Synchrotron radiation in archaeometry

January 2008 was the time of the official opening of SOLEIL's beamlines and guest house. This transition from construction to operational phase was made possible after commissioning of the 17°C water circuits of the beamlines. Users have access to eleven beamlines, from infrared to hard X-ray (AILES, SMIS, DESIRS, CASSIOPEE, TEMPO, DIFFABS, ODE, CRISTAL, SAMBA, PROXIMA1 and SWING). The LUCIA beamline, which has been operational on SLS since June 2004, will be installed at SOLEIL from mid-2008, and the XPEEM station of the future “soft X-ray microscopy” beamline is already producing fascinating XMCD and XMLD results at ELETTRA. Five beamlines are under construction.     

ALBA Synchrotron Facility

ALBA is the Spanish synchrotron facility located in the area of Barcelona. It is a low-emittance, 3 GeV machine having, at present, seven state-of-the-art operating beamlines covering soft and hard X-rays. The hard X-ray beamlines comprise macromolecular crystallography, non-crystalline diffraction (SAXS and WAXS), high-resolution powder diffraction, and absorption spectroscopy. The soft X-ray beamlines include a photoemission beamline with two endstations—one devoted to photoelectron microscopy (PEEM) and the second to near ambient pressure photoemission (NAPP)—and another beamline devoted to XMCD and soft X-ray scattering. Both beamlines allow full control of the polarization of the beam, since they are equipped with helical undulators. An additional soft X-ray beamline, installed on a bending magnet port, is equipped with a full-field transmission X-ray microscope. Additional information may be found at http://www.albasynchrotron.es/en/beamlines.     

Development of Hard X-ray Focusing Optics at Diamond Light Source

The short wavelength of X-rays makes them an excellent choice for probing materials on the nanometer scale and for crystallography of sub-micrometer crystallites. The objective of nanofocusing optics is to produce a small, focused beam size in order to obtain the highest X-ray flux on a small sample or as a fine spatial probe. Achieving nanometer-scale focused X-ray beam sizes puts great demands on the optical elements in an X-ray beamline—the optics must balance the requirements to de-magnify the electron beam X-ray source, to reduce the diffraction-limited focus size, and to minimize the contribution to the focus of aberrations in the optics while collecting the maximum X-ray flux into the focused beam. These requirements dictate that an extreme demagnifying geometry should be employed and that high-specification optical elements must be used. Nanofocusing optics has often been added as an upgrade to existing beamlines at Diamond, extending the range of science that can be carried out. Extreme nanofocusing also forms the basis of new beamlines at Diamond, such as the nanoprobe beamline (I14), which aims to provide sub-30-nm-dimension focused X-ray beams for mapping samples at high spatial resolution. The demand for nanometer-scale diffraction-limited X-ray beams is expected to grow at Diamond and requires corresponding advances in X-ray optics to exploit the present source and future lower emittance storage ring sources; for example, the proposed Diamond II upgrade, projected to give a factor 20 emittance reduction.     

Investigations of mechanical vibrations for beamlines at the Canadian Light Source

Vibration is often a problem causing poor quality of photon beams at synchrotron radiation facilities, since beamlines are quite sensitive to vibrations. Therefore, vibration analysis and control at synchrotron radiation facilities is crucial. This paper presents investigations on mechanical vibrations at four beamlines and endstations at the Canadian Light Source, i.e. the Canadian Macromolecular Crystallography Facility 08ID‐1 beamline, the Hard X‐ray MicroAnalysis 06ID‐1 beamline, the Resonant Elastic and Inelastic Soft X‐ray Scattering 10ID‐2 beamline, and the Scanning Transmission X‐ray Microscope endstation at the Spectromicroscopy 10ID‐1 beamline. This study identifies vibration sources and investigates the influence of mechanical vibrations on beamline performance. The results show that vibrations caused by movable mechanical equipment significantly affect the data acquired from beamlines.     

XMCD of a single layer of single molecule magnets

A detailed report on the X-ray Magnetic Circular Dichroism (XMCD) investigation of monolayers of Mn12-based single molecule magnets (SMMs) deposited on gold Au(111) is presented. A semi-quantitative analysis of data is provided in order to extract chemical and magnetic information on Mn ions, by comparison with XMCD on bulk samples. This work points that XMCD is a key-tool for the characterization of SMMs-based nanostructured systems. XMCD surface sensitivity and element-specificity will play a fundamental role in the identification of good candidates for SMMs based devices.     

A simple polarimeter for quantifying synchrotron polarization

There are currently no simple and easy to apply techniques for determining the degree of linear polarization of a soft X-ray beam delivered by a synchrotron beamline despite the fact that this parameter is important for a wide range of synchrotron-based soft X-ray experiments. This work presents a new method for the quantitative determination of the linear polarization state of synchrotron radiation using an HOPG crystal as the standard sample. The method is straightforward to perform without the need for experimental apparatus beyond that commonly available at beamlines in this energy range. In addition, the high-degree of order that can easily be achieved in a HOPG sample means that it is potentially more accurate than currently employed comparative methods. We show how the method can be applied to experimentally determine the linear polarization state of various soft X-ray synchrotron beamlines and we discuss the wide variations in the degree of linear polarization that are measured.     

X-ray Nanoprobe Beamline and Pioneering Electron Microscopy Facility Come into Focus

An exciting new hub for cutting-edge materials and life science research is well on its way to being built at Diamond. The new building, which is under construction next to the Imaging and Coherence beamline (I13), will house the X-ray Nanoprobe beamline (I14) along with the Electron Bio-imaging Centre (eBIC) and the Electron Microscopy Centre for physical sciences.     

A new ultra‐high‐vacuum variable temperature and high‐magnetic‐field X‐ray magnetic circular dichroism facility at LNLS

X‐ray magnetic circular dichroism (XMCD) is one of the most powerful tools for investigating the magnetic properties of different types of materials that display ferromagnetic behavior. Compared with other magnetic‐sensitive techniques, XMCD has the advantage of being element specific and is capable of separating the spin and magnetic moment contributions associated with each element in the sample. In samples involving, for example, buried atoms, clusters on surfaces or at interfaces, ultrathin films, nanoparticles and nanostructures, three experimental conditions must be present to perform state‐of‐the‐art XMCD measurements: high magnetic fields, low temperatures and an ultra‐high‐vacuum environment. This paper describes a new apparatus that can be easily installed at different X‐ray and UV beamlines at the Brazilian Synchrotron Light Laboratory (LNLS). The apparatus combines the three characteristics described above and different methods to measure the absorption signal. It also permits in situ sample preparation and transfer to another chamber for measurement by conventional surface science techniques such as low‐energy electron diffraction (LEED), reflection high‐energy electron diffraction (RHEED), X‐ray photoelectron spectroscopy (XPS) and X‐ray photoelectron diffraction (XPD). Examples are given of XMCD measurements performed with this set‐up on different materials.     

Obtaining local reciprocal lattice vectors from finite‐element analysis

Finite‐element analysis is frequently used by engineers at synchrotron beamlines to calculate the elastic deformation of a single crystal undergoing mechanical bending or thermal load. ANSYS^® Workbench? software is widely used for such simulations. However, although ANSYS^® Workbench? software provides useful information on the displacements, strains and stresses within the crystal, it does not yield the local reciprocal lattice vectors that would be required for X‐ray diffraction calculations. To bridge this gap, a method based on the shape functions and interpolation procedures of the software itself has been developed. An application to the double‐crystal bent Laue monochromator being designed for the I12 (JEEP) wiggler beamline at the Diamond Light Source is presented.     

Spin-flop ordering from frustrated ferro- and antiferromagnetic interactions: a combined theoretical and experimental study of a Mn/Fe(100) monolayer

The occurrence of a noncollinear magnetic structure at a Mn monolayer grown epitaxially on Fe(100) is predicted theoretically, using spinor density-functional theory, and observed experimentally, using x-ray magnetic circular dichroism (XMCD) and linear dichroism (XMLD) spectroscopies. The combined use of XMCD and XMLD at the Mn-absorption edge allows us to assess the existence of ferromagnetic and antiferromagnetic order at the interface, and also to determine the moment orientations with element specificity. The experimental results thus obtained are in excellent agreement with the magnetic structure determined theoretically.     

Overview of the tunable beamlines for protein crystallography at the EMBL Hamburg Outstation; an analysis of current and future usage and developments

The EMBL Hamburg Outstation currently operates two tunable protein crystallography beamlines suitable for single and multiple anomalous diffraction (SAD/MAD) experiments. The first beamline, designated X31, is located on a bending magnet of the DORIS III storage ring whereas the second beamline, BW7A, is positioned at a multipole wiggler at the same storage ring. X31 is equipped with an energy stabilization device to ensure constant wavelength during longer data-collection periods. The in-house built crystallographic end-station is now equipped with a Mar345 imaging-plate scanner as a detector. The wiggler beamline BW7A features a novel sagitally focusing monochromator. The end-station used here has also been developed and built in-house. The beamline is currently operated with a Mar 165 CCD detector. In this paper the hardware and software developments of the last years will be summarized and the outlook for substantial upgrades will be given. The future plans include the design and construction of a third tunable beamline, designated X12, for protein crystallography. The development of automated beamlines for protein crystallography is of particular importance with respect to structural genomics initiatives. The analysis of the projects of the last years shows the wide range of anomalous scatterer used on the tunable beamlines thus demonstrating the need of a wide range of accessible energies and fast and reliable energy changes.     

Third International Synchrotron Radiation Circular Dichroism Spectroscopy Meeting

The International Synchrotron Radiation Circular Dichroism (SRCD) Spectroscopy Meeting was held at the Physikzentrum, Bad Honnef, Germany on May 17–20, 2015, as the 590^th WE-Heraeus-Seminar. It was the third in the series of SRCD Workshops, following the first one held at the Daresbury Synchrotron (UK) in 2001, and the second at the Beijing Synchrotron Radiation Facility (BSRF) and the Institute of High Energy Physics (IHEP) in 2009. SRCD2015 was organized by Dr. Jochen Bürck, Prof. Anne Ulrich, and Dr. Dirk Windisch (all of Institute of Biological Interfaces (IBG-2), Karlsruhe Institute of Technology, Germany) and Prof. Bonnie Ann Wallace (Birkbeck College, University of London, UK). It was aimed at both synchrotron CD beamline scientists and scientific users of the beamlines, and included participants from 14 countries. For the first time, representatives of all operational SRCD beamlines worldwide were present at the same meeting, and scientists developing two new SRCD beamlines also participated.     

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.     

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

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

Imaging of magnetic domains with the X-ray microscope at BESSY using X-ray magnetic circular dichroism

X-ray Magnetic Circular Dichroism (X-MCD), i.e. the change of the absorption of circular polarized Xrays for reversed sample magnetization amounts at the L_{2, 3}-edges of 3d transition metals up to 50% percent. This can be used to obtain in energy-dispersive X-ray imaging techniques a considerable, element-specific magnetic contrast. On the other hand, with the transmission X-ray microscope (TXM) based on the zone-plate technique spatial resolutions of 30nm can be achieved. In this communication it is shown for the first time that the combination of the TXM with XMCD provides a huge contrast and is therefore a powerful new method to visualize in a quantitative and elementspecific manner magnetic domains. Using soft X-rays with a wavelength of 1:7nm corresponding to the energy of the Fe L₃-edge the variation of the shape and magnetization of domains in a magneto-optical GdFe layer system was studied with a lateral resolution of 60nm.     

XDS: a flexible beamline for X‐ray diffraction and spectroscopy at the Brazilian synchrotron

The majority of the beamlines at the Brazilian Synchrotron Light Source Laboratory (LNLS) use radiation produced in the storage‐ring bending magnets and are therefore currently limited in the flux that can be used in the harder part of the X‐ray spectrum (above ～10 keV). A 4 T superconducting multipolar wiggler (SCW) was recently installed at LNLS in order to improve the photon flux above 10 keV and fulfill the demands set by the materials science community. A new multi‐purpose beamline was then installed at the LNLS using the SCW as a photon source. The XDS is a flexible beamline operating in the energy range between 5 and 30 keV, designed to perform experiments using absorption, diffraction and scattering techniques. Most of the work performed at the XDS beamline concentrates on X‐ray absorption spectroscopy at energies above 18 keV and high‐resolution diffraction experiments. More recently, new setups and photon‐hungry experiments such as total X‐ray scattering, X‐ray diffraction under high pressures, resonant X‐ray emission spectroscopy, among others, have started to become routine at XDS. Here, the XDS beamline characteristics, performance and a few new experimental possibilities are described.     

Software for the high-throughput collection of SAXS data using an enhanced Blu-Ice/DCS control system

Biological small-angle X-ray scattering (SAXS) provides powerful complementary data for macromolecular crystallography (MX) by defining shape, conformation and assembly in solution. Although SAXS is in principle the highest throughput technique for structural biology, data collection is limited in practice by current data collection software. Here the adaption of beamline control software, historically developed for MX beamlines, for the efficient operation and high-throughput data collection at synchrotron SAXS beamlines is reported. The Blu-Ice GUI and Distributed Control System (DCS) developed in the Macromolecular Crystallography Group at the Stanford Synchrotron Radiation Laboratory has been optimized, extended and enhanced to suit the specific needs of the biological SAXS endstation at the SIBYLS beamline at the Advanced Light Source. The customizations reported here provide a potential route for other SAXS beamlines in need of robust and efficient beamline control software. As a great deal of effort and optimization has gone into crystallographic software, the adaption and extension of crystallographic software may prove to be a general strategy to provide advanced SAXS software for the synchrotron community. In this way effort can be put into optimizing features for SAXS rather than reproducing those that have already been successfully implemented for the crystallographic community.     

Meeting Report: PhotoEmission Electron Microscopy (PEEM) Workshop at Diamond Light Source

When Diamond Light Source goes into operation in January 2007, one of the first beamlines will house a state-of-the-art PhotoEmission Electron Microscope (PEEM). On July 12 and 13, 2006, Diamond hosted a workshop to promote the wide-ranging capabilities of PEEM to the user community. An international audience enjoyed talks and discussions on interface magnetism, geological science, surface chemistry and the principles of X-ray excited PEEM.     

Optimized IR synchrotron beamline design

Synchrotron infrared beamlines are powerful tools on which to perform spectroscopy on microscopic length scales but require working with large bending‐magnet source apertures in order to provide intense photon beams to the experiments. Many infrared beamlines use a single toroidal‐shaped mirror to focus the source emission which generates, for large apertures, beams with significant geometrical aberrations resulting from the shape of the source and the beamline optics. In this paper, an optical layout optimized for synchrotron infrared beamlines, that removes almost totally the geometrical aberrations of the source, is presented and analyzed. This layout is already operational on the IR beamline of the Brazilian synchrotron. An infrared beamline design based on a SOLEIL bending‐magnet source is given as an example, which could be useful for future IR beamline improvements at this facility.