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119 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
I15-1-X-ray Pair Distribution Function (XPDF)	Fast operando X-ray pair distribution function using the DRIX electrochemical cell Maria Diaz-lopez , Geoffrey L. Cutts , Phoebe K. Allan , Dean S. Keeble , Allan Ross , Valerie Pralong , Georg Spiekermann , Philip A. Chater Journal Of Synchrotron Radiation 27 DOI: 10.1107/S160057752000747X Diamond Proposal Number(s): [20893, 20094] Open Access Show Abstract ▼ Abstract: In situ electrochemical cycling combined with total scattering measurements can provide valuable structural information on crystalline, semi-crystalline and amorphous phases present during (dis)charging of batteries. In situ measurements are particularly challenging for total scattering experiments due to the requirement for low, constant and reproducible backgrounds. Poor cell design can introduce artefacts into the total scattering data or cause inhomogeneous electrochemical cycling, leading to poor data quality or misleading results. This work presents a new cell design optimized to provide good electrochemical performance while performing bulk multi-scale characterizations based on total scattering and pair distribution function methods, and with potential for techniques such as X-ray Raman spectroscopy. As an example, the structural changes of a nanostructured high-capacity cathode with a disordered rock-salt structure and composition Li4Mn2O5 are demonstrated. The results show that there is no contribution to the recorded signal from other cell components, and a very low and consistent contribution from the cell background.	Sep 2020
	A passive hutch-cooling system for achieving high thermal-stability operation at the Nanoprobe beamline, Diamond Light Source Fernando Cacho-nerin , Julia E. Parker , Paul D. Quinn Journal Of Synchrotron Radiation 27 DOI: 10.1107/S1600577520004932 Open Access Show Abstract ▼ Abstract: The development of low-emittance storage rings and the rapid developments in nano-optics and imaging techniques are leading to decreasing X-ray spot sizes and increasing requirements on the environmental and mechanical stability of beamline components. In particular, temperature stability in the experimental hutches is critical to minimize uncontrolled displacements caused by thermal expansion and ensure consistent performance. Here, the design and thermal performance of the experimental hutches of the Nanoprobe beamline at Diamond Light Source are described, where a standard deviation of the room temperature down to 0.017°C over extended periods is demonstrated. The rooms are kept at constant temperature using water-cooled radiant panels which line the ceiling and walls. Radiant panels are relatively common in high-end electron microscopy rooms, but this is the first demonstration of their use for fine temperature control in an X-ray hutch and may provide a useful basis for future upgrades at upcoming low-emittance sources.	Jul 2020
I18-Microfocus Spectroscopy	A single-crystal diamond X-ray pixel detector with embedded graphitic electrodes C. Bloomer , M. E. Newton , G. Rehm , P. S. Salter Journal Of Synchrotron Radiation 27 DOI: 10.1107/S160057752000140X Open Access Show Abstract ▼ Abstract: The first experimental results from a new transmissive diagnostic instrument for synchrotron X-ray beamlines are presented. The instrument utilizes a single-crystal chemical-vapour-deposition diamond plate as the detector material, with graphitic wires embedded within the bulk diamond acting as electrodes. The resulting instrument is an all-carbon transmissive X-ray imaging detector. Within the instrument's transmissive aperture there is no surface metallization that could absorb X-rays, and no surface structures that could be damaged by exposure to synchrotron X-ray beams. The graphitic electrodes are fabricated in situ within the bulk diamond using a laser-writing technique. Two separate arrays of parallel graphitic wires are fabricated, running parallel to the diamond surface and perpendicular to each other, at two different depths within the diamond. One array of wires has a modulated bias voltage applied; the perpendicular array is a series of readout electrodes. X-rays passing through the detector generate charge carriers within the bulk diamond through photoionization, and these charge carriers travel to the nearest readout electrode under the influence of the modulated electrical bias. Each of the crossing points between perpendicular wires acts as an individual pixel. The simultaneous read-out of all pixels is achieved using a lock-in technique. The parallel wires within each array are separated by 50 µm, determining the pixel pitch. Readout is obtained at 100 Hz, and the resolution of the X-ray beam position measurement is 600 nm for a 180 µm size beam.	May 2020
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
I16-Materials and Magnetism	High-pressure developments for resonant X-ray scattering experiments at I16 I. Povedano , A. Bombardi , D. G. Porter , M. Burt , S. Green , K. V. Kamenev Journal Of Synchrotron Radiation 27 DOI: 10.1107/S1600577519016308 Diamond Proposal Number(s): [17731, 19890, 20778, 21376] Show Abstract ▼ Abstract: An experimental setup to perform high-pressure resonant X-ray scattering (RXS) experiments at low temperature on I16 at Diamond Light Source is presented. The setup consists of a membrane-driven diamond anvil cell, a panoramic dome and an optical system that allows pressure to be measured in situ using the ruby fluorescence method. The membrane cell, inspired by the Merrill–Bassett design, presents an asymmetric layout in order to operate in a back-scattering geometry, with a panoramic aperture of 100° in the top and a bottom half dedicated to the regulation and measurement of pressure. It is specially designed to be mounted on the cold finger of a 4 K closed-cycle cryostat and actuated at low-temperature by pumping helium into the gas membrane. The main parts of the body are machined from a CuBe alloy (BERYLCO 25) and, when assembled, it presents an approximate height of 20–21 mm and fits into a 57 mm diameter. This system allows different materials to be probed using RXS in a range of temperatures between 30 and 300 K and has been tested up to 20 GPa using anvils with a culet diameter of 500 µm under quasi-cryogenic conditions. Detailed descriptions of different parts of the setup, operation and the developed methodology are provided here, along with some preliminary experimental results.	Mar 2020
	The HARE chip for efficient time-resolved serial synchrotron crystallography Pedram Mehrabi , Henrike Mueller-werkmeister , Jan-philipp Leimkohl , Hendrik Schikora , Jelena Ninkovic , Silvia Krivokuca , Ladislav Andriček , Sascha W. Epp , Darren A. Sherrell , Robin L. Owen , Arwen R. Pearson , Friedjof Tellkamp , Eike Schulz , R. J. Dwayne Miller Journal Of Synchrotron Radiation 27, 360 - 370 DOI: 10.1107/S1600577520000685 Open Access Show Abstract ▼ Abstract: Serial synchrotron crystallography (SSX) is an emerging technique for static and time-resolved protein structure determination. Using specifically patterned silicon chips for sample delivery, the `hit-and-return' (HARE) protocol allows for efficient time-resolved data collection. The specific pattern of the crystal wells in the HARE chip provides direct access to many discrete time points. HARE chips allow for optical excitation as well as on-chip mixing for reaction initiation, making a large number of protein systems amenable to time-resolved studies. Loading of protein microcrystals onto the HARE chip is streamlined by a novel vacuum loading platform that allows fine-tuning of suction strength while maintaining a humid environment to prevent crystal dehydration. To enable the widespread use of time-resolved serial synchrotron crystallography (TR-SSX), detailed technical descriptions of a set of accessories that facilitate TR-SSX workflows are provided.	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 , I. K. 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

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