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Journal of Synchrotron Radiation



Synchrotron radiation research is rapidly expanding with many new sources of radiation being created globally. Synchrotron radiation plays a leading role in pure science and in emerging technologies. The Journal of Synchrotron Radiation provides comprehen



Published: 2017-12-14

 



A compact and versatile tender X-ray single-shot spectrometer for online XFEL diagnostics

2018-01-01

One of the remaining challenges for accurate photon diagnostics at X-ray free-electron lasers (FELs) is the shot-to-shot, non-destructive, high-resolution characterization of the FEL pulse spectrum at photon energies between 2 keV and 4 keV, the so-called tender X-ray range. Here, a spectrometer setup is reported, based on the von Hamos geometry and using elastic scattering as a fingerprint of the FEL-generated spectrum. It is capable of pulse-to-pulse measurement of the spectrum with an energy resolution (ΔE/E) of 10−4, within a bandwidth of 2%. The Tender X-ray Single-Shot Spectrometer (TXS) will grant to experimental scientists the freedom to measure the spectrum in a single-shot measurement, keeping the transmitted beam undisturbed. It will enable single-shot reconstructions for easier and faster data analysis.



FLASH free-electron laser single-shot temporal diagnostic: terahertz-field-driven streaking

2018-01-01

The commissioning of a terahertz-field-driven streak camera installed at the free-electron laser (FEL) FLASH at DESY in Hamburg, being able to deliver photon pulse duration as well as arrival time information with ∼10 fs resolution for each single XUV FEL pulse, is reported. Pulse durations between 300 fs and <15 fs have been measured for different FLASH FEL settings. A comparison between the XUV pulse arrival time and the FEL electron bunch arrival time measured at the FLASH linac section exhibits a correlation width of 20 fs r.m.s., thus demonstrating the excellent operation stability of FLASH. In addition, the terahertz-streaking setup was operated simultaneously to an alternative method to determine the FEL pulse duration based on spectral analysis. FLASH pulse duration derived from simple spectral analysis is in good agreement with that from terahertz-streaking measurement.



X-ray beam-shaping via deformable mirrors: surface profile and point spread function computation for Gaussian beams using physical optics

2018-01-01

X-ray mirrors with high focusing performances are commonly used in different sectors of science, such as X-ray astronomy, medical imaging and synchrotron/free-electron laser beamlines. While deformations of the mirror profile may cause degradation of the focus sharpness, a deliberate deformation of the mirror can be made to endow the focus with a desired size and distribution, via piezo actuators. The resulting profile can be characterized with suitable metrology tools and correlated with the expected optical quality via a wavefront propagation code or, sometimes, predicted using geometric optics. In the latter case and for the special class of profile deformations with monotonically increasing derivative, i.e. concave upwards, the point spread function (PSF) can even be predicted analytically. Moreover, under these assumptions, the relation can also be reversed: from the desired PSF the required profile deformation can be computed analytically, avoiding the use of trial-and-error search codes. However, the computation has been so far limited to geometric optics, which entailed some limitations: for example, mirror diffraction effects and the size of the coherent X-ray source were not considered. In this paper, the beam-shaping formalism in the framework of physical optics is reviewed, in the limit of small light wavelengths and in the case of Gaussian intensity wavefronts. Some examples of shaped profiles are also shown, aiming at turning a Gaussian intensity distribution into a top-hat one, and checks of the shaping performances computing the at-wavelength PSF by means of the WISE code are made.



Diffraction gratings metrology and ray-tracing results for an XUV Raman spectrometer at FLASH

2018-01-01

The extreme-ultraviolet double-stage imaging Raman spectrometer is a permanent experimental endstation at the plane-grating monochromator beamline branch PG1 at FLASH at DESY in Hamburg, Germany. This unique instrument covers the photon energy range from 20 to 200 eV with high energy resolution of about 2 to 20 meV (design values) featuring an efficient elastic line suppression as well as effective stray light rejection. Such a design enables studies of low-energy excitations like, for example, phonons in solids close to the vicinity of the elastic line. The Raman spectrometer effectively operates with four reflective off-axial parabolic mirrors and two plane-grating units. The optics quality and their precise alignment are crucial to guarantee best performance of the instrument. Here, results on a comprehensive investigation of the quality of the spectrometer diffraction gratings are presented. The gratings have been characterized by ex situ metrology at the BESSY-II Optics Laboratory, employing slope measuring deflectometry and interferometry as well as atomic force microscopy studies. The efficiency of these key optical elements has been measured at the at-wavelength metrology laboratory using the reflectometer at the BESSY-II Optics beamline. Also, the metrology results are discussed with respect to the expected resolving power of the instrument by including them in ray-tracing studies of the instrument.



Performance of a hard X-ray split-and-delay optical system with a wavefront division

2018-01-01

The performance of a hard X-ray split-and-delay optical (SDO) system with a wavefront division scheme was investigated at the hard X-ray free-electron laser facility SACLA. For the wavefront division, beam splitters made of edge-polished perfect Si(220) crystals were employed. We characterized the beam properties of the SDO system, and investigated its capabilities for beam manipulation and diagnostics. First, it was confirmed that shot-to-shot non-invasive diagnostics of pulse energies for both branches in the SDO system was feasible. Second, nearly ideal and identical focal profiles for both branches were obtained with a spot size of ∼1.5 µm in full width at half-maximum. Third, a spatial overlap of the two focused beams with a sub-µm accuracy was achieved by fine tuning of the SDO system. Finally, a reliable tunability of the delay time between two pulses was confirmed. The time interval was measured with an X-ray streak camera by changing the path length of the variable-delay branch. Errors from the fitted line were evaluated to be as small as ±0.4 ps over a time range of 60 ps.



Non-invasive online wavelength measurements at FLASH2 and present benchmark

2018-01-01

At FLASH2, the free-electron laser radiation wavelength is routinely measured by an online spectrometer based on photoionization of gas targets. Photoelectrons are detected with time-of-flight spectrometers and the wavelength is determined by means of well known binding energies of the target species. The wavelength measurement is non-invasive and transparent with respect to running user experiments due to the low gas pressure applied. Sophisticated controls for setting the OPIS operation parameters have been created and integrated into the distributed object-oriented control system at FLASH2. Raw and processed data can be stored on request in the FLASH data acquisition system for later correlation with data from user experiments or re-analysis. In this paper, the commissioning of the instrument at FLASH2 and the challenges of space charge effects on wavelength determination are reported. Furthermore, strategies for fast data reduction and online data processing are presented.



Efficient high-order suppression system for a metrology beamline

2018-01-01

High-quality metrology with synchrotron radiation requires in particular a very high spectral purity of the incident beam. This is usually achieved by a set of transmission filters with suitable absorption edges to suppress high-order radiation of the monochromator. The at-wavelength metrology station at a BESSY-II bending-magnet collimated plane-grating monochromator (c-PGM) beamline has recently commissioned a high-order suppression system (HiOS) based on four reflections from mirrors which can be inserted into the beam path. Two pairs of mirrors are aligned parallel so as not to disturb the original beam path and are rotated clockwise and counter-clockwise. Three sets of coatings are available for the different energy ranges and the incidence angle is freely tunable to find the optimum figure of merit for maximum suppression at maximum transmission for each photon energy required. Measured performance results of the HiOS for the EUV and XUV range are compared with simulations, and applications are discussed.



Nanofocusing with aberration-corrected rotationally parabolic refractive X-ray lenses

2018-01-01

Wavefront errors of rotationally parabolic refractive X-ray lenses made of beryllium (Be CRLs) have been recovered for various lens sets and X-ray beam configurations. Due to manufacturing via an embossing process, aberrations of individual lenses within the investigated ensemble are very similar. By deriving a mean single-lens deformation for the ensemble, aberrations of any arbitrary lens stack can be predicted from the ensemble with \bar{\sigma} = 0.034λ. Using these findings the expected focusing performance of current Be CRLs are modeled for relevant X-ray energies and bandwidths and it is shown that a correction of aberrations can be realised without prior lens characterization but simply based on the derived lens deformation. The performance of aberration-corrected Be CRLs is discussed and the applicability of aberration-correction demonstrated over wide X-ray energy ranges.



Coatings for FEL optics: preparation and characterization of B4C and Pt

2018-01-01

Large X-ray mirrors are required for beam transport at both present-day and future free-electron lasers (FELs) and synchrotron sources worldwide. The demand for large mirrors with lengths up to 1 m single layers consisting of light or heavy elements has increased during the last few decades. Accordingly, surface finishing technology is now able to produce large substrate lengths with micro-roughness on the sub-nanometer scale. At the Helmholtz-Zentrum Geesthacht (HZG), a 4.5 m-long sputtering facility enables us to deposit a desired single-layer material some tens of nanometers thick. For the European XFEL project, the shape error should be less than 2 nm over the whole 1 m X-ray mirror length to ensure the safe and efficient delivery of X-ray beams to the scientific instruments. The challenge is to achieve thin-film deposition on silicon substrates, benders and gratings without any change in mirror shape. Thin films of boron carbide and platinum with a thickness in the range 30–100 nm were manufactured using the HZG sputtering facility. This setup is able to cover areas of up to 1500 mm × 120 mm in one step using rectangular sputtering sources. The coatings produced were characterized using various thin-film methods. It was possible to improve the coating process to achieve a very high uniformity of the layer thickness. The movement of the substrate in front of the sputtering source has been optimized. A variation in B4C layer thickness below 1 nm (peak-to-valley) was achieved at a mean thickness of 51.8 nm over a deposition length of 1.5 m. In the case of Pt, reflectometry and micro-roughness measurements were performed. The uniformity in layer thickness was about 1 nm (peak-to-valley). The micro-roughness of the Pt layers showed no significant change in the coated state for layer thicknesses of 32 nm and 102 nm compared with the uncoated substrate state. The experimental results achieved will be discussed with regard to current restrictions and future developments.



Laser power meters as an X-ray power diagnostic for LCLS-II

2018-01-01

For the LCLS-II X-ray instruments, laser power meters are being developed as compact X-ray power diagnostics to operate at soft and tender X-ray photon energies. These diagnostics can be installed at various locations along an X-ray free-electron laser (FEL) beamline in order to monitor the transmission of X-ray optics along the beam path. In addition, the power meters will be used to determine the absolute X-ray power at the endstations. Here, thermopile power meters, which measure average power, and have been chosen primarily for their compatibility with the high repetition rates at LCLS-II, are evaluated. A number of characteristics in the soft X-ray range are presented including linearity, calibrations conducted with a photodiode and a gas monitor detector as well as ultra-high-vacuum compatibility tests using residual gas analysis. The application of these power meters for LCLS-II and other X-ray FEL sources is discussed.



THz pulse doubler at FLASH: double pulses for pump–probe experiments at X-ray FELs

2018-01-01

FLASH, the X-ray free-electron laser in Hamburg, Germany, employs a narrowband high-field accelerator THz source for unique THz pump X-ray probe experiments. However, the large difference in optical paths of the THz and X-ray beamlines prevents utilization of the machine's full potential (e.g. extreme pulse energies in the soft X-ray range). To solve this issue, lasing of double electron bunches, separated by 28 periods of the driving radiofrequency (at 1.3 GHz), timed for the temporal overlap of THz and X-ray pulses at the experimental station has been employed. In order to optimize conditions for a typical THz pump X-ray probe experiment, X-ray lasing of the first bunch to one-sixth of that of the second has been suppressed. Finally, synchronization of THz radiation pulses was measured to be ∼20 fs (r.m.s.), and a solution for monitoring the arrival time for achieving higher temporal resolution is presented.



Grating configurations to compress free-electron laser pulses

2018-01-01

The optical layout of soft X-ray grating compressors designed to provide both positive and negative group-delay dispersion (GDD) is discussed. They are tailored for chirped-pulse-amplification experiments with seeded free-electron laser sources. Designs with plane or concave gratings are discussed, depending on the sign of the GDD to be introduced.



Double-grating monochromatic beamline with ultrafast response for FLASH2 at DESY

2018-01-01

The preliminary design of a monochromatic beamline for FLASH2 at DESY is presented. The monochromator is tunable in the 50–1000 eV energy range with resolving power higher than 1000 and temporal response below 50 fs over the whole energy range. A time-delay-compensated configuration using the variable-line-spacing monochromator design with two gratings is adopted: the first grating disperses the radiation on its output plane, where the intermediate slit performs the spectral selection; the second grating compensates for the pulse-front tilt and for the spectral dispersion due to diffraction from the first grating.



In situ electrochemical synchrotron radiation for Li-ion batteries

2018-01-01

Observing the electronic structure, compositional change and morphological evolution of the surface and interface of a battery during operation provides essential information for developing new electrode materials for Li-ion batteries (LIBs); this is because such observations demonstrate the fundamental reactions occurring inside the electrode materials. Moreover, obtaining detailed data on chemical phase changes and distributions by analyzing an operating LIB is the most effective method for exploring the intercalation/de-intercalation process, kinetics and the relationship between phase change or phase distribution and battery performance, as well as for further optimizing the material synthesis routes for advanced battery materials. However, most conventional in situ electrochemical techniques (other than by using synchrotron radiation) cannot clearly or precisely demonstrate structural change, electron valence change and chemical mapping information. In situ electrochemical-synchrotron radiation techniques such as X-ray absorption spectroscopy, X-ray diffraction spectroscopy and transmission X-ray microscopy can deliver accurate information regarding LIBs. This paper reviews studies regarding various applications of in situ electrochemical-synchrotron radiation such as crystallographic transformation, oxidation-state changes, characterization of the solid electrolyte interphase and Li-dendrite growth mechanism during the intercalation/de-intercalation process. The paper also presents the findings of previous review articles and the future direction of these methods.



Lead apatites: structural variations among Pb5(BO4)3Cl with B = P (pyromorphite), As (mimetite) and V (vanadinite)

2018-01-01

The crystal structure of four Pb apatite samples, Pb5(BO4)3Cl, was refined with synchrotron high-resolution powder X-ray diffraction data, Rietveld refinements, space group P63/m and Z = 2. For this isotypic series, B = P5+ is pyromorphite, B = As5+ is mimetite and B = V5+ is vanadinite. The ionic radius for As5+ (0.355 Å) is similar to that of V5+ (0.335 Å), and this is twice as large as that for P5+ (0.170 Å). However, the c unit-cell parameter for mimetite is surprisingly different from that of vanadinite, although their unit-cell volumes, V, are almost equal to each other. No explanation was available for this peculiar c-axis value for mimetite. Structural parameters such as average 〈B—O〉 [4], 〈Pb1—O9〉 [9] and 〈Pb2—O6Cl2〉 [8] distances increase linearly with V (the coordination numbers for the cations are given in square brackets). Mimetite has a short Pb2—O1 distance, so the O1 oxygen atom interacts with the 6s2 lone-pair electrons of the Pb2+ cation that causes the Cl—Cl distance (= c/2) to increase to the largest value in the series because of repulsion, which causes the c-axis to increase anomalously. Although Pb apatite minerals occur naturally in ore deposits, they are also formed as scaly deposits in lead water pipes that give rise to lead in tap water, as was found recently in Flint, Michigan, USA. It is important to identify Pb-containing phases in water-pipe deposits.



Transient thermal stress wave and vibrational analyses of a thin diamond crystal for X-ray free-electron lasers under high-repetition-rate operation

2018-01-01

High-brightness X-ray free-electron lasers (FELs) are perceived as fourth-generation light sources providing unprecedented capabilities for frontier scientific researches in many fields. Thin crystals are important to generate coherent seeds in the self-seeding configuration, provide precise spectral measurements, and split X-ray FEL pulses, etc. In all of these applications a high-intensity X-ray FEL pulse impinges on the thin crystal and deposits a certain amount of heat load, potentially impairing the performance. In the present paper, transient thermal stress wave and vibrational analyses as well as transient thermal analysis are carried out to address the thermomechanical issues for thin diamond crystals, especially under high-repetition-rate operation of an X-ray FEL. The material properties at elevated temperatures are considered. It is shown that, for a typical FEL pulse depositing tens of microjoules energy over a spot of tens of micrometers in radius, the stress wave emission is completed on the tens of nanoseconds scale. The amount of kinetic energy converted from a FEL pulse can reach up to ∼10 nJ depending on the layer thickness. Natural frequencies of a diamond plate are also computed. The potential vibrational amplitude is estimated as a function of frequency. Due to the decreasing heat conductivity with increasing temperature, a runaway temperature rise is predicted for high repetition rates where the temperature rises abruptly after ratcheting up to a point of trivial heat damping rate relative to heat deposition rate.



Pulse-resolved intensity measurements at a hard X-ray FEL using semi-transparent diamond detectors

2018-01-01

Solid-state ionization chambers are presented based on thin diamond crystals that allow pulse-resolved intensity measurements at a hard X-ray free-electron laser (FEL), up to the 4.5 MHz repetition rate that will become available at the European XFEL. Due to the small X-ray absorption of diamond the thin detectors are semi-transparent which eases their use as non-invasive monitoring devices in the beam. FELs are characterized by strong pulse-to-pulse intensity fluctuations due to the self-amplified spontaneous emission (SASE) process and in many experiments it is mandatory to monitor the intensity of each individual pulse. Two diamond detectors with different electrode materials, beryllium and graphite, were tested as intensity monitors at the XCS endstation of the Linac Coherent Light Source (LCLS) using the pink SASE beam at 9 keV. The performance is compared with LCLS standard monitors that detect X-rays backscattered from thin SiN foils placed in the beam. The graphite detector can also be used as a beam position monitor although with rather coarse resolution.



X-ray Fourier transform holography by amplitude-division-type Fresnel zone plate interferometer

2018-01-01

A two-block X-ray Fresnel zone plate system forms two-beams – a plane wave and a spherical wave – which interfere at the focal distance of the virtual source of the spherical wave. An object placed in the path of the plane wave forms an object wave and the spherical wave is the reference wave. The recorded intensity distribution is the Fourier transform hologram of the object. Analytical and numerical calculations show the possibilities of this scheme to record the hologram and reconstruct the object image. Examples of recording holograms of a one-dimensional cosine-like grating and a two-dimensional grid object as well as reconstruction of the images are considered.



X-ray natural circular dichroism in langasite crystal

2018-01-01

Optical activity in the X-ray range stems from the electric-dipole–electric-quadrupole interference terms mixing multipoles of opposite parity, and can be observed exclusively in systems with broken inversion symmetry. The gyration tensor formalism is used to describe the X-ray optical activity in langasite La3Ga5SiO14 crystal with the P321 space group. An experimental study of the X-ray natural circular dichroism (XNCD) near the Ga K-edge in La3Ga5SiO14 single crystal was performed at ESRF beamline ID12, both along and perpendicular to the crystal optical axis. The combination of the quantum mechanical calculations and high-quality experimental results has allowed us to separate the contributions into X-ray absorption and XNCD spectra of Ga atoms occupying three distinct Wyckoff positions.



Fast projection/backprojection and incremental methods applied to synchrotron light tomographic reconstruction

2018-01-01

Iterative methods for tomographic image reconstruction have the computational cost of each iteration dominated by the computation of the (back)projection operator, which take roughly O(N3) floating point operations (flops) for N × N pixels images. Furthermore, classical iterative algorithms may take too many iterations in order to achieve acceptable images, thereby making the use of these techniques unpractical for high-resolution images. Techniques have been developed in the literature in order to reduce the computational cost of the (back)projection operator to O(N2logN) flops. Also, incremental algorithms have been devised that reduce by an order of magnitude the number of iterations required to achieve acceptable images. The present paper introduces an incremental algorithm with a cost of O(N2logN) flops per iteration and applies it to the reconstruction of very large tomographic images obtained from synchrotron light illuminated data.



Digital fast pulse shape and height analysis on cadmium–zinc–telluride arrays for high-flux energy-resolved X-ray imaging

2018-01-01

Cadmium–zinc–telluride (CZT) arrays with photon-counting and energy-resolving capabilities are widely proposed for next-generation X-ray imaging systems. This work presents the performance of a 2 mm-thick CZT pixel detector, with pixel pitches of 500 and 250 µm, dc coupled to a fast and low-noise ASIC (PIXIE ASIC), characterized only by the preamplifier stage. A custom 16-channel digital readout electronics was used, able to digitize and process continuously the signals from each output ASIC channel. The digital system performs on-line fast pulse shape and height analysis, with a low dead-time and reasonable energy resolution at both low and high fluxes. The spectroscopic response of the system to photon energies below (109Cd source) and above (241Am source) the K-shell absorption energy of the CZT material was investigated, with particular attention to the mitigation of charge sharing and pile-up. The detector allows high bias voltage operation (>5000 V cm−1) and good energy resolution at moderate cooling (3.5% and 5% FWHM at 59.5 keV for the 500 and 250 µm arrays, respectively) by using fast pulse shaping with a low dead-time (300 ns). Charge-sharing investigations were performed using a fine time coincidence analysis (TCA), with very short coincidence time windows up to 10 ns. For the 500 µm pitch array (250 µm pitch array), sharing percentages of 36% (52%) and 60% (82%) at 22.1 and 59.5 keV, respectively, were measured. The potential of the pulse shape analysis technique for charge-sharing detection for corner/border pixels and at high rate conditions (250 kcps pixel−1), where the TCA fails, is also shown. Measurements demonstrated that significant amounts of charge are lost for interactions occurring in the volume of the inter-pixel gap. This charge loss must be accounted for in the correction of shared events. These activities are within the framework of an international collaboration on the development of energy-resolved photon-counting systems for high-flux energy-resolved X-ray imaging (1–140 keV).



A soft X-ray free-electron laser beamline at SACLA: the light source, photon beamline and experimental station

2018-01-01

The design and performance of a soft X-ray free-electron laser (FEL) beamline of the SPring-8 Compact free-electron LAser (SACLA) are described. The SPring-8 Compact SASE Source test accelerator, a prototype machine of SACLA, was relocated to the SACLA undulator hall for dedicated use for the soft X-ray FEL beamline. Since the accelerator is operated independently of the SACLA main linac that drives the two hard X-ray beamlines, it is possible to produce both soft and hard X-ray FEL simultaneously. The FEL pulse energy reached 110 µJ at a wavelength of 12.4 nm (i.e. photon energy of 100 eV) with an electron beam energy of 780 MeV.



DA+ data acquisition and analysis software at the Swiss Light Source macromolecular crystallography beamlines

2018-01-01

Data acquisition software is an essential component of modern macromolecular crystallography (MX) beamlines, enabling efficient use of beam time at synchrotron facilities. Developed at the Paul Scherrer Institute, the DA+ data acquisition software is implemented at all three Swiss Light Source (SLS) MX beamlines. DA+ consists of distributed services and components written in Python and Java, which communicate via messaging and streaming technologies. The major components of DA+ are the user interface, acquisition engine, online processing and database. Immediate data quality feedback is achieved with distributed automatic data analysis routines. The software architecture enables exploration of the full potential of the latest instrumentation at the SLS MX beamlines, such as the SmarGon goniometer and the EIGER X 16M detector, and development of new data collection methods.