and crystalline compounds with similar atomic densities and compositions. Furthermore, such a diffraction-tomography experiment can be carried out simultaneously with X-ray fluorescence, Compton and absorption tomographies, enabling a multimodal analysis of prime importance in materials science, chemistry, geology, environmental science, medical science, palaeontology and cultural heritage.

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.

Small Angle X-ray Scattering for Nanoparticle Research

DOE PAGES

Li, Tao; Senesi, Andrew J.; Lee, Byeongdu

2016-04-07

X-ray scattering is a structural characterization tool that has impacted diverse fields of study. It is unique in its ability to examine materials in real time and under realistic sample environments, enabling researchers to understand morphology at nanometer and ångström length scales using complementary small and wide angle X-ray scattering (SAXS, WAXS), respectively. Herein, we focus on the use of SAXS to examine nanoscale particulate systems. We provide a theoretical foundation for X-ray scattering, considering both form factor and structure factor, as well as the use of correlation functions, which may be used to determine a particle’s size, size distribution,more » shape, and organization into hierarchal structures. The theory is expanded upon with contemporary use cases. Both transmission and reflection (grazing incidence) geometries are addressed, as well the combination of SAXS with other X-ray and non-X ray characterization tools. Furthermore, we conclude with an examination of several key areas of research where X-rays scattering has played a pivotal role, including in situ nanoparticle synthesis, nanoparticle assembly, and in operando studies of catalysts and energy storage materials. Throughout this review we highlight the unique capabilities of X-ray scattering for structural characterization of materials in their native environment.« less

Small Angle X-ray Scattering for Nanoparticle Research

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

Li, Tao; Senesi, Andrew J.; Lee, Byeongdu

X-ray scattering is a structural characterization tool that has impacted diverse fields of study. It is unique in its ability to examine materials in real time and under realistic sample environments, enabling researchers to understand morphology at nanometer and ångström length scales using complementary small and wide angle X-ray scattering (SAXS, WAXS), respectively. Herein, we focus on the use of SAXS to examine nanoscale particulate systems. We provide a theoretical foundation for X-ray scattering, considering both form factor and structure factor, as well as the use of correlation functions, which may be used to determine a particle’s size, size distribution,more » shape, and organization into hierarchal structures. The theory is expanded upon with contemporary use cases. Both transmission and reflection (grazing incidence) geometries are addressed, as well the combination of SAXS with other X-ray and non-X ray characterization tools. Furthermore, we conclude with an examination of several key areas of research where X-rays scattering has played a pivotal role, including in situ nanoparticle synthesis, nanoparticle assembly, and in operando studies of catalysts and energy storage materials. Throughout this review we highlight the unique capabilities of X-ray scattering for structural characterization of materials in their native environment.« less

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

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.

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.

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.

Wide-angle x-ray scattering and solid-state nuclear magnetic resonance data combined to test models for cellulose microfibrils in mung bean cell walls.

PubMed

Newman, Roger H; Hill, Stefan J; Harris, Philip J

2013-12-01

A synchrotron wide-angle x-ray scattering study of mung bean (Vigna radiata) primary cell walls was combined with published solid-state nuclear magnetic resonance data to test models for packing of (1→4)-β-glucan chains in cellulose microfibrils. Computer-simulated peak shapes, calculated for 36-chain microfibrils with perfect order or uncorrelated disorder, were sharper than those in the experimental diffractogram. Introducing correlated disorder into the models broaden the simulated peaks but only when the disorder was increased to unrealistic magnitudes. Computer-simulated diffractograms, calculated for 24- and 18-chain models, showed good fits to experimental data. Particularly good fits to both x-ray and nuclear magnetic resonance data were obtained for collections of 18-chain models with mixed cross-sectional shapes and occasional twinning. Synthesis of 18-chain microfibrils is consistent with a model for cellulose-synthesizing complexes in which three cellulose synthase polypeptides form a particle and six particles form a rosette.

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

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.

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.

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.

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.

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

Insight into Evolution, Processing and Performance of Multi-length-scale Structures in Planar Heterojunction Perovskite Solar Cells.

PubMed

Huang, Yu-Ching; Tsao, Cheng-Si; Cho, Yi-Ju; Chen, Kuan-Chen; Chiang, Kai-Ming; Hsiao, Sheng-Yi; Chen, Chang-Wen; Su, Chun-Jen; Jeng, U-Ser; Lin, Hao-Wu

2015-09-04

The structural characterization correlated to the processing control of hierarchical structure of planar heterojunction perovskite layer is still incomplete due to the limitations of conventional microscopy and X-ray diffraction. This present study performed the simultaneously grazing-incidence small-angle scattering and wide-angle scattering (GISAXS/GIWAXS) techniques to quantitatively probe the hierarchical structure of the planar heterojunction perovskite solar cells. The result is complementary to the currently microscopic study. Correlation between the crystallization behavior, crystal orientation, nano- and meso-scale internal structure and surface morphology of perovskite film as functions of various processing control parameters is reported for the first time. The structural transition from the fractal pore network to the surface fractal can be tuned by the chloride percentage. The GISAXS/GIWAXS measurement provides the comprehensive understanding of concurrent evolution of the film morphology and crystallization correlated to the high performance. The result can provide the insight into formation mechanism and rational synthesis design.

Insight into Evolution, Processing and Performance of Multi-length-scale Structures in Planar Heterojunction Perovskite Solar Cells

NASA Astrophysics Data System (ADS)

Huang, Yu-Ching; Tsao, Cheng-Si; Cho, Yi-Ju; Chen, Kuan-Chen; Chiang, Kai-Ming; Hsiao, Sheng-Yi; Chen, Chang-Wen; Su, Chun-Jen; Jeng, U.-Ser; Lin, Hao-Wu

2015-09-01

The structural characterization correlated to the processing control of hierarchical structure of planar heterojunction perovskite layer is still incomplete due to the limitations of conventional microscopy and X-ray diffraction. This present study performed the simultaneously grazing-incidence small-angle scattering and wide-angle scattering (GISAXS/GIWAXS) techniques to quantitatively probe the hierarchical structure of the planar heterojunction perovskite solar cells. The result is complementary to the currently microscopic study. Correlation between the crystallization behavior, crystal orientation, nano- and meso-scale internal structure and surface morphology of perovskite film as functions of various processing control parameters is reported for the first time. The structural transition from the fractal pore network to the surface fractal can be tuned by the chloride percentage. The GISAXS/GIWAXS measurement provides the comprehensive understanding of concurrent evolution of the film morphology and crystallization correlated to the high performance. The result can provide the insight into formation mechanism and rational synthesis design.

Molecular Organization of Cholesterol in Docosahexaenoate-Rich Lipid Bilayers

NASA Astrophysics Data System (ADS)

Wassall, Stephen R.; Brzustowicz, Michael R.; Cherezov, Vadim; Caffrey, Martin; Zerouga, Mustapha; Stillwell, William

2002-03-01

We investigated the molecular organization of cholesterol in 1,2-didocosahexaenoylphosphatidylcholine (22:6-22:6PC) and 1-stearoyl-2-docosahexaenoylphosphatidylcholine (18:0-22:6PC) bilayers. The solubility of the sterol measured by wide-angle x-ray diffraction was < 20 mol% in 22:6-22:6PC bilayers which contrasts with > 50 mol% in 18:0-22:6PC. Solid state ^2H NMR of [3α-^2H_1]cholesterol suggests that the reduction in solubility correlates with a larger tilt angle α0 = 24^o for the steroid moiety in 22:6-22:6PC bilayers than in 18:0-22:6PC where α0 < 24^o. We attribute the low solubility of cholesterol in 22:6-22:6PC membranes to steric incompatibility between the rigid steroid moiety and the highly polyunsaturated docosahexaenoic acid (DHA) chain, which has the potential to promote lateral heterogeneity within neural membranes rich in DHA and has implications for receptor activation.

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.

Laboratory and In-Flight In-Situ X-ray Imaging and Scattering Facility for Materials, Biotechnology and Life Sciences

NASA Technical Reports Server (NTRS)

2003-01-01

We propose a multifunctional X-ray facility for the Materials, Biotechnology and Life Sciences Programs to visualize formation and behavior dynamics of materials, biomaterials, and living organisms, tissues and cells. The facility will combine X-ray topography, phase micro-imaging and scattering capabilities with sample units installed on the goniometer. This should allow, for the first time, to monitor under well defined conditions, in situ, in real time: creation of imperfections during growth of semiconductors, metal, dielectric and biomacromolecular crystals and films, high-precision diffraction from crystals within a wide range of temperatures and vapor, melt, solution conditions, internal morphology and changes in living organisms, tissues and cells, diffraction on biominerals, nanotubes and particles, radiation damage, also under controlled formation/life conditions. The system will include an ultrabright X-ray source, X-ray mirror, monochromator, image-recording unit, detectors, and multipurpose diffractometer that fully accommodate and integrate furnaces and samples with other experimental environments. The easily adjustable laboratory and flight versions will allow monitoring processes under terrestrial and microgravity conditions. The flight version can be made available using a microsource combined with multilayer or capillary optics.

A small-angle neutron scattering study of the kinetics of phase separation in a supersaturated Ni-12.5 at. pct Si alloy

NASA Astrophysics Data System (ADS)

Polat, S.; Chen, Haydn; Epperson, J. E.

1989-04-01

The kinetic behavior of precipitation in a supersaturated Ni-12.5 at. pct Si alloy single crystal has been studied by the small-angle neutron scattering (SANS) technique to supplement earlier transmission electron microscopy (TEM) and wide-angle X-ray diffraction (XRD) work. The SANS measurements performed at room temperature on quenched specimens subjected to isothermal anneals at 400, 450, 505, and 550 °C for various amounts of time have revealed the presence of an interference peak in the scattering function. The particle size, determined according to the Guinier approximation, is found to grow in accordance with the diffusion controlled model put forth by Lifshitz and Slyozov, and independently by Wagner. The activation energy for solute diffusion is determined using the rate constants governing the growth of particle size and the variation of the mean interparticle distance. Results are in agreement with the values given in the literature. Transition from an earlier growth stage has been observed, and enhanced diffusion is noted at temperatures below 505 °C; both observations are consistent with the previous X-ray results. The dynamical scaling law appears to be followed by the data obtained in the coarsening stage. A disruption of scaling occurs at the point when the particle growth changes from a parabolic rate behavior to a cubic coarsening rate. Dynamical scaling offers the potential for projecting the service lifetimes for components from experimental measurements carried out over a much shorter time interval. Discrepancies in the size parameters determined by different techniques are discussed.

In situ X-ray powder diffraction studies of the synthesis of graphene oxide and formation of reduced graphene oxide

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

Storm, Mie Møller, E-mail: mmst@dtu.dk; Johnsen, Rune E.; Norby, Poul

2016-08-15

Graphene oxide (GO) and reduced graphene oxide (rGO) are important materials in a wide range of fields. The modified Hummers methods, for synthesizing GO, and subsequent thermal reduction to rGO, are often employed for production of rGO. However, the mechanism behinds these syntheses methods are still unclear. We present an in situ X-ray diffraction study of the synthesis of GO and thermal reduction of GO. The X-ray diffraction revealed that the Hummers method includes an intercalation state and finally formation of additional crystalline material. The formation of GO is observed during both the intercalation and the crystallization stage. During thermalmore » reduction of GO three stages were observed: GO, a disordered stage, and the rGO stage. The appearance of these stages depends on the heating ramp. The aim of this study is to provide deeper insight into the chemical and physical processes during the syntheses. - Graphical abstract: In situ X-ray diffraction results for of the modified Hummers synthesis and the thermal reduction of graphene oxide, revealing three stages for both syntheses as well as new GO diffraction peaks and unidentified crystalline material for the Hummers synthesis and a disordered stage for the thermal reduction of graphene oxide. Display Omitted - Highlights: • Hummers synthesis consists of three stages: dissolution, intercalation and crystal. • GO is produced early on during the synthesis and display new diffraction peaks. • An unidentified triclinic phase is observed for the Hummers synthesis. • Thermal reduction of GO display three stages: GO, a disordered stage and rGO. • In situ XRD indicate reformation of rGO even for fast heated thermal reduction.« less

High-pressure studies with x-rays using diamond anvil cells

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

Shen, Guoyin; Mao, Ho Kwang

2016-11-22

Pressure profoundly alters all states of matter. The symbiotic development of ultrahigh-pressure diamond anvil cells, to compress samples to sustainable multi-megabar pressures; and synchrotron x-ray techniques, to probe materials' properties in situ, has enabled the exploration of rich high-pressure (HP) science. In this article, we first introduce the essential concept of diamond anvil cell technology, together with recent developments and its integration with other extreme environments. We then provide an overview of the latest developments in HP synchrotron techniques, their applications, and current problems, followed by a discussion of HP scientific studies using x-rays in the key multidisciplinary fields. Thesemore » HP studies include: HP x-ray emission spectroscopy, which provides information on the filled electronic states of HP samples; HP x-ray Raman spectroscopy, which probes the HP chemical bonding changes of light elements; HP electronic inelastic x-ray scattering spectroscopy, which accesses high energy electronic phenomena, including electronic band structure, Fermi surface, excitons, plasmons, and their dispersions; HP resonant inelastic x-ray scattering spectroscopy, which probes shallow core excitations, multiplet structures, and spin-resolved electronic structure; HP nuclear resonant x-ray spectroscopy, which provides phonon densities of state and time-resolved Mössbauer information; HP x-ray imaging, which provides information on hierarchical structures, dynamic processes, and internal strains; HP x-ray diffraction, which determines the fundamental structures and densities of single-crystal, polycrystalline, nanocrystalline, and non-crystalline materials; and HP radial x-ray diffraction, which yields deviatoric, elastic and rheological information. Integrating these tools with hydrostatic or uniaxial pressure media, laser and resistive heating, and cryogenic cooling, has enabled investigations of the structural, vibrational, electronic, and magnetic properties of materials over a wide range of pressure-temperature conditions.« less

High-pressure studies with x-rays using diamond anvil cells

NASA Astrophysics Data System (ADS)

Shen, Guoyin; Mao, Ho Kwang

2017-01-01

Pressure profoundly alters all states of matter. The symbiotic development of ultrahigh-pressure diamond anvil cells, to compress samples to sustainable multi-megabar pressures; and synchrotron x-ray techniques, to probe materials’ properties in situ, has enabled the exploration of rich high-pressure (HP) science. In this article, we first introduce the essential concept of diamond anvil cell technology, together with recent developments and its integration with other extreme environments. We then provide an overview of the latest developments in HP synchrotron techniques, their applications, and current problems, followed by a discussion of HP scientific studies using x-rays in the key multidisciplinary fields. These HP studies include: HP x-ray emission spectroscopy, which provides information on the filled electronic states of HP samples; HP x-ray Raman spectroscopy, which probes the HP chemical bonding changes of light elements; HP electronic inelastic x-ray scattering spectroscopy, which accesses high energy electronic phenomena, including electronic band structure, Fermi surface, excitons, plasmons, and their dispersions; HP resonant inelastic x-ray scattering spectroscopy, which probes shallow core excitations, multiplet structures, and spin-resolved electronic structure; HP nuclear resonant x-ray spectroscopy, which provides phonon densities of state and time-resolved Mössbauer information; HP x-ray imaging, which provides information on hierarchical structures, dynamic processes, and internal strains; HP x-ray diffraction, which determines the fundamental structures and densities of single-crystal, polycrystalline, nanocrystalline, and non-crystalline materials; and HP radial x-ray diffraction, which yields deviatoric, elastic and rheological information. Integrating these tools with hydrostatic or uniaxial pressure media, laser and resistive heating, and cryogenic cooling, has enabled investigations of the structural, vibrational, electronic, and magnetic properties of materials over a wide range of pressure-temperature conditions.

Sensitivity and Limitations of Structures from X-ray and Neutron-Based Diffraction Analyses of Transition Metal Oxide Lithium-Battery Electrodes

DOE PAGES

Liu, Hao; Liu, Haodong; Lapidus, Saul H.; ...

2017-06-21

Lithium transition metal oxides are an important class of electrode materials for lithium-ion batteries. Binary or ternary (transition) metal doping brings about new opportunities to improve the electrode’s performance and often leads to more complex stoichiometries and atomic structures than the archetypal LiCoO 2. Rietveld structural analyses of X-ray and neutron diffraction data is a widely-used approach for structural characterization of crystalline materials. But, different structural models and refinement approaches can lead to differing results, and some parameters can be difficult to quantify due to the inherent limitations of the data. Here, through the example of LiNi 0.8Co 0.15Al 0.05Omore » 2 (NCA), we demonstrated the sensitivity of various structural parameters in Rietveld structural analysis to different refinement approaches and structural models, and proposed an approach to reduce refinement uncertainties due to the inexact X-ray scattering factors of the constituent atoms within the lattice. Furthermore, this refinement approach was implemented for electrochemically-cycled NCA samples and yielded accurate structural parameters using only X-ray diffraction data. The present work provides the best practices for performing structural refinement of lithium transition metal oxides.« less

Sensitivity and Limitations of Structures from X-ray and Neutron-Based Diffraction Analyses of Transition Metal Oxide Lithium-Battery Electrodes

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

Liu, Hao; Liu, Haodong; Lapidus, Saul H.

Lithium transition metal oxides are an important class of electrode materials for lithium-ion batteries. Binary or ternary (transition) metal doping brings about new opportunities to improve the electrode’s performance and often leads to more complex stoichiometries and atomic structures than the archetypal LiCoO 2. Rietveld structural analyses of X-ray and neutron diffraction data is a widely-used approach for structural characterization of crystalline materials. But, different structural models and refinement approaches can lead to differing results, and some parameters can be difficult to quantify due to the inherent limitations of the data. Here, through the example of LiNi 0.8Co 0.15Al 0.05Omore » 2 (NCA), we demonstrated the sensitivity of various structural parameters in Rietveld structural analysis to different refinement approaches and structural models, and proposed an approach to reduce refinement uncertainties due to the inexact X-ray scattering factors of the constituent atoms within the lattice. Furthermore, this refinement approach was implemented for electrochemically-cycled NCA samples and yielded accurate structural parameters using only X-ray diffraction data. The present work provides the best practices for performing structural refinement of lithium transition metal oxides.« less

Simultaneous nanocalorimetry and fast XRD measurements to study the silicide formation in Pd/a-Si bilayers.

PubMed

Molina-Ruiz, Manel; Ferrando-Villalba, Pablo; Rodríguez-Tinoco, Cristian; Garcia, Gemma; Rodríguez-Viejo, Javier; Peral, Inma; Lopeandía, Aitor F

2015-05-01

The use of a membrane-based chip nanocalorimeter in a powder diffraction beamline is described. Simultaneous wide-angle X-ray scattering and scanning nanocalorimetric measurements are performed on a thin-film stack of palladium/amorphous silicon (Pd/a-Si) at heating rates from 0.1 to 10 K s(-1). The nanocalorimeter works under a power-compensation scheme previously developed by the authors. Kinetic and structural information of the consumed and created phases can be obtained from the combined techniques. The formation of Pd2Si produces a broad calorimetric peak that contains overlapping individual processes. It is shown that Pd consumption precedes the formation of the crystalline Pd2Si phase and that the crystallite size depends on the heating rate of the experiment.

Influence of the anions on the N-cationic benzethonium salts in the solid state and solution: Chloride, bromide, hydroxide and citrate hydrates

NASA Astrophysics Data System (ADS)

Paradies, Henrich H.; Reichelt, Hendrik

2016-06-01

The crystal structures of the hydrated cationic surfactant benzethonium (Bzth) chloride, bromide, hydroxide, and citrate have been determined by X-ray diffraction analysis and compared with their structures in solution well above their critical micelle concentration. The differences in the nature of the various anions of the four Bzth-X materials lead to unique anion environments and 3-D molecular arrangements. The water molecule in the monoclinic Bzth-Cl or Bzth-Br forms is hydrogen bonded to the halides and particularly to the hydrogens of the methoxy groups of the Bzth moiety notwithstanding the weak Brønsted acidity of the methoxy hydrogens. The citrate strongly interacts with the hydrogens of the methoxy group forming an embedded anionic spherical cluster of a radius of 2.6 Å. The Bzth-OH crystallizes in a hexagonal lattice with two water molecules and reveals free water molecules forming hydrogen bonded channels through the Bzth-OH crystal along the c-axis. The distances between the cationic nitrogen and the halides are 4.04 Å and 4.20 Å, significantly longer than expected for typical van der Waals distances of 3.30 Å. The structures show weakly interacting, alternating apolar and polar layers, which run parallel to the crystallographic a-b planes or a-c planes. The Bzth-X salts were also examined in aqueous solution containing 20% (v/v) ethanol and 1.0 % (v/v) glycerol well above their critical micelle concentration by small-angle X-ray scattering (SAXS) and wide-angle X-ray scattering (WAXS). The [1,1,1] planes for the Bzth Cl or Br, the [0,0,2] and [1,1,0] planes for the Bzth-citrate, the [2,-1,0] planes and the [0,0,1] planes for the Bzth-OH found in the crystalline phase were also present in the solution phase, accordingly, the preservation of these phases are a strong indication of periodicity in the solution phase.

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

Expression, purification and preliminary X-ray diffraction studies of the transcriptional factor PyrR from Bacillus halodurans

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

Arreola, Rodrigo; Vega-Miranda, Anita; Gómez-Puyou, Armando

The gene-regulation factor PyrR from B. halodurans has been crystallized in two crystal forms. Preliminary crystallographic analysis showed that the protein forms tetramers in both space groups. The PyrR transcriptional regulator is widely distributed in bacteria. This RNA-binding protein is involved in the control of genes involved in pyrimidine biosynthesis, in which uridyl and guanyl nucleotides function as effectors. Here, the crystallization and preliminary X-ray diffraction analysis of two crystal forms of Bacillus halodurans PyrR are reported. One of the forms belongs to the monoclinic space group P2{sub 1} with unit-cell parameters a = 59.7, b = 87.4, c =more » 72.1 Å, β = 104.4°, while the other form belongs to the orthorhombic space group P22{sub 1}2{sub 1} with unit-cell parameters a = 72.7, b = 95.9, c = 177.1 Å. Preliminary X-ray diffraction data analysis and molecular-replacement solution revealed the presence of four and six monomers per asymmetric unit; a crystallographic tetramer is formed in both forms.« less

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

Synchrotron WAXS and XANES studies of silica (SiO2) powders synthesized from Indonesian natural sands

NASA Astrophysics Data System (ADS)

Muchlis, Khairanissa; Aini Fauziyah, Nur; Soontaranon, Siriwat; Limpirat, Wanwisa; Pratapa, Suminar

2017-01-01

In this study, we have investigated polymorphic silica (SiO2) powders using, Wide Angle X-ray Scattering (WAXS) and X-Ray Absorption Near Edge Spectroscopy (XANES), laboratory X-Ray Diffraction (XRD) instruments. The WAXS and XANES spectra were collected using synchrotron radiation at Synchrotron Light Research Institute (SLRI), Nakhon Ratchasima, Thailand. The silica powders were obtained by processing silica sand from Tanah Laut, South Kalimantan, Indonesia. Purification process of silica sand was done by magnetic separation and immersion with HCl. The purification step was needed to reduce impurity or undesirable non Si elements. Three polymorphs of silica were produced, i.e. amorphous phase (A), quartz (B), and cristobalite (C). WAXS profile for each phase was presented in terms of intensity vs. 2θ prior to analyses. Both XRD (λCuKα=1.54056 Å) and WAXS (λ=1.09 Å) patttern show that (1) A sample contains no crystallites, (2) B sample is monophasic, contains only quartz, and (3) C sample contains cristobalite and trydimite. XRD quantitative analysis using Rietica gave 98,8 wt% cristobalite, while the associated WAXS data provided 98.7 wt% cristobalite. Si K-edge XANES spectra were measured at energy range 1840 to 1920 eV. Qualitatively, the pre-edge and edge features for all phases are similar, but their main peaks in the post-edge region are different.

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.

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

High pressure single-crystal micro X-ray diffraction analysis with GSE_ADA/RSV software

NASA Astrophysics Data System (ADS)

Dera, Przemyslaw; Zhuravlev, Kirill; Prakapenka, Vitali; Rivers, Mark L.; Finkelstein, Gregory J.; Grubor-Urosevic, Ognjen; Tschauner, Oliver; Clark, Simon M.; Downs, Robert T.

2013-08-01

GSE_ADA/RSV is a free software package for custom analysis of single-crystal micro X-ray diffraction (SCμXRD) data, developed with particular emphasis on data from samples enclosed in diamond anvil cells and subject to high pressure conditions. The package has been in extensive use at the high pressure beamlines of Advanced Photon Source (APS), Argonne National Laboratory and Advanced Light Source (ALS), Lawrence Berkeley National Laboratory. The software is optimized for processing of wide-rotation images and includes a variety of peak intensity corrections and peak filtering features, which are custom-designed to make processing of high pressure SCμXRD easier and more reliable.

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.

Graphene-based microfluidics for serial crystallography.

PubMed

Sui, Shuo; Wang, Yuxi; Kolewe, Kristopher W; Srajer, Vukica; Henning, Robert; Schiffman, Jessica D; Dimitrakopoulos, Christos; Perry, Sarah L

2016-08-02

Microfluidic strategies to enable the growth and subsequent serial crystallographic analysis of micro-crystals have the potential to facilitate both structural characterization and dynamic structural studies of protein targets that have been resistant to single-crystal strategies. However, adapting microfluidic crystallization platforms for micro-crystallography requires a dramatic decrease in the overall device thickness. We report a robust strategy for the straightforward incorporation of single-layer graphene into ultra-thin microfluidic devices. This architecture allows for a total material thickness of only ∼1 μm, facilitating on-chip X-ray diffraction analysis while creating a sample environment that is stable against significant water loss over several weeks. We demonstrate excellent signal-to-noise in our X-ray diffraction measurements using a 1.5 μs polychromatic X-ray exposure, and validate our approach via on-chip structure determination using hen egg white lysozyme (HEWL) as a model system. Although this work is focused on the use of graphene for protein crystallography, we anticipate that this technology should find utility in a wide range of both X-ray and other lab on a chip applications.

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

Nanospheres with a smectic hydrophobic core and an amorphous PEG hydrophilic shell: structural changes and implications for drug delivery

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

Murthy, N. Sanjeeva; Zhang, Zheng; Borsadia, Siddharth

The structural changes in nanospheres with a crystalline core and an amorphous diffuse shell were investigated by small-angle neutron scattering (SANS), small-, medium-, and wide-angle X-ray scattering (SAXS, MAXS and WAXS), and differential scanning calorimetry (DSC).

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.

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

The ASTRO-H SXT Performance to the Large Off-Set Angles

NASA Technical Reports Server (NTRS)

Sato, Toshiki; Iizuka, Ryo; Mori, Hideyuki; Hayashi, Takayuki; Maeda, Yoshitomo; Ishida, Manabu; Kikuchi, Naomichi; Kurashima, Sho; Nakaniwa, Nozomi; Okajima, Takashi;

Difference structures from time-resolved small-angle and wide-angle x-ray scattering

NASA Astrophysics Data System (ADS)

Nepal, Prakash; Saldin, D. K.

2018-05-01

Time-resolved small-angle x-ray scattering/wide-angle x-ray scattering (SAXS/WAXS) is capable of recovering difference structures directly from difference SAXS/WAXS curves. It does so by means of the theory described here because the structural changes in pump-probe detection in a typical time-resolved experiment are generally small enough to be confined to a single residue or group in close proximity which is identified by a method akin to the difference Fourier method of time-resolved crystallography. If it is assumed, as is usual with time-resolved structures, that the moved atoms lie within the residue, the 100-fold reduction in the search space (assuming a typical protein has about 100 residues) allows the exaction of the structure by a simulated annealing algorithm with a huge reduction in computing time and leads to a greater resolution by varying the positions of atoms only within that residue. This reduction in the number of potential moved atoms allows us to identify the actual motions of the individual atoms. In the case of a crystal, time-resolved calculations are normally performed using the difference Fourier method, which is, of course, not directly applicable to SAXS/WAXS. The method developed in this paper may be thought of as a substitute for that method which allows SAXS/WAXS (and hence disordered molecules) to also be used for time-resolved structural work.

A Unified Model for Tidal Disruption Events

NASA Astrophysics Data System (ADS)

Dai, Lixin; McKinney, Jonathan C.; Roth, Nathaniel; Ramirez-Ruiz, Enrico; Miller, M. Coleman

2018-06-01

In the past few years wide-field optical and UV transient surveys and X-ray telescopes have allowed us to identify a few dozen candidate tidal disruption events (TDEs). While in theory the physical processes in TDEs are ubiquitous, a few distinct classes of TDEs have been observed. Some TDEs radiate mainly in NUV/optical, while others produce prominent X-rays. Moreover, relativistic jets have been observed in only a handful of TDEs. This diversity might be related to the details of the super-Eddington accretion and emission physics relevant to TDE disks. In this Letter, we utilize novel three-dimensional general relativistic radiation magnetohydrodynamics simulations to study the super-Eddington compact disk phase expected in TDEs. Consistent with previous studies, geometrically thick disks, wide-angle optically thick fast outflows, and relativistic jets are produced. The outflow density and velocity depend sensitively on the inclination angle, and hence so does the reprocessing of emission produced from the inner disk. We then use Monte Carlo radiative transfer to calculate the reprocessed spectra and find that that the observed ratio of optical to X-ray fluxes increases with increasing inclination angle. This naturally leads to a unified model for different classes of TDEs in which the spectral properties of the TDE depend mainly on the viewing angle of the observer with respect to the orientation of the disk.

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

Microstructural Parameters in 8 MeV Electron-Irradiated BOMBYX MORI Silk Fibers by Wide-ANGLE X-Ray Scattering Studies (waxs)

NASA Astrophysics Data System (ADS)

Sangappa, Asha, S.; Sanjeev, Ganesh; Subramanya, G.; Parameswara, P.; Somashekar, R.

2010-01-01

The present work looks into the microstructural modification in electron irradiated Bombyx mori P31 silk fibers. The irradiation process was performed in air at room temperature using 8 MeV electron accelerator at different doses: 0, 25, 50 and 100 kGy. Irradiation of polymer is used to cross-link or degrade the desired component or to fix the polymer morphology. The changes in microstructural parameters in these natural polymer fibers have been computed using wide angle X-ray scattering (WAXS) data and employing line profile analysis (LPA) using Fourier transform technique of Warren. Exponential, Lognormal and Reinhold functions for the column length distributions have been used for the determination of crystal size, lattice strain and enthalpy parameters.

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.

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.

Specific features of two diffraction schemes for a widely divergent X-ray beam

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

Avetyan, K. T.; Levonyan, L. V.; Semerjian, H. S.

2015-03-15

We investigated the specific features of two diffraction schemes for a widely divergent X-ray beam that use a circular diaphragm 30–50 μm in diameter as a point source of characteristic radiation. In one of the schemes, the diaphragm was set in front of the crystal (the diaphragm-crystal (d-c) scheme); in the other, it was installed behind the crystal (the crystal-diaphragm (c-d) scheme). It was established that the diffraction image in the c-d scheme is a topographic map of the investigated crystal area. In the d-c scheme at L = 2l (l and L are the distances between the crystal andmore » the diaphragm and between the photographic plate and the diaphragm, respectively), the branches of hyperbolas formed in this family of planes (hkl) by the characteristic K{sub α} and K{sub β} radiations, including higher order reflections, converge into one straight line. It is experimentally demonstrated that this convergence is very sensitive to structural inhomogeneities in the crystal under study.« less

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.

Using X-ray Thomson Scattering to Characterize Highly Compressed, Near-Degenerate Plasmas at the NIF

NASA Astrophysics Data System (ADS)

Doeppner, Tilo; Kraus, D.; Neumayer, P.; Bachmann, B.; Divol, L.; Kritcher, A. L.; Landen, O. L.; Fletcher, L.; Glenzer, S. H.; Falcone, R. W.; MacDonald, M. J.; Saunders, A.; Witte, B.; Redmer, R.; Chapman, D.; Baggott, R.; Gericke, D. O.; Yi, S. A.

2017-10-01

We are developing x-ray Thomson scattering for implosion experiments at the National Ignition Facility to characterize plasma conditions in plastic and beryllium capsules near stagnation, reaching more than 20x compression and electron densities of 1025 cm-3, corresponding to a Fermi energy of 170 eV. Using a zinc He- α x-ray source at 9 keV, experiments at a large scattering angle of 120° measure non-collective scattering spectra with high sensitivity to K-shell ionization, and find higher charge states than predicted by widely used ionization models. Reducing the scattering angle to 30° probes the collective scattering regime with sensitivity to collisions and conductivity. We will discuss recent results and future plans. This work was performed under the auspices of the US Department of Energy by Lawrence Livermore National Laboratory under Contract DE-AC52-07NA27344.

DISTRIBUTION SYSTEM SOLIDS - A RESEARCH APPROACH

EPA Science Inventory

The U.S. EPA's AWBERC research facility is equipped with capabilities to analyze a variety of solids in support many Laboratory-wide research studies. Techniques available on site include X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microsco...

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.

Analysis of doping concentration and composition in wide bandgap AlGaN:Si by wavelength dispersive x-ray spectroscopy

NASA Astrophysics Data System (ADS)

Kusch, Gunnar; Mehnke, Frank; Enslin, Johannes; Edwards, Paul R.; Wernicke, Tim; Kneissl, Michael; Martin, Robert W.

2017-03-01

Detailed knowledge of the dopant concentration and composition of wide band gap Al x Ga{}1-x{{N}} layers is of crucial importance for the fabrication of ultra violet light emitting diodes. This paper demonstrates the capabilities of wavelength dispersive x-ray (WDX) spectroscopy in accurately determining these parameters and compares the results with those from high resolution x-ray diffraction (HR-XRD) and secondary ion mass spectrometry (SIMS). WDX spectroscopy has been carried out on different silicon-doped wide bandgap Al x Ga{}1-x{{N}} samples (x between 0.80 and 1). This study found a linear increase in the Si concentration with the SiH4/group-III ratio, measuring Si concentrations between 3× {10}18 cm-3 and 2.8× {10}19 cm-3, while no direct correlation between the AlN composition and the Si incorporation ratio was found. Comparison between the composition obtained by WDX and by HR-XRD showed very good agreement in the range investigated, while comparison of the donor concentration between WDX and SIMS found only partial agreement, which we attribute to a number of effects.

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.

Soft x-ray holographic tomography for biological specimens

NASA Astrophysics Data System (ADS)

Gao, Hongyi; Chen, Jianwen; Xie, Honglan; Li, Ruxin; Xu, Zhizhan; Jiang, Shiping; Zhang, Yuxuan

2003-10-01

In this paper, we present some experimental results on X -ray holography, holographic tomography, and a new holographic tomography method called pre-amplified holographic tomography is proposed. Due to the shorter wavelength and the larger penetration depths, X-rays provide the potential of higher resolution in imaging techniques, and have the ability to image intact, living, hydrated cells w ithout slicing, dehydration, chemical fixation or stain. Recently, using X-ray source in National Synchrotron Radiation Laboratory in Hefei, we have successfully performed some soft X-ray holography experiments on biological specimen. The specimens used in the experiments was the garlic clove epidermis, we got their X-ray hologram, and then reconstructed them by computer programs, the feature of the cell walls, the nuclei and some cytoplasm were clearly resolved. However, there still exist some problems in realization of practical 3D microscopic imaging due to the near-unity refractive index of the matter. There is no X-ray optics having a sufficient high numerical aperture to achieve a depth resolution that is comparable to the transverse resolution. On the other hand, computer tomography needs a record of hundreds of views of the test object at different angles for high resolution. This is because the number of views required for a densely packed object is equal to the object radius divided by the desired depth resolution. Clearly, it is impractical for a radiation-sensitive biological specimen. Moreover, the X-ray diffraction effect makes projection data blur, this badly degrades the resolution of the reconstructed image. In order to observe 3D structure of the biological specimens, McNulty proposed a new method for 3D imaging called "holographic tomography (HT)" in which several holograms of the specimen are recorded from various illumination directions and combined in the reconstruction step. This permits the specimens to be sampled over a wide range of spatial frequencies to improve the depth resolution. In NSRL, we performed soft X-ray holographic tomography experiments. The specimen was the spider filaments and PM M A as recording medium. By 3D CT reconstruction of the projection data, three dimensional density distribution of the specimen was obtained. Also, we developed a new X-ray holographic tomography m ethod called pre-amplified holographic tomography. The method permits a digital real-time 3D reconstruction with high-resolution and a simple and compact experimental setup as well.

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

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.

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.

Collagen insulated from tensile damage by domains that unfold reversibly: in situ X-ray investigation of mechanical yield and damage repair in the mussel byssus

PubMed Central

Harrington, Matthew J.; Gupta, Himadri S.; Fratzl, Peter; Waite, J. Herbert

2009-01-01

The byssal threads of the California mussel, Mytilus californianus, are highly hysteretic, elastomeric fibers that collectively perform a holdfast function in wave-swept rocky seashore habitats. Following cyclic loading past the mechanical yield point, threads exhibit a damage-dependent reduction in mechanical performance. However, the distal portion of the byssal thread is capable of recovering initial material properties through a time-dependent healing process in the absence of active cellular metabolism. Byssal threads are composed almost exclusively of multi-domain hybrid collagens known as preCols, which largely determine the mechanical properties of the thread. Here, the structure-property relationships that govern thread mechanical performance are further probed. The molecular rearrangements that occur during yield and damage repair were investigated using time-resolved in situ wide angle X-ray diffraction (WAXD) coupled with cyclic tensile loading of threads and through thermally enhanced damage-repair studies. Results indicate that the collagen domains in byssal preCols are mechanically protected by the unfolding of sacrificial non-collagenous domains that refold on a slower time-scale. Time-dependent healing is primarily attributed to stochastic recoupling of broken histidine-metal coordination complexes. PMID:19275941

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

Stiubianu, George, E-mail: george.stiubianu@icmpp.ro; Bele, Adrian; Cazacu, Maria

Highlights: • Composite ceramics nanoparticles (MCN) with zirconium dioxide and lead zirconate. • Dielectric elastomer films wDith PDMS matrix and MCN as dielectric filler. • Hydrophobic character—water resistant and good flexibility specific to siloxanes. • Increased value of dielectric constant with the content of MCN in dielectric films. • Increased energy output from uniaxial deformation of the dielectric elastomer films. - Abstract: A ceramic material consisting in a zirconium dioxide-lead zirconate mixture has been obtained by precipitation method, its composition being proved by wide angle X-ray powder diffraction and energy-dispersive X-ray spectroscopy. The average diameter of the ceramic particles rangedmore » between 50 and 100 nm, as revealed by transmission electron microscopy images. These were surface treated and used as filler for a high molecular mass polydimethylsiloxane-α,ω-diol (Mn = 450,000) prepared in laboratory, the resulted composites being further processed as films and crosslinked. A condensation procedure, unusual for polydimethylsiloxane having such high molecular mass, with a trifunctional silane was approached for the crosslinking. The effect of filler content on electrical and mechanical properties of the resulted materials was studied and it was found that the dielectric permittivity of nanocomposites increased in line with the concentration of ceramic nanoparticles.« less

Nanostructured Black Phosphorus/Ketjenblack-Multiwalled Carbon Nanotubes Composite as High Performance Anode Material for Sodium-Ion Batteries.

PubMed

Xu, Gui-Liang; Chen, Zonghai; Zhong, Gui-Ming; Liu, Yuzi; Yang, Yong; Ma, Tianyuan; Ren, Yang; Zuo, Xiaobing; Wu, Xue-Hang; Zhang, Xiaoyi; Amine, Khalil

2016-06-08

Sodium-ion batteries are promising alternatives to lithium-ion batteries for large-scale applications. However, the low capacity and poor rate capability of existing anodes for sodium-ion batteries are bottlenecks for future developments. Here, we report a high performance nanostructured anode material for sodium-ion batteries that is fabricated by high energy ball milling to form black phosphorus/Ketjenblack-multiwalled carbon nanotubes (BPC) composite. With this strategy, the BPC composite with a high phosphorus content (70 wt %) could deliver a very high initial Coulombic efficiency (>90%) and high specific capacity with excellent cyclability at high rate of charge/discharge (∼1700 mAh g(-1) after 100 cycles at 1.3 A g(-1) based on the mass of P). In situ electrochemical impedance spectroscopy, synchrotron high energy X-ray diffraction, ex situ small/wide-angle X-ray scattering, high resolution transmission electronic microscopy, and nuclear magnetic resonance were further used to unravel its superior sodium storage performance. The scientific findings gained in this work are expected to serve as a guide for future design on high performance anode material for sodium-ion batteries.

Diffusion and Binding of Laponite Clay Nanoparticles into Collagen Fibers for the Formation of Leather Matrix.

PubMed

Shi, Jiabo; Wang, Chunhua; Ngai, To; Lin, Wei

2018-06-13

Understanding accessibility and interactions of clay nanoparticles with collagen fibers is an important fundamental issue for the conversion of collagen to leather matrix. In this study, we have investigated the diffusion and binding of Laponite into the collagen fiber network. Our results indicate that the diffusion behaviors of Laponite into the collagen exhibit the Langmuir adsorption, verifying its affinity for collagen. The introduction of Laponite leads to a shift in the isoelectric point of collagen from ∼6.8 to ∼4.5, indicating the ionic bonding between the positively charged amino groups of the collagen and negatively charged Laponite under the tanning conditions. Fluorescence microscopy, atomic force microscopy, field-emission scanning electron microscopy, energy-dispersive X-ray spectroscopy, and wide-angle X-ray diffraction analyses reveal that Laponite nanoparticles can penetrate into collagen microstructure and evenly distributed onto collagen fibrils, not altering native D-periodic banding patterns of collagen fibrils. Attenuated total reflectance-Fourier transform infrared and Raman spectroscopy detections further demonstrate the presence of noncovalent interactions, namely, ionic and hydrogen bonding, between Laponite and collagen. These findings provide a theoretical basis for the use of Laponite as an emerging tanning agent in leather manufacture.

Synthesis of superhydrophobic ultralight aerogels from nanofibrillated cellulose isolated from natural reed for high-performance adsorbents

NASA Astrophysics Data System (ADS)

Jiao, Yue; Wan, Caichao; Qiang, Tiangang; Li, Jian

2016-07-01

Reed is one of the widely available aquatic plant resources, and its applications are generally limited to some traditional areas like papermaking and animals' fodder. Besides, most of reed is wasted or directly burned every year causing serious air pollution (like atmospheric haze). Therefore, it is worth to further develop new forms of high-value applications of reed. Herein, natural reed was collected to fabricate ultralight adsorbents namely nanofibrillated cellulose (NFC) aerogels via an easily operated method, which includes chemical purification, ultrasonication, and freeze drying. The NFC aerogels with an ultra-low density of 4.9 mg cm-3 were characterized by scanning electron microscopy, energy-dispersive X-ray spectrometer, Fourier transform infrared spectroscopy, X-ray diffraction, and thermogravimetric analysis. For acquiring good hydrophobicity, the NFC aerogels were subjected to a hydrophobic treatment by methyltrichlorosilane. The superhydrophobic NFC aerogels with contact angles of as high as 151°-155° have excellent adsorption efficiency (53-93 g g-1) for various organic solvents and waste oil. More importantly, the aerogels also exhibit favorable adsorption recyclability, which can maintain more than 80 % of the initial adsorption efficiency after the five cycles.

Extending the Utility of the Parabolic Approximation in Medical Ultrasound Using Wide-Angle Diffraction Modeling.

PubMed

Soneson, Joshua E

2017-04-01

Wide-angle parabolic models are commonly used in geophysics and underwater acoustics but have seen little application in medical ultrasound. Here, a wide-angle model for continuous-wave high-intensity ultrasound beams is derived, which approximates the diffraction process more accurately than the commonly used Khokhlov-Zabolotskaya-Kuznetsov (KZK) equation without increasing implementation complexity or computing time. A method for preventing the high spatial frequencies often present in source boundary conditions from corrupting the solution is presented. Simulations of shallowly focused axisymmetric beams using both the wide-angle and standard parabolic models are compared to assess the accuracy with which they model diffraction effects. The wide-angle model proposed here offers improved focusing accuracy and less error throughout the computational domain than the standard parabolic model, offering a facile method for extending the utility of existing KZK codes.

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.

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.

Effect of reflection and refraction on NEXAFS spectra measured in TEY mode

PubMed Central

2018-01-01

The evolution of near-edge X-ray absorption fine structure in the vicinity of the K-absorption edge of oxygen for HfO2 over a wide range of incidence angles is analyzed by simultaneous implementation of the total-electron-yield (TEY) method and X-ray reflection spectroscopy. It is established that the effect of refraction on the TEY spectrum is greater than that of reflection and extends into the angular region up to angles 2θc. Within angles that are less than the critical angle, both the reflection and refraction strongly distort the shape of the TEY spectrum. Limitations of the technique for the calculation of optical constants from the reflection spectra using the Kramers–Kronig relation in the limited energy region in the vicinity of thresholds are discussed in detail. PMID:29271772

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.

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.

Unified Theory for Decoding the Signals from X-Ray Florescence and X-Ray Diffraction of Mixtures.

PubMed

Chung, Frank H

2017-05-01

For research and development or for solving technical problems, we often need to know the chemical composition of an unknown mixture, which is coded and stored in the signals of its X-ray fluorescence (XRF) and X-ray diffraction (XRD). X-ray fluorescence gives chemical elements, whereas XRD gives chemical compounds. The major problem in XRF and XRD analyses is the complex matrix effect. The conventional technique to deal with the matrix effect is to construct empirical calibration lines with standards for each element or compound sought, which is tedious and time-consuming. A unified theory of quantitative XRF analysis is presented here. The idea is to cancel the matrix effect mathematically. It turns out that the decoding equation for quantitative XRF analysis is identical to that for quantitative XRD analysis although the physics of XRD and XRF are fundamentally different. The XRD work has been published and practiced worldwide. The unified theory derives a new intensity-concentration equation of XRF, which is free from the matrix effect and valid for a wide range of concentrations. The linear decoding equation establishes a constant slope for each element sought, hence eliminating the work on calibration lines. The simple linear decoding equation has been verified by 18 experiments.

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

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.

Energy-dispersive X-ray emission spectroscopy using an X-ray free-electron laser in a shot-by-shot mode

DOE PAGES

Alonso-Mori, Roberto; Kern, Jan; Gildea, Richard J.; ...

2012-11-05

The ultrabright femtosecond X-ray pulses provided by X-ray free-electron lasers open capabilities for studying the structure and dynamics of a wide variety of systems beyond what is possible with synchrotron sources. Recently, this “probe-before-destroy” approach has been demonstrated for atomic structure determination by serial X-ray diffraction of microcrystals. There has been the question whether a similar approach can be extended to probe the local electronic structure by X-ray spectroscopy. To address this, we have carried out femtosecond X-ray emission spectroscopy (XES) at the Linac Coherent Light Source using redox-active Mn complexes. XES probes the charge and spin states as wellmore » as the ligand environment, critical for understanding the functional role of redox-active metal sites. Kβ 1,3 XES spectra of Mn II and Mn 2 III,IV complexes at room temperature were collected using a wavelength dispersive spectrometer and femtosecond X-ray pulses with an individual dose of up to >100 MGy. The spectra were found in agreement with undamaged spectra collected at low dose using synchrotron radiation. Our results demonstrate that the intact electronic structure of redox active transition metal compounds in different oxidation states can be characterized with this shot-by-shot method. This opens the door for studying the chemical dynamics of metal catalytic sites by following reactions under functional conditions. Furthermore, the technique can be combined with X-ray diffraction to simultaneously obtain the geometric structure of the overall protein and the local chemistry of active metal sites and is expected to prove valuable for understanding the mechanism of important metalloproteins, such as photosystem II.« less