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114 items found (0 items not approved), displaying 1 to 10.[First/Prev] 1, 2, 3, 4, 5, 6, 7, 8 [Next/Last]

Instruments / Technical Area	Publication Details	Published
B16-Test Beamline Detectors	Room-temperature X-ray response of cadmium–zinc–telluride pixel detectors grown by the vertical Bridgman technique Leonardo Abbene , Fabio Principato , Gaetano Gerardi , Antonino Buttacavoli , Donato Cascio , Manuele Bettelli , Nicola Sarzi Amade , Paul Seller , Matthew C. Veale , Oliver Fox , Kawal Sawhney , Silvia Zanettini , Elio Tomarchio , Andrea Zappettini Journal Of Synchrotron Radiation 27 DOI: 10.1107/S1600577519015996 Diamond Proposal Number(s): [20545] Show Abstract ▼ Abstract: In this work, the spectroscopic performances of new cadmium–zinc–telluride (CZT) pixel detectors recently developed at IMEM-CNR of Parma (Italy) are presented. Sub-millimetre arrays with pixel pitch less than 500 µm, based on boron oxide encapsulated vertical Bridgman grown CZT crystals, were fabricated. Excellent room-temperature performance characterizes the detectors even at high-bias-voltage operation (9000 V cm−1), with energy resolutions (FWHM) of 4% (0.9 keV), 1.7% (1 keV) and 1.3% (1.6 keV) at 22.1, 59.5 and 122.1 keV, respectively. Charge-sharing investigations were performed with both uncollimated and collimated synchrotron X-ray beams with particular attention to the mitigation of the charge losses at the inter-pixel gap region. High-rate measurements demonstrated the absence of high-flux radiation-induced polarization phenomena up to 2 × 106 photons mm−2 s−1. These activities are in the framework of an international collaboration on the development of energy-resolved photon-counting systems for high-flux energy-resolved X-ray imaging.	Mar 2020
I15-Extreme Conditions	The HXD95: a modified Bassett-type hydrothermal diamond-anvil cell for in situ XRD experiments up to 5 GPa and 1300 K Marion Louvel , James W. E. Drewitt , Allan Ross , Richard Thwaites , Benedict J. Heinen , Dean S. Keeble , Christine M. Beavers , Michael J. Walter , Simone Anzellini Journal Of Synchrotron Radiation 27 DOI: 10.1107/S1600577519016801 Diamond Proposal Number(s): [19339] Open Access Show Abstract ▼ Abstract: A new diamond-anvil cell apparatus for in situ synchrotron X-ray diffraction measurements of liquids and glasses, at pressures from ambient to 5 GPa and temperatures from ambient to 1300 K, is reported. This portable setup enables in situ monitoring of the melting of complex compounds and the determination of the structure and properties of melts under moderately high pressure and high temperature conditions relevant to industrial processes and magmatic processes in the Earth's crust and shallow mantle. The device was constructed according to a modified Bassett-type hydrothermal diamond-anvil cell design with a large angular opening (θ = 95°). This paper reports the successful application of this device to record in situ synchrotron X-ray diffraction of liquid Ga and synthetic PbSiO3 glass to 1100 K and 3 GPa.	Mar 2020
I13-2-Diamond Manchester Imaging	Phase-contrast 3D tomography of HeLa cells grown in PLLA polymer electrospun scaffolds using synchrotron X-rays A. Bhartiya , K. Madi , C. M. Disney , L. Courtois , A. Jupe , F. Zhang , A. J. Bodey , P. Lee , C. Rau , Ian Robinson , M. Yusuf Journal Of Synchrotron Radiation 27, 158 - 163 DOI: 10.1107/S1600577519015583 Diamond Proposal Number(s): [14187] Show Abstract ▼ Abstract: Advanced imaging is useful for understanding the three-dimensional (3D) growth of cells. X-ray tomography serves as a powerful noninvasive, nondestructive technique that can fulfill these purposes by providing information about cell growth within 3D platforms. There are a limited number of studies taking advantage of synchrotron X-rays, which provides a large field of view and suitable resolution to image cells within specific biomaterials. In this study, X-ray synchrotron radiation microtomography at Diamond Light Source and advanced image processing were used to investigate cellular infiltration of HeLa cells within poly L-lactide (PLLA) scaffolds. This study demonstrates that synchrotron X-rays using phase contrast is a useful method to understand the 3D growth of cells in PLLA electrospun scaffolds. Two different fiber diameter (2 and 4 µm) scaffolds with different pore sizes, grown over 2, 5 and 8 days in vitro, were examined for infiltration and cell connectivity. After performing visualization by segmentation of the cells from the fibers, the results clearly show deeper cell growth and higher cellular interconnectivity in the 4 µm fiber diameter scaffold. This indicates the potential for using such 3D technology to study cell–scaffold interactions for future medical use.	Jan 2020
I13-2-Diamond Manchester Imaging	Full-field spectroscopic measurement of the X-ray beam from a multilayer monochromator using a hyperspectral X-ray camera Matthieu N Boone , Frederic Van Assche , Sander Vanheule , Silvia Cipiccia , Hongchang Wang , Laszlo Vincze , Luc Van Hoorebeke Journal Of Synchrotron Radiation 27 DOI: 10.1107/S1600577519015212 Diamond Proposal Number(s): [14696, 19579, 21682] Open Access Show Abstract ▼ Abstract: Multilayer monochromator devices are commonly used at (imaging) beamlines of synchrotron facilities to shape the X-ray beam to relatively small bandwidth and high intensity. However, stripe artefacts are often observed and can deteriorate the image quality. Although the intensity distribution of these artefacts has been described in the literature, their spectral distribution is currently unknown. To assess the spatio-spectral properties of the monochromated X-ray beam, the direct beam has been measured for the first time using a hyperspectral X-ray detector. The results show a large number of spectral features with different spatial distributions for a [Ru, B4C] strip monochromator, associated primarily with the higher-order harmonics of the undulator and monochromator. It is found that their relative contributions are sufficiently low to avoid an influence on the imaging data. The [V, B4C] strip suppresses these high-order harmonics even more than the former, yet at the cost of reduced efficiency.	Dec 2019
I18-Microfocus Spectroscopy	Iterative energy self-calibration of Fe XANES spectra Michael W. M. Jones , Guilherme Mallmann , Jeremy L. Wykes , Joseph Knafelc , Scott E. Bryan , Daryl L. Howard Journal Of Synchrotron Radiation 27 DOI: 10.1107/S1600577519014267 Show Abstract ▼ Abstract: Determining the oxidation state of Fe through parameterization of X-ray absorption near-edge structure (XANES) spectral features is highly dependent on accurate and repeatable energy calibration between spectra. Small errors in energy calibration can lead to vastly different interpretations. While simultaneous measurement of a reference foil is often undertaken on X-ray spectroscopy beamlines, other beamlines measure XANES spectra without a reference foil and therefore lack a method for correcting energy drift. Here a method is proposed that combines two measures of Fe oxidation state taken from different parts of the spectrum to iteratively correct for an unknown energy offset between spectra, showing successful iterative self-calibration not only during individual beam time but also across different beamlines.	Nov 2019
I24-Microfocus Macromolecular Crystallography	Reducing sample consumption for serial crystallography using acoustic drop ejection Bradley Davy , Danny Axford , John H. Beale , Agata Butryn , Peter Docker , Ali Ebrahim , Gabriel Leen , Allen M. Orville , Robin L. Owen , Pierre Aller Journal Of Synchrotron Radiation 26 DOI: 10.1107/S1600577519009329 Diamond Proposal Number(s): [14493, 19458] Open Access Show Abstract ▼ Abstract: Efficient sample delivery is an essential aspect of serial crystallography at both synchrotrons and X-ray free-electron lasers. Rastering fixed target chips through the X-ray beam is an efficient method for serial delivery from the perspectives of both sample consumption and beam time usage. Here, an approach for loading fixed targets using acoustic drop ejection is presented that does not compromise crystal quality, can reduce sample consumption by more than an order of magnitude and allows serial diffraction to be collected from a larger proportion of the crystals in the slurry.	Sep 2019
I24-Microfocus Macromolecular Crystallography	Radiation-damage investigation of a DNA 16-mer Valeria Bugris , Veronika Harmat , Györgyi Ferenc , Sándor Brockhauser , Ian Carmichael , Elspeth F. Garman Journal Of Synchrotron Radiation 26 DOI: 10.1107/S160057751900763X Diamond Proposal Number(s): [18069] Show Abstract ▼ Abstract: In macromolecular crystallography, a great deal of effort has been invested in understanding radiation-damage progression. While the sensitivity of protein crystals has been well characterized, crystals of DNA and of DNA–protein complexes have not thus far been studied as thoroughly. Here, a systematic investigation of radiation damage to a crystal of a DNA 16-mer diffracting to 1.8 Å resolution and held at 100 K, up to an absorbed dose of 45 MGy, is reported. The RIDL (Radiation-Induced Density Loss) automated computational tool was used for electron-density analysis. Both the global and specific damage to the DNA crystal as a function of dose were monitored, following careful calibration of the X-ray flux and beam profile. The DNA crystal was found to be fairly radiation insensitive to both global and specific damage, with half of the initial diffraction intensity being lost at an absorbed average diffraction-weighted dose, D1/2, of 19 MGy, compared with 9 MGy for chicken egg-white lysozyme crystals under the same beam conditions but at the higher resolution of 1.4 Å. The coefficient of sensitivity of the DNA crystal was 0.014 Å2 MGy−1, which is similar to that observed for proteins. These results imply that the significantly greater radiation hardness of DNA and RNA compared with protein observed in a DNA–protein complex and an RNA–protein complex could be due to scavenging action by the protein, thereby protecting the DNA and RNA in these studies. In terms of specific damage, the regions of DNA that were found to be sensitive were those associated with some of the bound calcium ions sequestered from the crystallization buffer. In contrast, moieties farther from these sites showed only small changes even at higher doses.	Jul 2019
I24-Microfocus Macromolecular Crystallography	Direct measurement of X-ray-induced heating of microcrystals Anna Warren , Danny Axford , Robin L. Owen Journal Of Synchrotron Radiation 26 DOI: 10.1107/S1600577519003849 Open Access Show Abstract ▼ Abstract: Temperature control is a key aspect of macromolecular crystallography, with the technique of cryocooling routinely being used to mitigate X-ray-induced damage. Beam-induced heating could cause the temperature of crystals to rise above the glass transition temperature, greatly increasing the rate of damage. X-ray-induced heating of ruby crystals of 20–40 µm in size has been quantified non-invasively by monitoring the emission wavelengths of X-ray-induced fluorescence during exposure to the X-ray beam. For the beam sizes and dose rates typically used in macromolecular crystallography, the temperature rises are of the order of 20 K. The temperature changes observed are compared with models in the literature and can be used as a validation tool for future models.	Jul 2019
I12-JEEP: Joint Engineering, Environmental and Processing	A kinetic and mechanistic study into the transformation of calcium sulfate hemihydrate to dihydrate Sebastian Gurgul , Gabriel Seng , Gareth Williams Journal Of Synchrotron Radiation DOI: 10.1107/S1600577519001929 Diamond Proposal Number(s): [16022] Open Access Show Abstract ▼ Abstract: The conversion of CaSO4·0.5H2O to CaSO4·2H2O is of great importance industrially, being the reaction behind plasterboard production and the setting of medical plasters. A detailed kinetic and mechanistic study of this process was conducted using time-resolved synchrotron X-ray diffraction in this work. The CaSO4·2H2O product is very similar regardless of whether the α- or β-form of CaSO4·0.5H2O is used as the starting material, but the reaction process is very different. The induction time is usually shorter for α-CaSO4·0.5H2O than β-CaSO4·0.5H2O, and a greater conversion percentage is observed with the former (although in neither case does the reaction proceed to 100% completion). The temperature of the system, widely used in industry as an indirect measure of the extent of the hydration process, is found to be a poor proxy for this, with the maximum temperature reached well before the reaction is complete. The Avrami–Erofe'ev and Gualtieri models could both be fitted to the experimental data, with the fits being substantially closer in the case of α-CaSO4·0.5H2O. The rate of reaction in the Avrami model tends to increase with the amount of gypsum seeds added to accelerate the process, and the importance of nucleation declines. The Gualtieri analysis suggested that the rate of nucleation increases substantially with the amount of seeds added, while there are less distinct changes in the rate of crystal growth. At low seed concentrations (<0.5% w/w) the rate of crystal growth is greater than the rate of nucleation, but at concentrations above 0.5% w/w nucleation is faster. These findings represent the first synchrotron study of the conversion of CaSO4·0.5H2O to CaSO4·2H2O, and will be of importance to gypsum producers globally.	May 2019
Optics	Structure, stress and optical properties of Cr/C multilayers for the tender X-ray range Jiangtao Feng , Qiushi Huang , Hongchang Wang , Xiaowei Yang , Angelo Giglia , Chun Xie , Zhanshan Wang Journal Of Synchrotron Radiation 26 DOI: 10.1107/S1600577519001668 Show Abstract ▼ Abstract: Cr/C multilayer optics are a suitable choice for the tender X-ray range (1–4 keV) that covers the K absorption edges of P, S, Cl and 3d transition metals as well as the L absorption edges of 4d transition metals. In particular, these optics are studied in order to optimize the optical properties of collimated plane-grating monochromators. In this paper, the structure, stress and optical properties of Cr/C multilayers (fabricated using direct-current magnetron sputtering) with bi-layer number of 20 and the same period (about 11.64 nm) but different Cr thickness ratio (0.20–0.80) are investigated. Firstly, the grazing-incidence X-ray reflectivity at 8.04 keV was measured. These measurements were fitted assuming a multilayer structure with a four-layer and non-periodic model. Results and fitting show that interface widths increase with the Cr thickness ratio. The results obtained from X-ray diffraction at 8.04 keV were consistent with high-resolution transmission electron microscopy which showed an increase in grain size of the Cr layers. In addition, the stresses of the Cr/C multilayers have been measured and the results show that the stress value approaches zero when the Cr thickness ratio is about 0.45. The reflectivity of a Cr/C multilayer with Cr thickness ratio of 0.37 was measured and reaches 26.6% at 1.04 keV. The measured reflectivity matches very well with the predicted value using the four-layer and non-periodic model, which confirmed the viability of the prediction. Thus, the reflectivity at 1.04 keV of a Cr/C multilayer with different Cr thickness ratio was predicted and was found to drastically decrease when the Cr thickness ratio is larger than 0.37. It has been determined that a Cr thickness ratio value of 0.37 is the best choice for a Cr/C multilayer in view of high reflectivity and low stress.	May 2019

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