Brightness of synchrotron radiation from undulators and bending magnets
The maximum of the Wigner distribution (WD) of synchrotron radiation (SR) fields is considered as a possible definition of SR source brightness. Such a figure of merit was originally introduced in the SR community by Kim [(1986), Nucl. Instrum. Methods Phys. Res. A, 246, 71–76]. The brightness defined in this way is always positive and, in the geometrical optics limit, can be interpreted as the maximum density of photon flux in phase space. For undulator and bending magnet radiation from a single electron, the WD function can be explicitly calculated. In the case of an electron beam with a finite emittance the bright...
Source: Journal of Synchrotron Radiation - February 3, 2015 Category: Physics Authors: Geloni, G.Kocharyan, V.Saldin, E. Tags: brightness Wigner distribution undulator radiation bending magnet radiation lead articles Source Type: research
CDApps: integrated software for experimental planning and data processing at beamline B23, Diamond Light Source
The B23 Circular Dichroism beamline at Diamond Light Source has been operational since 2009 and has seen visits from more than 200 user groups, who have generated large amounts of data. Based on the experience of overseeing the users' progress at B23, four key areas requiring the most assistance are identified: planning of experiments and note-keeping; designing titration experiments; processing and analysis of the collected data; and production of experimental reports. To streamline these processes an integrated software package has been developed and made available for the users. The subsequent article summarizes the mai...
Source: Journal of Synchrotron Radiation - January 31, 2015 Category: Physics Authors: Hussain, R.Benning, K.Javorfi, T.Longo, E.Rudd, T.R.Pulford, B.Siligardi, G. Tags: synchrotron radiation circular dichroism (SRCD) vacuum-ultraviolet (VUV) secondary structure protein denaturation CDApps integrated software beamlines Source Type: research
In situ synchrotron X-ray diffraction investigation of the evolution of a PbO2/PbSO4 surface layer on a copper electrowinning Pb anode in a novel electrochemical flow cell
This paper describes the quantitative measurement, by in situ synchrotron X-ray diffraction (S-XRD) and subsequent Rietveld-based quantitative phase analysis and thickness calculations, of the evolution of the PbO2 and PbSO4 surface layers formed on a pure lead anode under simulated copper electrowinning conditions in a 1.6 M H2SO4 electrolyte at 318 K. This is the first report of a truly in situ S-XRD study of the surface layer evolution on a Pb substrate under cycles of galvanostatic and power interruption conditions, of key interest to the mining, solvent extraction and lead acid battery communities. The design of a...
Source: Journal of Synchrotron Radiation - January 31, 2015 Category: Physics Authors: Clancy, M.Styles, M.J.Bettles, C.J.Birbilis, N.Chen, M.Zhang, Y.Gu, Q.Kimpton, J.A.Webster, N.A.S. Tags: PbO2 PbSO4 electrochemical cycling flow cell in situ X-ray diffraction Rietveld refinement quantitative phase analysis research papers Source Type: research
Ancient administrative handwritten documents: X-ray analysis and imaging
Handwritten characters in administrative antique documents from three centuries have been detected using different synchrotron X-ray imaging techniques. Heavy elements in ancient inks, present even for everyday administrative manuscripts as shown by X-ray fluorescence spectra, produce attenuation contrast. In most cases the image quality is good enough for tomography reconstruction in view of future applications to virtual page-by-page `reading'. When attenuation is too low, differential phase contrast imaging can reveal the characters from refractive index effects. The results are potentially important for new information...
Source: Journal of Synchrotron Radiation - January 30, 2015 Category: Physics Authors: Albertin, F.Astolfo, A.Stampanoni, M.Peccenini, E.Hwu, Y.Kaplan, F.Margaritondo, G. Tags: cultural heritage ancient manuscripts ancient inks X-ray fluorescence phase contrast refractive index imaging differential phase contrast research papers Source Type: research
Radiation damage to nucleoprotein complexes in macromolecular crystallography
Significant progress has been made in macromolecular crystallography over recent years in both the understanding and mitigation of X-ray induced radiation damage when collecting diffraction data from crystalline proteins. In contrast, despite the large field that is productively engaged in the study of radiation chemistry of nucleic acids, particularly of DNA, there are currently very few X-ray crystallographic studies on radiation damage mechanisms in nucleic acids. Quantitative comparison of damage to protein and DNA crystals separately is challenging, but many of the issues are circumvented by studying pre-formed biolog...
Source: Journal of Synchrotron Radiation - January 30, 2015 Category: Physics Authors: Bury, C.Garman, E.F.Ginn, H.M.Ravelli, R.B.G.Carmichael, I.Kneale, G.McGeehan, J.E. Tags: macromolecular crystallography radiation damage protein – DNA complexes specific damage research papers Source Type: research
Effective beam method for element concentrations
There is a great diversity of research being conducted at synchrotron facilities around the world and a diverse set of beamlines to accommodate this research. Time is a precious commodity at synchrotron facilities; therefore, methods that can maximize the time spent collecting data are of value. At the same time the incident radiation spectrum, necessary for some research, may not be known on a given beamline. A preliminary presentation of a method applicable to X-ray fluorescence spectrocopic analyses that overcomes the lack of information about the incident beam spectrum that addresses both of these concerns is given her...
Source: Journal of Synchrotron Radiation - January 29, 2015 Category: Physics Authors: Tolhurst, T.Barbi, M.Tokaryk, T. Tags: beam method element concentration research papers Source Type: research
Noncrystalline structure of Ni–P nanoparticles prepared by liquid pulse discharge
Noncrystalline nickel phosphide (Ni–P) nanoparticles have drawn great attention due to their high potential as catalysts. However, the structure of noncrystalline Ni–P nanoparticles is still unknown, which may shed light on explaining the catalysis mechanism of the Ni–P nanoparticles. In this paper, noncrystalline Ni–P nanoparticles were synthesized. Their morphology, particle size, element contents, local atomic structures, as well as the catalysis in the thermal decomposition of ammonium perchlorate were studied. The results demonstrate that the as-prepared Ni–P nanoparticles are spherical w...
Source: Journal of Synchrotron Radiation - January 29, 2015 Category: Physics Authors: Tan, Y.Yu, H.Wu, Z.Yang, B.Gong, Y.Yan, S.Du, R.Chen, Z.Sun, D. Tags: noncrystalline structure Ni – P nanoparticles pulse discharge local structure model research papers Source Type: research
Stroboscopic detection of nuclear resonance in an arbitrary scattering channel
The theory of heterodyne/stroboscopic detection of nuclear resonance scattering is developed, starting from the total scattering matrix as a product of the matrix of the reference sample and the sample under study. This general approach holds for all dynamical scattering channels. In the forward channel, which has been discussed in detail in the literature, the electronic scattering manifests itself only in an energy-independent diminution of the scattered intensity. In all other channels, complex resonance line shapes of the heterodyne/stroboscopic spectra are encountered, as a result of the interference of electronic and...
Source: Journal of Synchrotron Radiation - January 28, 2015 Category: Physics Authors: Deák, L.Bottyán, L.Callens, R.Coussement, R.Major, M.Nasu, S.Serdons, I.Spiering, H.Yoda, Y. Tags: nuclear resonant scattering stroboscopic detection multilayer research papers Source Type: research
Thermal stress prediction in mirror and multilayer coatings
Multilayer optics for X-rays typically consist of hundreds of periods of two types of alternating sub-layers which are coated on a silicon substrate. The thickness of the coating is well below 1 µm (tens or hundreds of nanometers). The high aspect ratio (∼107) between the size of the optics and the thickness of the multilayer can lead to a huge number of elements (∼1016) for the numerical simulation (by finite-element analysis using ANSYS code). In this work, the finite-element model for thermal-structural analysis of multilayer optics has been implemented using the ANSYS layer-functioned elements. The numb...
Source: Journal of Synchrotron Radiation - January 28, 2015 Category: Physics Authors: Cheng, X.Zhang, L.Morawe, C.Sanchez del Rio, M. Tags: multilayer optics finite-element analysis (FEA) thermal mismatch stress liquid-nitrogen cooling research papers Source Type: research
Pushing the limits: an instrument for hard X-ray imaging below 20 nm
Hard X-ray microscopy is a prominent tool suitable for nanoscale-resolution non-destructive imaging of various materials used in different areas of science and technology. With an ongoing effort to push the 2D/3D imaging resolution down to 10 nm in the hard X-ray regime, both the fabrication of nano-focusing optics and the stability of the microscope using those optics become extremely challenging. In this work a microscopy system designed and constructed to accommodate multilayer Laue lenses as nanofocusing optics is presented. The developed apparatus has been thoroughly characterized in terms of resolution and stabilit...
Source: Journal of Synchrotron Radiation - January 28, 2015 Category: Physics Authors: Nazaretski, E.Lauer, K.Kalbfleisch, S.Wagner, U.Rau, C.Chu, Y.S.Yan, H.Bouet, N.Zhou, J.Conley, R.Huang, X.Xu, W.Lu, M.Gofron, K. Tags: scanning X-ray microscopy multilayer Laue lenses interferometry nanopositioning research papers Source Type: research
A new extra-focus monochromator designed for high-performance VUV beamlines
A new monochromator called an extra-focus constant-included-angle varied-line-spacing (VLS) cylindrical-grating monochromator (extra-focus CIA-VCGM) is described. This monochromator is based on the Hettrick–Underwood scheme where the plane VLS grating is replaced by a cylindrical one in order to zero the defocus at three reference photon energies in the vacuum-ultraviolet range. It has a simple mechanical structure and a fixed focus spot with high performance over a wide energy range. Furthermore, its mechanical compatibility with a standard VLS plane-grating monochromator allows convenient extension into the soft-X-...
Source: Journal of Synchrotron Radiation - January 28, 2015 Category: Physics Authors: Xue, C.Wu, Y.Zou, Y.Xue, L.Wang, Y.Xu, Z.Tai, R. Tags: VUV beamline monochromator research papers Source Type: research
New methods in time-resolved Laue pump–probe crystallography at synchrotron sources
Newly developed methods for time-resolved studies using the polychromatic and in particular the pink-Laue technique, suitable for medium and small-size unit cells typical in chemical crystallography, are reviewed. The order of the sections follows that of a typical study, starting with a description of the pink-Laue technique, followed by the strategy of data collection for analysis with the RATIO method. Novel procedures are described for spot integration, orientation matrix determination for relatively sparse diffraction patterns, scaling of multi-crystal data sets, use of Fourier maps for initial assessment and analysis...
Source: Journal of Synchrotron Radiation - January 28, 2015 Category: Physics Authors: Coppens, P.Fournier, B. Tags: photocrystallography pink-Laue orientation matrix determination spot integration multicrystal data sets lead articles Source Type: research
XFEL diffraction: developing processing methods to optimize data quality
Serial crystallography, using either femtosecond X-ray pulses from free-electron laser sources or short synchrotron-radiation exposures, has the potential to reveal metalloprotein structural details while minimizing damage processes. However, deriving a self-consistent set of Bragg intensities from numerous still-crystal exposures remains a difficult problem, with optimal protocols likely to be quite different from those well established for rotation photography. Here several data processing issues unique to serial crystallography are examined. It is found that the limiting resolution differs for each shot, an effect that ...
Source: Journal of Synchrotron Radiation - January 28, 2015 Category: Physics Authors: Sauter, N.K. Tags: serial femtosecond crystallography X-ray free-electron laser partiality postrefinement mosaicity research papers Source Type: research
Extended X-ray absorption fine structure and multiple-scattering simulation of nickel dithiolene complexes Ni[S2C2(CF3)2]2n (n = −2, −1, 0) and an olefin adduct Ni[S2C2(CF3)2]2(1-hexene)
A series of Ni dithiolene complexes Ni[S2C2(CF3)]2n (n = −2, −1, 0) (1, 2, 3) and a 1-hexene adduct Ni[S2C2(CF3)2]2(C6H12) (4) have been examined by Ni K-edge X-ray absorption near-edge structure (XANES) and extended X-ray absorption fine-structure (EXAFS) spectroscopies. Ni XANES for 1–3 reveals clear pre-edge features and approximately +0.7 eV shift in the Ni K-edge position for `one-electron' oxidation. EXAFS simulation shows that the Ni—S bond distances for 1, 2 and 3 (2.11–2.16 Å) are within the typical values for square planar complexes and decrease by ∼0.022 Å for ...
Source: Journal of Synchrotron Radiation - December 24, 2014 Category: Physics Authors: Gu, W.Wang, H.Wang, K. Tags: Ni dithiolene complexes olefin adduct extended X-ray absorption fine structure (EXAFS) X-ray absorption near-edge structure (XANES) single scattering multiple research papers Source Type: research
JSR – XFELs, DLSRs and beamline articles
(Source: Journal of Synchrotron Radiation)
Source: Journal of Synchrotron Radiation - December 23, 2014 Category: Physics Authors: van der Veen, J.F. Tags: editorial Source Type: research
Tuning the phase transition of ZnO thin films through lithography: an integrated bottom-up and top-down processing
An innovative approach towards the physico-chemical tailoring of zinc oxide thin films is reported. The films have been deposited by liquid phase using the sol–gel method and then exposed to hard X-rays, provided by a synchrotron storage ring, for lithography. The use of surfactant and chelating agents in the sol allows easy-to-pattern films made by an organic–inorganic matrix to be deposited. The exposure to hard X-rays strongly affects the nucleation and growth of crystalline ZnO, triggering the formation of two intermediate phases before obtaining a wurtzite-like structure. At the same time, X-ray lithograph...
Source: Journal of Synchrotron Radiation - December 16, 2014 Category: Physics Authors: Malfatti, L.Pinna, A.Enzo, S.Falcaro, P.Marmiroli, B.Innocenzi, P. Tags: zinc oxide thin film sol – gel lithography bottom-up/top-down research papers Source Type: research
Compton scattering imaging of a working battery using synchrotron high-energy X-rays
Results of studies on Compton scattering imaging using synchrotron high-energy X-rays are reported. The technique is applied to a discharging coin cell, and the intensity of Compton scattered X-rays from the inside of the cell has been measured as a function of position and time. The position–time intensity map captures the migration of lithium ions in the positive electrode and reveals the structural change due to the volume expansion of the electrode. This experiment is a critical step in developing synchrotron-based Compton scattering imaging for electrochemical cells at a product level. (Source: Journal of Synchrotron Radiation)
Source: Journal of Synchrotron Radiation - December 12, 2014 Category: Physics Authors: Itou, M.Orikasa, Y.Gogyo, Y.Suzuki, K.Sakurai, H.Uchimoto, Y.Sakurai, Y. Tags: synchrotron X-ray imaging lithium battery in situ analysis Compton scattering research papers Source Type: research
Monitoring the thin film formation during sputter deposition of vanadium carbide
The thin film formation of magnetron sputtered polycrystalline coatings was monitored by in situ X-ray reflectivity measurements. The measured intensity was analyzed using the Parratt algorithm for time-dependent thin film systems. Guidelines for the on-line interpretation of the data were developed. For thick coatings, the experimental resolution needs to be included in the data evaluation in order to avoid misinterpretations. Based on a simple layer model, the time-dependent mean electron density, roughness and growth velocity were extracted from the data. As an example, the method was applied to the hard coating materia...
Source: Journal of Synchrotron Radiation - December 12, 2014 Category: Physics Authors: Kaufholz, M.Krause, B.Kotapati, S.Köhl, M.Mantilla, M.F.Stüber, M.Ulrich, S.Schneider, R.Gerthsen, D.Baumbach, T. Tags: in situ X-ray reflectivity composite sputter deposition research papers Source Type: research
Direct nano-scale patterning of Ag films using hard X-ray induced oxidation
The morphological change of silver nano-particles (AgNPs) exposed to an intense synchrotron X-ray beam was investigated for the purpose of direct nano-scale patterning of metal thin films. AgNPs irradiated by hard X-rays in oxygen ambient were oxidized and migrated out of the illuminated region. The observed X-ray induced oxidation was utilized to fabricate nano-scale metal line patterns using sectioned WSi2/Si multilayers as masks. Lines with a width as small as 21 nm were successfully fabricated on Ag films on silicon nitride. Au/Ag nano-lines were also fabricated using the proposed method. (Source: Journal of Synchrotron Radiation)
Source: Journal of Synchrotron Radiation - December 10, 2014 Category: Physics Authors: Kim, J.M.Lee, S.Y.Kang, H.C.Noh, D.Y. Tags: hard X-ray focusing Fresnel zone plate X-ray lithography research papers Source Type: research
Polytypism in GaAs nanowires: determination of the interplanar spacing of wurtzite GaAs by X-ray diffraction
In GaAs nanowires grown along the cubic c direction, zinc blende and wurtzite arrangements have been observed in their stacking sequence, since the energetic barriers for nucleation are typically of similar order of magnitude. It is known that the interplanar spacing of the (111)c Ga (or As) planes in the zinc blende polytype varies slightly from the wurtzite polytype. However, different values have been reported in the literature. Here, the ratio of the interplanar spacing of these polytypes is extracted based on X-ray diffraction measurements for thin GaAs nanowires with a mean diameter of 18–25 nm. The meas...
Source: Journal of Synchrotron Radiation - December 10, 2014 Category: Physics Authors: Köhl, M.Schroth, P.Minkevich, A.A.Hornung, J.-W.Dimakis, E.Somaschini, C.Geelhaar, L.Aschenbrenner, T.Lazarev, S.Grigoriev, D.Pietsch, U.Baumbach, T. Tags: GaAs nanowires polytypism X-ray diffraction nanofocus research papers Source Type: research
X-ray phase-contrast computed tomography visualizes the microstructure and degradation profile of implanted biodegradable scaffolds after spinal cord injury
Tissue engineering strategies for spinal cord repair are a primary focus of translational medicine after spinal cord injury (SCI). Many tissue engineering strategies employ three-dimensional scaffolds, which are made of biodegradable materials and have microstructure incorporated with viable cells and bioactive molecules to promote new tissue generation and functional recovery after SCI. It is therefore important to develop an imaging system that visualizes both the microstructure of three-dimensional scaffolds and their degradation process after SCI. Here, X-ray phase-contrast computed tomography imaging based on the Talb...
Source: Journal of Synchrotron Radiation - December 10, 2014 Category: Physics Authors: Takashima, K.Hoshino, M.Uesugi, K.Yagi, N.Matsuda, S.Nakahira, A.Osumi, N.Kohzuki, M.Onodera, H. Tags: X-ray phase-contrast CT Talbot grating interferometer biodegradation tissue engineering spinal cord injury research papers Source Type: research
MX1: a bending-magnet crystallography beamline serving both chemical and macromolecular crystallography communities at the Australian Synchrotron
MX1 is a bending-magnet crystallography beamline at the 3 GeV Australian Synchrotron. The beamline delivers hard X-rays in the energy range from 8 to 18 keV to a focal spot at the sample position of 120 µm FWHM. The beamline endstation and ancillary equipment facilitate local and remote access for both chemical and biological macromolecular crystallography. Here, the design of the beamline and endstation are discussed. The beamline has enjoyed a full user program for the last seven years and scientific highlights from the user program are also presented. (Source: Journal of Synchrotron Radiation)
Source: Journal of Synchrotron Radiation - December 7, 2014 Category: Physics Authors: Cowieson, N.P.Aragao, D.Clift, M.Ericsson, D.J.Gee, C.Harrop, S.J.Mudie, N.Panjikar, S.Price, J.R.Riboldi-Tunnicliffe, A.Williamson, R.Caradoc-Davies, T. Tags: crystallography beamline bending magnet beamlines Source Type: research
Functionalized synchrotron in-line phase-contrast computed tomography: a novel approach for simultaneous quantification of structural alterations and localization of barium-labelled alveolar macrophages within mouse lung samples
In this study we applied in-line free propagation X-ray phase-contrast CT (XPCT) in an allergic asthma mouse model to assess structural changes as well as the biodistribution of barium-labelled macrophages in lung tissue. Alveolar macrophages that were barium-sulfate-loaded and fluorescent-labelled were instilled intratracheally into asthmatic and control mice. Mice were sacrificed after 24 h, lungs were kept in situ, inflated with air and scanned utilizing XPCT at the SYRMEP beamline (Elettra Synchrotron Light Source, Italy). Single-distance phase retrieval was used to generate data sets with ten times greater contrast-...
Source: Journal of Synchrotron Radiation - December 4, 2014 Category: Physics Authors: Dullin, C.dal Monego, S.Larsson, E.Mohammadi, S.Krenkel, M.Garrovo, C.Biffi, S.Lorenzon, A.Markus, A.Napp, J.Salditt, T.Accardo, A.Alves, F.Tromba, G. Tags: phase-contrast CT single-distance phase retrieval functional CT imaging research papers Source Type: research
Large-acceptance diamond planar refractive lenses manufactured by laser cutting
For the first time, single-crystal diamond planar refractive lenses have been fabricated by laser micromachining in 300 µm-thick diamond plates which were grown by chemical vapour deposition. Linear lenses with apertures up to 1 mm and parabola apex radii up to 500 µm were manufactured and tested at the ESRF ID06 beamline. The large acceptance of these lenses allows them to be used as beam-conditioning elements. Owing to the unsurpassed thermal properties of single-crystal diamond, these lenses should be suitable to withstand the extreme flux densities expected at the planned fourth-generation X-ray sourc...
Source: Journal of Synchrotron Radiation - December 3, 2014 Category: Physics Authors: Polikarpov, M.Snigireva, I.Morse, J.Yunkin, V.Kuznetsov, S.Snigirev, A. Tags: X-ray optics refractive lenses diamond planar lenses beam conditioning diamond processing laser micromachining research papers Source Type: research
X-ray diffraction strain analysis of a single axial InAs1–xPx nanowire segment
The spatial strain distribution in and around a single axial InAs1–xPx hetero-segment in an InAs nanowire was analyzed using nano-focused X-ray diffraction. In connection with finite-element-method simulations a detailed quantitative picture of the nanowire's inhomogeneous strain state was achieved. This allows for a detailed understanding of how the variation of the nanowire's and hetero-segment's dimensions affect the strain in its core region and in the region close to the nanowire's side facets. Moreover, ensemble-averaging high-resolution diffraction experiments were used to determine statistical information on ...
Source: Journal of Synchrotron Radiation - December 3, 2014 Category: Physics Authors: Keplinger, M.Mandl, B.Kriegner, D.Holý, V.Samuelsson, L.Bauer, G.Deppert, K.Stangl, J. Tags: nanowire nano-focus strain analysis hetero-structure finite-element simulation research papers Source Type: research
Simultaneous X-ray diffraction and phase-contrast imaging for investigating material deformation mechanisms during high-rate loading
Using a high-speed camera and an intensified charge-coupled device (ICCD), a simultaneous X-ray imaging and diffraction technique has been developed for studying dynamic material behaviors during high-rate tensile loading. A Kolsky tension bar has been used to pull samples at 1000 s−1 and 5000 s−1 strain-rates for super-elastic equiatomic NiTi and 1100-O series aluminium, respectively. By altering the ICCD gating time, temporal resolutions of 100 ps and 3.37 µs have been achieved in capturing the diffraction patterns of interest, thus equating to single-pulse and 22-pulse X-ray exposure. Furthermo...
Source: Journal of Synchrotron Radiation - December 3, 2014 Category: Physics Authors: Hudspeth, M.Sun, T.Parab, N.Guo, Z.Fezzaa, K.Luo, S.Chen, W. Tags: Kolsky bar dynamic diffraction research papers Source Type: research
Biology with Free-Electron X-ray Lasers: Papers of a Discussion Meeting Issue, Philos. Trans. R. Soc. B, 17 July 2014, Vol. 369, No. 1647, edited by John C. H. Spence and Henry N. Chapman. London: The Royal Society
(Source: Journal of Synchrotron Radiation)
Source: Journal of Synchrotron Radiation - November 28, 2014 Category: Physics Authors: Helliwell, J.R. Tags: book reviews Source Type: research
Energy optimization of a regular macromolecular crystallography beamline for ultra-high-resolution crystallography
A practical method for operating existing undulator synchrotron beamlines at photon energies considerably higher than their standard operating range is described and applied at beamline 19-ID of the Structural Biology Center at the Advanced Photon Source enabling operation at 30 keV. Adjustments to the undulator spectrum were critical to enhance the 30 keV flux while reducing the lower- and higher-energy harmonic contamination. A Pd-coated mirror and Al attenuators acted as effective low- and high-bandpass filters. The resulting flux at 30 keV, although significantly lower than with X-ray optics designed and optimize...
Source: Journal of Synchrotron Radiation - November 28, 2014 Category: Physics Authors: Rosenbaum, G.Ginell, S.L.Chen, J.C.-H. Tags: undulator high energy monochromator harmonic short communications Source Type: research
Inelastic X-ray scattering with 0.75 meV resolution at 25.7 keV using a temperature-gradient analyzer
The use of temperature-gradient analyzers for non-resonant high-resolution inelastic X-ray scattering is investigated. The gradient compensates for geometrical broadening of the energy resolution by adjusting the lattice spacing of the analyzer crystal. Applying a ∼12 mK temperature gradient across a 9.5 cm analyzer, resolutions of 0.75 (2) meV FWHM at 25.7 keV for Si(13 13 13) and 1.25 (2) meV at 21.7 keV for Si(11 11 11) were measured, while retaining large (250 mm) clearance between the sample position and detector, and reasonable (9.3 mrad × 8.8 mrad) analyzer acceptance. The tem...
Source: Journal of Synchrotron Radiation - November 28, 2014 Category: Physics Authors: Ishikawa, D.Ellis, D.S.Uchiyama, H.Baron, A.Q.R. Tags: inelastic X-ray scattering high-resolution analyzer X-ray optics research papers Source Type: research
X-ray irradiation induces local rearrangement of silica particles in swollen rubber
X-ray photon correlation spectroscopy (XPCS) of swollen rubber containing spherical silica nanoparticles is reported. It is shown that irradiation by intense X-rays leads to the breakdown of cross-links, thereby inducing the local rearrangement of silica nanoparticles. This rearrangement process depends on the cross-link density and is characterized by a compressed exponential relaxation with aging behaviour, which resembles a common feature of complex fluids observed with XPCS. (Source: Journal of Synchrotron Radiation)
Source: Journal of Synchrotron Radiation - November 28, 2014 Category: Physics Authors: Shinohara, Y.Yamamoto, N.Kishimoto, H.Amemiya, Y. Tags: X-ray photon correlation spectroscopy filled rubber research papers Source Type: research
Confocal soft X-ray scanning transmission microscopy: setup, alignment procedure and limitations
Zone-plate-based scanning transmission soft X-ray microspectroscopy (STXM) is a well established technique for high-contrast imaging of sufficiently transparent specimens (e.g. ultrathin biological tissues, polymer materials, archaeometric specimens or magnetic thin films) with spatial resolutions in the regime of 20 nm and high spectroscopic or chemical sensitivity. However, due to the relatively large depth of focus of zone plates, the resolution of STXM along the optical axis so far stays unambiguously behind for thicker X-ray transparent specimens. This challenge can be addressed by the implementation of a second zon...
Source: Journal of Synchrotron Radiation - November 28, 2014 Category: Physics Authors: Späth, A.Raabe, J.Fink, R.H. Tags: STXM soft X-ray microscopy confocal microscopy zone plate research papers Source Type: research
Structure and effects of annealing in colloidal matrix-free Ge quantum dots
The structure of small (2–5 nm) Ge quantum dots prepared by the colloidal synthesis route is examined. Samples were synthesized using either GeO2 or GeCl4 as precursor. As-prepared samples were further annealed under Ar or H2/Ar atmosphere at different temperatures in order to understand the effect of annealing on their structure. It was found that as-prepared samples possess distinctly different structures depending on their synthesis route as indicated by their long-range ordering. An appreciable amount of oxygen was found to be bound to Ge in samples prepared with GeO2 as a precursor; however, not for GeCl4. Bas...
Source: Journal of Synchrotron Radiation - November 27, 2014 Category: Physics Authors: Zhang, Y.Karatutlu, A.Ersoy, O.Little, W.Cibin, G.Dent, A.Sapelkin, A. Tags: Ge quantum dots (QDs) annealing matrix-free combined characterization core-shell model research papers Source Type: research
X-ray focusing scheme with continuously variable lens
A novel hybrid X-ray focusing scheme was developed for operation of the X-ray streak camera at the Advanced Photon Source: an X-ray lens focuses vertically from a long distance of 16 m and produces an extended focus that has a small footprint on an inexpensive sagittal mirror. A patented method is used to continuously adjust the focal length of the lens and compensate for chromatic dispersion in energy scans. (Source: Journal of Synchrotron Radiation)
Source: Journal of Synchrotron Radiation - November 27, 2014 Category: Physics Authors: Adams, B.W.Rose-Petruck, C. Tags: X-ray focusing continuously variable focal length research papers Source Type: research
The pH dependence of Am(III) complexation with acetate: an EXAFS study
The complexation of acetate with Am(III) is studied as a function of the pH (1–6) by extended X-ray absorption fine-structure (EXAFS) spectroscopy. The molecular structure of the Am(III)–acetate complexes (coordination numbers, oxygen and carbon distances) is determined from the raw k3-weighted Am LIII-edge EXAFS spectra. The results show a continuous shift of Am(III) speciation with increasing pH value towards the complexed species. Furthermore, it is verified that acetate coordinates in a bidentate coordination mode to Am(III) (Am—C distance: 2.82 ± 0.03 Å). The EXAFS data are analyzed by...
Source: Journal of Synchrotron Radiation - November 27, 2014 Category: Physics Authors: Fröhlich, D.R.Skerencak-Frech, A.Bauer, N.Rossberg, A.Panak, P.J. Tags: americium acetate coordination chemistry EXAFS ITFA research papers Source Type: research
Design and development of a controlled pressure/temperature set-up for in situ studies of solid–gas processes and reactions in a synchrotron X-ray powder diffraction station
A novel set-up has been designed and used for synchrotron radiation X-ray high-resolution powder diffraction (SR-HRPD) in transmission geometry (spinning capillary) for in situ solid–gas reactions and processes in an isobaric and isothermal environment. The pressure and temperature of the sample are controlled from 10−3 to 1000 mbar and from 80 to 1000 K, respectively. To test the capacities of this novel experimental set-up, structure deformation in the porous material zeolitic imidazole framework (ZIF-8) by gas adsorption at cryogenic temperature has been studied under isothermal and isobaric conditions. ...
Source: Journal of Synchrotron Radiation - November 27, 2014 Category: Physics Authors: Salas-Colera, E.Muñoz-Noval, Á.Heyman, C.Ania, C.O.Parra, J.B.García-Granda, S.Calero, S.Rubio-Zuazo, J.Castro, G.R. Tags: X-ray powder diffraction isobaric/isothermal environment research papers Source Type: research
In situ synchrotron X-ray diffraction analysis of deformation behaviour in Ti–Ni-based thin films
Deformation mechanisms of as-deposited and post-annealed Ti50.2Ni49.6, Ti50.3Ni46.2Cu3.5 and Ti48.5Ni40.8Cu7.5 thin films were investigated using the in situ synchrotron X-ray diffraction technique. Results showed that initial crystalline phases determined the deformation mechanisms of all the films during tensile loading. For the films dominated by monoclinic martensites (B19′), tensile stress induced the detwinning of 〈011〉 type-II twins and resulted in the preferred orientations of (002)B19′ parallel to the loading direction (∥ LD) and (020)B19′ perpendicular to the LD (⊥ LD)....
Source: Journal of Synchrotron Radiation - November 27, 2014 Category: Physics Authors: Wang, H.Sun, G.Wang, X.Chen, B.Zu, X.Liu, Y.Li, L.Pan, G.Sheng, L.Liu, Y.Fu, Y.Q. Tags: shape memory Ti – Ni thin film deformation behaviour detwinning synchrotron X-ray diffraction research papers Source Type: research
Synchrotron radiation computed laminography using an inclined detector
Synchrotron radiation computed laminography (SR-CL) has been in use in three-dimensional non-destructive imaging of flat objects for several years. A new set-up is proposed based on the traditional SR-CL method but with the detector inclined at the same angle as the sample inclination to collect projections. The results of computer simulations and real-sample experiments demonstrate that reconstructions acquired using an inclined detector are of better quality compared with those acquired using ordinary detecting methods, especially for the situation of few projections and small difference of attenuation ratio of the sampl...
Source: Journal of Synchrotron Radiation - November 27, 2014 Category: Physics Authors: Zhang, J.Li, G.Yi, Q.Chen, Y.Gao, Z.Jiang, X. Tags: computed laminography inclining detector research papers Source Type: research
Upgrade of MacCHESS facility for X-ray scattering of biological macromolecules in solution
X-ray scattering of biological macromolecules in solution is an increasingly popular tool for structural biology and benefits greatly from modern high-brightness synchrotron sources. The upgraded MacCHESS BioSAXS station is now located at the 49-pole wiggler beamline G1. The 20-fold improved flux over the previous beamline F2 provides higher sample throughput and autonomous X-ray scattering data collection using a unique SAXS/WAXS dual detectors configuration. This setup achieves a combined q-range from 0.007 to 0.7 Å−1, enabling better characterization of smaller molecules, while opening opportunities for em...
Source: Journal of Synchrotron Radiation - November 25, 2014 Category: Physics Authors: Acerbo, A.S.Cook, M.J.Gillilan, R.E. Tags: SAXS high throughput MacCHESS beamlines Source Type: research
The GALAXIES beamline at the SOLEIL synchrotron: inelastic X-ray scattering and photoelectron spectroscopy in the hard X-ray range
The GALAXIES beamline at the SOLEIL synchrotron is dedicated to inelastic X-ray scattering (IXS) and photoelectron spectroscopy (HAXPES) in the 2.3–12 keV hard X-ray range. These two techniques offer powerful complementary methods of characterization of materials with bulk sensitivity, chemical and orbital selectivity, resonant enhancement and high resolving power. After a description of the beamline components and endstations, the beamline capabilities are demonstrated through a selection of recent works both in the solid and gas phases and using either IXS or HAXPES approaches. Prospects for studies on liquids ar...
Source: Journal of Synchrotron Radiation - November 25, 2014 Category: Physics Authors: Rueff, J.-P.Ablett, J.M.Céolin, D.Prieur, D.Moreno, T.Balédent, V.Lassalle-Kaiser, B.Rault, J.E.Simon, M.Shukla, A. Tags: inelastic X-ray scattering RIXS photoemission HAXPES beamlines Source Type: research
A portable ultrahigh-vacuum system for advanced synchrotron radiation studies of thin films and nanostructures: EuSi2 nano-islands
A portable ultrahigh-vacuum system optimized for in situ variable-temperature X-ray scattering and spectroscopy experiments at synchrotron radiation beamlines was constructed and brought into operation at the synchrotron radiation facility ANKA of the Karlsruhe Institute of Technology, Germany. Here the main features of the new instrument are described and its capabilities demonstrated. The surface morphology, structure and stoichiometry of EuSi2 nano-islands are determined by in situ grazing-incidence small-angle X-ray scattering and X-ray absorption spectroscopy. A size reduction of about a factor of two of the nano-isla...
Source: Journal of Synchrotron Radiation - November 25, 2014 Category: Physics Authors: Ibrahimkutty, S.Seiler, A.Prüßmann, T.Vitova, T.Pradip, R.Bauder, O.Wochner, P.Plech, A.Baumbach, T.Stankov, S. Tags: in situ experiments GISAXS EXAFS XANES rare-earth silicides research papers Source Type: research
Investigation of damaged interior walls using synchrotron-based XPS and XANES
Evidence of internal sulfate attack in field exposure was demonstrated by the damaged interior wall of a three-year-old house situated in Nakhon Ratchasima Province, Thailand. Partial distension of the mortar was clearly observed together with an expansion of a black substance. Removal of the black substance revealed a dense black layer. This layer was only found in the vicinity of the damaged area, suggesting that this black material is possibly involved in the wall cracking. By employing synchrotron-based X-ray photoelectron spectroscopy (XPS) and X-ray absorption near-edge structure (XANES) techniques, the unknown sampl...
Source: Journal of Synchrotron Radiation - November 21, 2014 Category: Physics Authors: Poo-arporn, Y.Thachepan, S.Palangsuntikul, R. Tags: cement mortar internal sulfate attack XPS XANES research papers Source Type: research
Cooling dynamics of self-assembled monolayer coating for integrated gold nanocrystals on a glass substrate
Picosecond time-resolved X-ray diffraction has been used to study the nanoscale thermal transportation dynamics of bare gold nanocrystals and thiol-based self-assembled monolayer (SAM)-coated integrated gold nanocrystals on a SiO2 glass substrate. A temporal lattice expansion of 0.30–0.33% was observed in the bare and SAM-coated nanocrystals on the glass substrate; the thermal energy inside the gold nanocrystals was transported to the contacted substrate through the gold–SiO2 interface. The interfacial thermal conductivity between the single-layered gold nanocrystal film and the SiO2 substrate is estimated to b...
Source: Journal of Synchrotron Radiation - November 21, 2014 Category: Physics Authors: Ichiyanagi, K.Sekiguchi, H.Sato, T.Nozawa, S.Tomita, A.Hoshino, M.Adachi, S.-Sasaki, Y.C. Tags: time-resolved X-ray diffraction thermal conductance nanocrystal thermal flow research papers Source Type: research
Characterization of a next-generation piezo bimorph X-ray mirror for synchrotron beamlines
Piezo bimorph mirrors are versatile active optics used on many synchrotron beamlines. However, many bimorphs suffer from the `junction effect': a periodic deformation of the optical surface which causes major aberrations to the reflected X-ray beam. This effect is linked to the construction of such mirrors, where piezo ceramics are glued directly below the thin optical substrate. In order to address this problem, a next-generation bimorph with piezos bonded to the side faces of a monolithic substrate was developed at Thales-SESO and optimized at Diamond Light Source. Using metrology feedback from the Diamond-NOM, the optic...
Source: Journal of Synchrotron Radiation - November 21, 2014 Category: Physics Authors: Alcock, S.G.Nistea, I.Sutter, J.P.Sawhney, K.Fermé, J.-J.Thellièr, C.Peverini, L. Tags: piezo bimorph mirror synchrotron X-ray optics active optics Diamond-NOM junction effect research papers Source Type: research
Solvent minimization induces preferential orientation and crystal clustering in serial micro-crystallography on micro-meshes, in situ plates and on a movable crystal conveyor belt
X-ray diffraction data were obtained at the National Synchrotron Light Source from insulin and lysozyme crystals that were densely deposited on three types of surfaces suitable for serial micro-crystallography: MiTeGen MicroMeshes™, Greiner Bio-One Ltd in situ micro-plates, and a moving kapton crystal conveyor belt that is used to deliver crystals directly into the X-ray beam. 6° wedges of data were taken from ∼100 crystals mounted on each material, and these individual data sets were merged to form nine complete data sets (six from insulin crystals and three from lysozyme crystals). Insulin crystals have a p...
Source: Journal of Synchrotron Radiation - October 9, 2014 Category: Physics Authors: Soares, A.S.Mullen, J.D.Parekh, R.M.McCarthy, G.S.Roessler, C.G.Jackimowicz, R.Skinner, J.M.Orville, A.M.Allaire, M.Sweet, R.M. Tags: in situ X-ray data collection crystallography acoustic droplet ejection serial research papers Source Type: research
Correcting for surface topography in X-ray fluorescence imaging
Samples with non-planar surfaces present challenges for X-ray fluorescence imaging analysis. Here, approximations are derived to describe the modulation of fluorescence signals by surface angles and topography, and suggestions are made for reducing this effect. A correction procedure is developed that is effective for trace element analysis of samples having a uniform matrix, and requires only a fluorescence map from a single detector. This procedure is applied to fluorescence maps from an incised gypsum tablet. (Source: Journal of Synchrotron Radiation)
Source: Journal of Synchrotron Radiation - October 9, 2014 Category: Physics Authors: Geil, E.C.Thorne, R.E. Tags: X-ray fluorescence imaging surface angle surface orientation topography research papers Source Type: research
Investigation of short-range structural order in Zr69.5Cu12Ni11Al7.5 and Zr41.5Ti41.5Ni17 glasses, using X-ray absorption spectroscopy and ab initio molecular dynamics simulations
Short-range order has been investigated in Zr69.5Cu12Ni11Al7.5 and Zr41.5Ti41.5Ni17 metallic glasses using X-ray absorption spectroscopy and ab initio molecular dynamics simulations. While both of these alloys are good glass formers, there is a difference in their glass-forming abilities (Zr41.5Ti41.5Ni17> Zr69.5Cu12Ni11Al7.5). This difference is explained by inciting the relative importance of strong chemical order, icosahedral content, cluster symmetry and configuration diversity. (Source: Journal of Synchrotron Radiation)
Source: Journal of Synchrotron Radiation - October 8, 2014 Category: Physics Authors: Lahiri, D.Sharma, S.M.Verma, A.K.Vishwanadh, B.Dey, G.K.Schumacher, G.Scherb, T.Riesemeier, H.Reinholz, U.Radtke, M.Banerjee, S. Tags: multi-component alloy glass-forming ability XAFS local structure AIMD simulation research papers Source Type: research
Quantitative and dynamic measurements of biological fresh samples with X-ray phase contrast tomography
X-ray phase contrast tomography using a Talbot grating interferometer was applied to biological fresh samples which were not fixed by any fixatives. To achieve a high-throughput measurement for the fresh samples the X-ray phase contrast tomography measurement procedure was improved. The three-dimensional structure of a fresh mouse fetus was clearly depicted as a mass density map using X-ray phase contrast tomography. The mouse fetus measured in the fresh state was then fixed by formalin and measured in the fixed state. The influence of the formalin fixation on soft tissue was quantitatively evaluated by comparing the fresh...
Source: Journal of Synchrotron Radiation - October 8, 2014 Category: Physics Authors: Hoshino, M.Uesugi, K.Tsukube, T.Yagi, N. Tags: X-ray phase contrast tomography quantitative imaging three-dimensional densitometry dynamic imaging research papers Source Type: research
Double-focusing mixing jet for XFEL study of chemical kinetics
Several liquid sample injection methods have been developed to satisfy the requirements for serial femtosecond X-ray nanocrystallography, which enables radiation-damage-free determination of molecular structure at room temperature. Time-resolved nanocrystallography would combine structure analysis with chemical kinetics by determining the structures of the transient states and chemical kinetic mechanisms simultaneously. A windowless liquid mixing jet device has been designed for this purpose. It achieves fast uniform mixing of substrates and enzymes in the jet within 250 µs, with an adjustable delay between mixing ...
Source: Journal of Synchrotron Radiation - October 7, 2014 Category: Physics Authors: Wang, D.Weierstall, U.Pollack, L.Spence, J. Tags: time-resolved diffraction mixing jet sample injection chemical kinetics short communications Source Type: research