High‐performance X‐ray detectors for the new powder diffraction beamline I11 at Diamond

The design and performance characterization of a new light‐weight and compact X‐ray scintillation detector is presented. The detectors are intended for use on the new I11 powder diffraction beamline at the third‐generation Diamond synchrotron facility where X‐ray beams of high photon brightness are generated by insertion devices. The performance characteristics of these detection units were measured first using a radioactive source (efficiency of detection and background count rate) and then synchrotron X‐rays (peak stability, light yield linearity and response consistency). Here, the results obtained from these tests are reported, and the suitability of the design for the Diamond powder beamline is demonstrated by presenting diffraction data obtained from a silicon powder standard using a prototype multicrystal analyser stage.     

Implementation of a beam deflection system for studies of liquid interfaces on beamline I07 at Diamond

X‐ray optics, based on a double‐crystal deflection scheme, that enable reflectivity measurements from liquid surfaces/interfaces have been designed, built and commissioned on beamline I07 at Diamond Light Source. This system is able to deflect the beam onto a fixed sample position located at the centre of a five‐circle diffractometer. Thus the incident angle can be easily varied without moving the sample, and the reflected beam is tracked either by a moving Pilatus 100K detector mounted on the diffractometer arm or by a stationary Pilatus 2M detector positioned appropriately for small‐angle scattering. Thus the system can easily combine measurements of the reflectivity from liquid interfaces (Q_z > 1 Å^?1) with off‐specular data collection, both in the form of grazing‐incidence small‐angle X‐ray scattering (GISAXS) or wider‐angle grazing‐incidence X‐ray diffraction (GIXD). The device allows operation over the energy range 10–28 keV.     

Status of PRESS-MAG-O: The experimental apparatus to probe materials and phenomena under extreme conditions at Frascati

In this contribution we up-to-date the status of the PRESS-MAG-O device, a new instrument under commissioning at the INFN designed to perform magnetic and spectroscopic experiments on samples under extreme conditions. The system has been designed to work at SINBAD, the IR synchrotron radiation beamline operational at DAΦNE. The instrument, that is the result of a significant R&D, will allow performing concurrent high harmonic ac magnetic susceptibility measurements and magneto-optic experiments on a sample under high pressure, with a variable DC magnetic field in a wide temperature range. The vacuum vessel has been designed with four crossing windows to allow optical measurements in the transmission geometry on the sample loaded inside a Diamond Anvil Cell. A new superconducting miniaturized micro-SQUID gradiometer has been also developed to detect the low magnetic signal of the sample and a customized optical system has also been designed to perform IR synchrotron radiation experiments.     

A flow‐through reaction cell for in situ X‐ray diffraction and absorption studies of heterogeneous powder–liquid reactions and phase transformations

A portable powder–liquid high‐corrosion‐resistant reaction cell has been designed to follow in situ reactions by X‐ray powder diffraction (XRD) and X‐ray absorption spectroscopy (XAS) techniques. The cell has been conceived to be mounted on the experimental stations for diffraction and absorption of the Spanish CRG SpLine‐BM25 beamline at the European Synchrotron Radiation Facility. Powder reactants and/or products are kept at a fixed position in a vertical geometry in the X‐ray pathway by a porous membrane, under forced liquid reflux circulation. Owing to the short pathway of the X‐ray beam through the cell, XRD and XAS measurements can be carried out in transmission configuration/mode. In the case of the diffraction technique, data can be collected with either a point detector or a two‐dimensional CCD detector, depending on specific experimental requirements in terms of space or time resolution. Crystallization processes, heterogeneous catalytic processes and several varieties of experiments can be followed by these techniques with this cell. Two experiments were carried out to demonstrate the cell feasibility: the phase transformations of layered titanium phosphates in boiling aqueous solutions of phosphoric acid, and the reaction of copper carbonate and l ‐isoleucine amino acid powders in boiling aqueous solution. In this last case the shrinking of the solid reactants and the formation of Cu(isoleucine)₂ is observed. The crystallization processes and several phase transitions have been observed during the experiments, as well as an unexpected reaction pathway.     

A twelve‐analyzer detector system for high‐resolution powder diffraction

A dedicated high‐resolution high‐throughput X‐ray powder diffraction beamline has been constructed at the Advanced Photon Source (APS). In order to achieve the goals of both high resolution and high throughput in a powder instrument, a multi‐analyzer detector system is required. The design and performance of the 12‐analyzer detector system installed on the powder diffractometer at the 11‐BM beamline of APS are presented.     

I19, the small‐molecule single‐crystal diffraction beamline at Diamond Light Source

The dedicated small‐molecule single‐crystal X‐ray diffraction beamline (I19) at Diamond Light Source has been operational and supporting users for over three years. I19 is a high‐flux tunable‐wavelength beamline and its key details are described in this article. Much of the work performed on the beamline involves structure determination from small and weakly diffracting crystals. Other experiments that have been supported to date include structural studies at high pressure, studies of metastable species, variable‐temperature crystallography, studies involving gas exchange in porous materials and structural characterizations that require analysis of the diffuse scattering between Bragg reflections. A range of sample environments to facilitate crystallographic studies under non‐ambient conditions are available as well as a number of options for automation. An indication of the scope of the science carried out on the beamline is provided by the range of highlights selected for this paper.     

I18 – the microfocus spectroscopy beamline at the Diamond Light Source

The design and performance of the microfocus spectroscopy beamline at the Diamond Light Source are described. The beamline is based on a 27 mm‐period undulator to give an operable energy range between 2 and 20.7 keV, enabling it to cover the K‐edges of the elements from P to Mo and the L₃‐edges from Sr to Pu. Micro‐X‐ray fluorescence, micro‐EXAFS and micro‐X‐ray diffraction have all been achieved on the beamline with a spot size of ～3 µm. The principal optical elements of the beamline consist of a toroid mirror, a liquid‐nitrogen‐cooled double‐crystal monochromator and a pair of bimorph Kirkpatrick–Baez mirrors. The performance of the optics is compared with theoretical values and a few of the early experimental results are summarized.     

Using an in‐vacuum CCD detector for simultaneous small‐ and wide‐angle scattering at beamline X9

The implementation of simultaneous small‐ and wide‐angle X‐ray scattering at beamline X9 of the National Synchrotron Light Source is described. By utilizing an in‐vacuum CCD detector with a truncated cone‐shaped head and positioned at ～20° off‐axis from the direct beam, the overlap of the scattering angle coverage between the wide‐angle detector and the conventional small‐angle detector is maximized. The combined q‐range for measurements in transmission geometry is typically 0.006–2.0 Å^?1 at 13.5 keV, with overlapping data within the range ～0.1–0.2 Å^?1. Simultaneous data collection can also be performed in grazing‐incident measurements of flat substrate‐supported samples, in which case the wide‐angle detector can collect the scattering data along the sample normal as well as parallel to the sample surface without blocking the direct beam. Data processing and correction procedures will be discussed and examples presented.     

Technical Report: The Fastest Relativistic Jets from Quasars and Active Galactic Nuclei

This workshop was held to gather scientists interested in exploiting beamlines I06 and I10 of the Surface and Interfaces Village at Diamond Light Source from June 10–11, 2009. Sarnjeet Dhesi introduced the meeting with a short explanation of the village structure at Diamond. This village includes the Nanoscience beamline (I06), catering for soft X-rays for Photo-Emission Electron Microscopy (PEEM) and X-ray Magnetic Circular and Linear Dichroism (XMCD and XMLD), and the Beam Line for Advanced Dichroism Experiments (BLADE, beamline I10), which is a polarized soft X-ray beam for XMCD, XMLD, and soft X-ray diffraction. I06 has been operational for over two years, while I10 is scheduled to come on-line in late 2010. In addition, there are two surface science beamlines (I07 and I09) in the village dedicated to surface diffraction and X-ray standing waves.     

First experiments on the Australian Synchrotron Imaging and Medical beamline,including investigations of the effective source size in respect of X‐ray imaging

The Imaging and Medical beamline at the Australian Synchrotron achieved `first light' in December 2008. Here, the first experiments performed on the beamline are reported, which involved both X‐ray imaging and tomography studies for a range of samples. The use of a plastic‐edge phantom for quantitative measurements of contrast and resolution proved to be very instructive and helped to confirm certain parameter values such as the effective horizontal source size, detector resolution and average X‐ray energy for the polychromatic beam.     

Fabrication and testing of a newly designed slit system for depth‐resolved X‐ray diffraction measurements

A new system of slits called `spiderweb slits' have been developed for depth‐resolved powder or polycrystalline X‐ray diffraction measurements. The slits act on diffracted X‐rays to select a particular gauge volume of sample, while absorbing diffracted X‐rays from outside of this volume. Although the slit geometry is to some extent similar to that of previously developed conical slits or spiral slits, this new design has advantages over the previous ones in use for complex heterogeneous materials and in situ and operando diffraction measurements. For example, the slits can measure a majority of any diffraction cone for any polycrystalline material, over a continuous range of diffraction angles, and work for X‐ray energies of tens to hundreds of kiloelectronvolts. The design is generated and optimized using ray‐tracing simulations, and fabricated through laser micromachining. The first prototype was successfully tested at the X17A beamline at the National Synchrotron Light Source, and shows similar performance to simulations, demonstrating gauge volume selection for standard powders, for all diffraction peaks over angles of 2–10°. A similar, but improved, design will be implemented at the X‐ray Powder Diffraction beamline at the National Synchrotron Light Source II.     

Multi‐use high/low‐temperature and pressure compatible portable chamber for in situ grazing‐incidence X‐ray scattering studies

The multipurpose portable ultra‐high‐vacuum‐compatible chamber described in detail in this article has been designed to carry out grazing‐incidence X‐ray scattering techniques on the BM25‐SpLine CRG beamline at the ESRF. The chamber has a cylindrical form, built on a 360° beryllium double‐ended conflate flange (CF) nipple. The main advantage of this chamber design is the wide sample temperature range, which may be varied between 60 and 1000 K. Other advantages of using a cylinder are that the wall thickness is reduced to a minimum value, keeping maximal solid angle accessibility and keeping wall absorption of the incoming X‐ray beam constant. The heat exchanger is a customized compact liquid‐nitrogen (LN2) continuous‐flow cryostat. LN2 is transferred from a storage Dewar through a vacuum‐isolated transfer line to the heat exchanger. The sample is mounted on a molybdenum support on the heat exchanger, which is equipped with a BORALECTRIC heater element. The chamber versatility extends to the operating pressure, ranging from ultra‐high vacuum (<10^?10 mbar) to high pressure (up to 3 × 10³ mbar). In addition, it is equipped with several CF ports to allocate auxiliary components such as capillary gas‐inlet, viewports, leak valves, ion gun, turbo pump, etc., responding to a large variety of experiment requirements. A movable slits set‐up has been foreseen to reduce the background and diffuse scattering produced at the beryllium wall. Diffraction data can be recorded either with a point detector or with a bi‐dimensional CCD detector, or both detectors simultaneously. The system has been designed to carry out a multitude of experiments in a large variety of environments. The system feasibility is demonstrated by showing temperature‐dependence grazing‐incidence X‐ray diffraction and conductivity measurements on a 20 nm‐thick La_0.7Ca_0.3MnO₃ thin film grown on a SrTiO₃(001) substrate.     

Energy-dispersive X-ray diffraction beamline at Indus-2 synchrotron source

An energy-dispersive X-ray diffraction beamline has been designed, developed and commissioned at BL-11 bending magnet port of the Indian synchrotron source, Indus-2. The performance of this beamline has been benchmarked by measuring diffraction patterns from various elemental metals and standard inorganic powdered samples. A few recent high-pressure investigations are presented to demonstrate the capabilities of the beamline.     

The multi‐purpose hard X‐ray beamline BL10 at the DELTA storage ring

The layout and the characteristics of the hard X‐ray beamline BL10 at the superconducting asymmetric wiggler at the 1.5 GeV Dortmund Electron Accelerator DELTA are described. This beamline is equipped with a Si(111) channel‐cut monochromator and is dedicated to X‐ray studies in the spectral range from ～4 keV to ～16 keV photon energy. There are two different endstations available. While X‐ray absorption studies in different detection modes (transmission, fluorescence, reflectivity) can be performed on a designated table, a six‐axis kappa diffractometer is installed for X‐ray scattering and reflectivity experiments. Different detector set‐ups are integrated into the beamline control software, i.e. gas‐filled ionization chambers, different photodiodes, as well as a Pilatus 2D‐detector are permanently available. The performance of the beamline is illustrated by high‐quality X‐ray absorption spectra from several reference compounds. First applications include temperature‐dependent EXAFS experiments from liquid‐nitrogen temperature in a bath cryostat up to ～660 K by using a dedicated furnace. Besides transmission measurements, fluorescence detection for dilute sample systems as well as surface‐sensitive reflection‐mode experiments are presented.     

A new small‐angle X‐ray scattering set‐up on the crystallography beamline I711 at MAX‐lab

A small‐angle X‐ray scattering (SAXS) set‐up has recently been developed at beamline I711 at the MAX II storage ring in Lund (Sweden). An overview of the required modifications is presented here together with a number of application examples. The accessible q range in a SAXS experiment is 0.009–0.3 Å^?1 for the standard set‐up but depends on the sample‐to‐detector distance, detector offset, beamstop size and wavelength. The SAXS camera has been designed to have a low background and has three collinear slit sets for collimating the incident beam. The standard beam size is about 0.37 mm × 0.37 mm (full width at half‐maximum) at the sample position, with a flux of 4 × 10¹⁰ photons s^?1 and λ = 1.1 Å. The vacuum is of the order of 0.05 mbar in the unbroken beam path from the first slits until the exit window in front of the detector. A large sample chamber with a number of lead‐throughs allows different sample environments to be mounted. This station is used for measurements on weakly scattering proteins in solutions and also for colloids, polymers and other nanoscale structures. A special application supported by the beamline is the effort to establish a micro‐fluidic sample environment for structural analysis of samples that are only available in limited quantities. Overall, this work demonstrates how a cost‐effective SAXS station can be constructed on a multipurpose beamline.     

Protein crystallography beamline (PX‐BL21) at Indus‐2 synchrotron

The protein crystallography beamline (PX‐BL21), installed at the 1.5 T bending‐magnet port at the Indian synchrotron (Indus‐2), is now available to users. The beamline can be used for X‐ray diffraction measurements on a single crystal of macromolecules such as proteins, nucleic acids and their complexes. PX‐BL21 has a working energy range of 5–20 keV for accessing the absorption edges of heavy elements commonly used for phasing. A double‐crystal monochromator [Si(111) and Si(220)] and a pair of rhodium‐coated X‐ray mirrors are used for beam monochromatization and manipulation, respectively. This beamline is equipped with a single‐axis goniometer, Rayonix MX225 CCD detector, fluorescence detector, cryogenic sample cooler and automated sample changer. Additional user facilities include a workstation for on‐site data processing and a biochemistry laboratory for sample preparation. In this article the beamline, other facilities and some recent scientific results are briefly described.     

Energy resolution of the CdTe‐XPAD detector: calibration and potential for Laue diffraction measurements on protein crystals

The XPAD3S‐CdTe, a CdTe photon‐counting pixel array detector, has been used to measure the energy and the intensity of the white‐beam diffraction from a lysozyme crystal. A method was developed to calibrate the detector in terms of energy, allowing incident photon energy measurement to high resolution (approximately 140 eV), opening up new possibilities in energy‐resolved X‐ray diffraction. In order to demonstrate this, Laue diffraction experiments were performed on the bending‐magnet beamline METROLOGIE at Synchrotron SOLEIL. The X‐ray energy spectra of diffracted spots were deduced from the indexed Laue patterns collected with an imaging‐plate detector and then measured with both the XPAD3S‐CdTe and the XPAD3S‐Si, a silicon photon‐counting pixel array detector. The predicted and measured energy of selected diffraction spots are in good agreement, demonstrating the reliability of the calibration method. These results open up the way to direct unit‐cell parameter determination and the measurement of high‐quality Laue data even at low resolution. Based on the success of these measurements, potential applications in X‐ray diffraction opened up by this type of technology are discussed.     

Characterization of wax as a potential diffraction intensity standard for macromolecular crystallography beamlines

A number of commercially available waxes in the form of thin disc samples have been investigated as possible diffraction intensity standards for macromolecular crystallography synchrotron beamlines. Synchrotron X‐ray powder diffraction measurements show that beeswax offers the best performance of these waxes owing to its polycrystallinity. Crystallographic lattice parameters and diffraction intensities were examined between 281 and 309 K, and show stable and predictable thermal behaviour. Using an X‐ray beam of known incident flux at λ = 1 Å, the diffraction power of two strong Bragg reflections for beeswax were quantified as a function of sample thickness and normalized to 10¹⁰ photons s^?1. To demonstrate its feasibility as a diffraction intensity standard, test measurements were then performed on a new third‐generation macromolecular crystallography synchrotron beamline.     

X‐Treme beamline at SLS: X‐ray magnetic circular and linear dichroism at high field and low temperature

X‐Treme is a soft X‐ray beamline recently built in the Swiss Light Source at the Paul Scherrer Institut in collaboration with École Polytechnique Fédérale de Lausanne. The beamline is dedicated to polarization‐dependent X‐ray absorption spectroscopy at high magnetic fields and low temperature. The source is an elliptically polarizing undulator. The end‐station has a superconducting 7 T–2 T vector magnet, with sample temperature down to 2 K and is equipped with an in situ sample preparation system for surface science. The beamline commissioning measurements, which show a resolving power of 8000 and a maximum flux at the sample of 4.7 × 10¹² photons s^?1, are presented. Scientific examples showing X‐ray magnetic circular and X‐ray magnetic linear dichroism measurements are also presented.     

The small‐angle and wide‐angle X‐ray scattering set‐up at beamline BL9 of DELTA

The multi‐purpose experimental endstation of beamline BL9 at the Dortmund Electron Accelerator (DELTA) is dedicated to diffraction experiments in grazing‐incidence geometry, reflectivity and powder diffraction measurements. Moreover, fluorescence analysis and inelastic X‐ray scattering experiments can be performed. Recently, a new set‐up for small‐angle and wide‐angle X‐ray scattering utilizing detection by means of an image‐plate scanner was installed and is described in detail here. First small‐angle X‐ray scattering experiments on aqueous solutions of lysozyme with different cosolvents and of staphylococcal nuclease are discussed. The application of the set‐up for texture analysis is emphasized and a study of the crystallographic texture of natural bio‐nanocomposites, using lobster and crab cuticles as model materials, is presented.