Multi-segment cooling design of a reflection mirror based on the finite-element method
High-repetition-rate free-electron lasers impose stringent requirements on thermal deformations of optics in the beamline. The Shanghai HIgh-repetition-rate XFEL aNd Extreme light facility (SHINE) experiences high average thermal power and demands wavefront preservation. To effectively manage thermal deformation in the first reflection mirrors M1, we optimized the cooling length and position of the cooling groove with numerical calculations. For example, the root mean square of the height error of the thermal deformation of the mirror at a photon energy of 900 eV was optimized, resulting in a 12.7× reduction, from 13.76 nm to 1.08 nm. This optimized design also eliminated stray light in the focus spot at the sample and resulted in a 177% increase in the peak intensity of the beam's focus spot at the sample, from 3.08 × 10 to 8.53 × 10. The multi-segment cooling design of the mirror advanced the quality of the beam's focus spot at the sample and ensured the stable operation of SHINE under high repetition rates.
Hard X-ray single-shot spectrometer of PAL-XFEL
A transmissive single-shot spectrometer has been developed to monitor shot-to-shot spectral structures in the hard X-ray beamline of the Pohang Accelerator Laboratory X-ray Free Electron Laser (PAL-XFEL). The established spectrometer comprises 10 µm-thick Si crystals bent to a radius of curvature of 100 mm. Depending on the photon energy range, either the Si (111) or Si (110) crystal can be selected for spectral analysis. Especially in the energy range 4.5-17 keV, the spectrometer is designed to cover a spectral range wider than the full free-electron laser bandwidth and to guarantee a high resolution sufficient for resolving each spectral spike. This paper presents the design specifications, instruments and performance of this spectrometer, which has also been applied to demonstrate the spectral properties of various XFEL sources, such as self-amplified spontaneous emission, monochromatic and seeded beams.
30 years of Journal of Synchrotron Radiation and synchrotron science
Journal of Synchrotron Radiation (JSR) came into being with the publication of its inaugural issue in October 1994 that contained 15 full articles comprising 100 pages. Thirty years of JSR has coincided with several Nobel Prizes that have arisen from the work undertaken on synchrotron radiation sources, with the first of these awarded to Sir John Walker in 1997, just three years after the launch of JSR, and celebrated on the front cover of the journal's July 1999 issue. This article provides an insight into the motivation as well as the journey of establishing this important journal for the IUCr and the synchrotron radiation community which has continued to grow. We also highlight some of the well cited papers for each of the five-year-periods during these 30 years and demonstrate how the journal has become the natural home for all aspects of synchrotron radiation science and technology.
Reducing heat load density with asymmetric and inclined double-crystal monochromators: principles and requirements revisited
xxxx Asymmetric double-crystal monochromators (aDCMs) and inclined DCMs (iDCMs) can significantly expand the X-ray beam footprint and consequently reduce the heat load density and gradient. Based on rigorous dynamical theory calculations, the major principles and properties of aDCMs and iDCMs are presented to guide their design and development, particularly for fourth-generation synchrotrons. In addition to the large beam footprint, aDCMs have very large bandwidths (up to ∼10 eV) and angular acceptance, but the narrow angular acceptance of the second crystal requires precise control of the relative orientations and strains. Based on Fourier coupled-wave diffraction theory calculations, it is rigorously proved that the iDCM has almost the same properties as the conventional symmetric DCM, including the efficiency, angular acceptance, bandwidth, tuning energy range and sensitivity to misalignment. The exception is that, for the extremely inclined geometry that can achieve very large footprint expansion, the iDCM has (beneficially) a larger bandwidth and wider angular acceptance. Inclined diffraction has the `rho-kick effect' that can be cancelled by the second reflection of the iDCM (even with misalignment), except that inhomogeneous strains may cause non-uniform rho-kick angles. At present, fabrication/mounting-induced strains pose low risk since they can be controlled to <0.5 µrad over large areas. The only uncertain challenge is the thermally induced strains, yet it is estimated that these strains are naturally lowered by the large footprint and may be further mitigated by optimized cryogenic cooling to the 1-2 µrad level. Overall, aDCMs and iDCMs have more stringent requirements than normal DCMs, but they are feasible schemes in practice.
Development of MHz X-ray phase contrast imaging at the European XFEL
We report on recent developments that enable megahertz hard X-ray phase contrast imaging (MHz XPCI) experiments at the Single Particles, Clusters, and Biomolecules and Serial Femtosecond Crystallography (SPB/SFX) instrument of the European XFEL facility (EuXFEL). We describe the technical implementation of the key components, including an MHz fast camera and a modular indirect X-ray microscope system based on fast scintillators coupled through a high-resolution optical microscope, which enable full-field X-ray microscopy with phase contrast of fast and irreversible phenomena. The image quality for MHz XPCI data showed significant improvement compared with a pilot demonstration of the technique using parallel beam illumination, which also allows access to up to 24 keV photon energies at the SPB/SFX instrument of the EuXFEL. With these developments, MHz XPCI was implemented as a new method offered for a broad user community (academic and industrial) and is accessible via standard user proposals. Furthermore, intra-train pulse diagnostics with a high few-micrometre spatial resolution and recording up to 128 images of consecutive pulses in a train at up to 1.1 MHz repetition rate is available upstream of the instrument. Together with the diagnostic camera upstream of the instrument and the MHz XPCI setup at the SPB/SFX instrument, simultaneous two-plane measurements for future beam studies and feedback for machine parameter tuning are now possible.
Mitigation of DMM-induced stripe patterns in synchrotron X-ray radiography through dynamic tilting
In synchrotron X-ray radiography, achieving high image resolution and an optimal signal-to-noise ratio (SNR) is crucial for the subsequent accurate image analysis. Traditional methods often struggle to balance these two parameters, especially in situ applications where rapid data acquisition is essential to capture specific dynamic processes. For quantitative image data analysis, using monochromatic X-rays is essential. A double multilayer monochromator (DMM) is successfully used for this aim at the BAMline, BESSY II (Helmholtz Zentrum Berlin, Germany). However, such DMMs are prone to producing an unstable horizontal stripe pattern. Such an unstable pattern renders proper signal normalization difficult and thereby causes a reduction of the SNR. We introduce a novel approach to enhance SNR while preserving resolution: dynamic tilting of the DMM. By adjusting the orientation of the DMM during the acquisition of radiographic projections, we optimize the X-ray imaging quality, thereby enhancing the SNR. The corresponding shift of the projection during this movement is corrected in post-processing. The latter correction allows a good resolution to be preserved. This dynamic tilting technique enables the homogenization of the beam profile and thereby effectively reduces noise while maintaining high resolution. We demonstrate that data captured using this proposed technique can be seamlessly integrated into the existing radiographic data workflow, as it does not need hardware modifications to classical X-ray imaging beamline setups. This facilitates further image analysis and processing using established methods.
A miniature X-ray diffraction setup on ID20 at the European Synchrotron Radiation Facility
We describe an ultra-compact setup for in situ X-ray diffraction on the inelastic X-ray scattering beamline ID20 at the European Synchrotron Radiation Facility. The main motivation for the design and construction of this setup is the increasing demand for on-the-fly sample characterization, as well as ease of navigation through a sample's phase diagram, for example subjected to high-pressure and/or high-temperature conditions. We provide technical details and demonstrate the performance of the setup.
A general Bayesian algorithm for the autonomous alignment of beamlines
Autonomous methods to align beamlines can decrease the amount of time spent on diagnostics, and also uncover better global optima leading to better beam quality. The alignment of these beamlines is a high-dimensional expensive-to-sample optimization problem involving the simultaneous treatment of many optical elements with correlated and nonlinear dynamics. Bayesian optimization is a strategy of efficient global optimization that has proved successful in similar regimes in a wide variety of beamline alignment applications, though it has typically been implemented for particular beamlines and optimization tasks. In this paper, we present a basic formulation of Bayesian inference and Gaussian process models as they relate to multi-objective Bayesian optimization, as well as the practical challenges presented by beamline alignment. We show that the same general implementation of Bayesian optimization with special consideration for beamline alignment can quickly learn the dynamics of particular beamlines in an online fashion through hyperparameter fitting with no prior information. We present the implementation of a concise software framework for beamline alignment and test it on four different optimization problems for experiments on X-ray beamlines at the National Synchrotron Light Source II and the Advanced Light Source, and an electron beam at the Accelerator Test Facility, along with benchmarking on a simulated digital twin. We discuss new applications of the framework, and the potential for a unified approach to beamline alignment at synchrotron facilities.
A study of structural effects on the focusing and imaging performance of hard X-rays with 20-30 nm zone plates
Hard X-ray microscopes with 20-30 nm spatial resolution ranges are an advanced tool for the inspection of materials at the nanoscale. However, the limited efficiency of the focusing optics, for example, a Fresnel zone plate (ZP) lens, can significantly reduce the power of a nanoprobe. Despite several reports on ZP lenses that focus hard X-rays with 20 nm resolution - mainly constructed by zone-doubling techniques - a systematic investigation into the limiting factors has not been reported. We report the structural effects on the focusing and imaging efficiency of 20-30 nm-resolution ZPs, employing a modified beam-propagation method. The zone width and the duty cycle (zone width/ring pitch) were optimized to achieve maximum efficiency, and a comparative analysis of the zone materials was conducted. The optimized zone structures were used in the fabrication of Pt-hydrogen silsesquioxane (HSQ) ZPs. The highest focusing efficiency of the Pt-HSQ-ZP with a resolution of 30 nm was 10% at 7 keV and >5% in the range 6-10 keV, whereas the highest efficiency of the Pt-HSQ-ZP with a resolution of 20 nm was realized at 7 keV with an efficiency of 7.6%. Optical characterization conducted at X-ray beamlines demonstrated significant enhancement of the focusing and imaging efficiency in a broader range of hard X-rays from 5 keV to 10 keV, demonstrating the potential application in hard X-ray focusing and imaging.
Development of crystal optics for X-ray multi-projection imaging for synchrotron and XFEL sources
X-ray multi-projection imaging (XMPI) is an emerging experimental technique for the acquisition of rotation-free, time-resolved, volumetric information on stochastic processes. The technique is developed for high-brilliance light-source facilities, aiming to address known limitations of state-of-the-art imaging methods in the acquisition of 4D sample information, linked to their need for sample rotation. XMPI relies on a beam-splitting scheme, that illuminates a sample from multiple, angularly spaced viewpoints, and employs fast, indirect, X-ray imaging detectors for the collection of the data. This approach enables studies of previously inaccessible phenomena of industrial and societal relevance such as fractures in solids, propagation of shock waves, laser-based 3D printing, or even fast processes in the biological domain. In this work, we discuss in detail the beam-splitting scheme of XMPI. More specifically, we explore the relevant properties of X-ray splitter optics for their use in XMPI schemes, both at synchrotron insertion devices and XFEL facilities. Furthermore, we describe two distinct XMPI schemes, designed to faciliate large samples and complex sample environments. Finally, we present experimental proof of the feasibility of MHz-rate XMPI at the European XFEL. This detailed overview aims to state the challenges and the potential of XMPI and act as a stepping stone for future development of the technique.
Synchrotron CT dosimetry for wiggler operation at reduced magnetic field and spatial modulation with bow tie filters
The Australian Synchrotron Imaging and Medical Beamline (IMBL) uses a superconducting multipole wiggler (SCMPW) source, dual crystal Laue monochromator and 135 m propagation distance to enable imaging and computed tomography (CT) studies of large samples with mono-energetic radiation. This study aimed to quantify two methods for CT dose reduction: wiggler source operation at reduced magnetic field strength, and beam modulation with spatial filters placed upstream from the sample. Transmission measurements with copper were used to indirectly quantify the influence of third harmonic radiation. Operation at lower wiggler magnetic field strength reduces dose rates by an order of magnitude, and suppresses the influence of harmonic radiation, which is of significance near 30 keV. Beam shaping filters modulate the incident beam profile for near constant transmitted signal, and offer protection to radio-sensitive surface organs: the eye lens, thyroid and female breast. Their effect is to reduce the peripheral dose and the dose to the scanned volume by about 10% for biological samples of 35-50 mm diameter and by 20-30% for samples of up to 160 mm diameter. CT dosimetry results are presented as in-air measurements that are specific to the IMBL, and as ratios to in-air measurements that may be applied to other beamlines. As CT dose calculators for small animals are yet to be developed, results presented here and in a previous study may be used to estimate absorbed dose to organs near the surface and the isocentre.
VMXm - A sub-micron focus macromolecular crystallography beamline at Diamond Light Source
VMXm joins the suite of operational macromolecular crystallography beamlines at Diamond Light Source. It has been designed to optimize rotation data collections from protein crystals less than 10 µm and down to below 1 µm in size. The beamline has a fully focused beam of 0.3 × 2.3 µm (vertical × horizontal) with a tuneable energy range (6-28 keV) and high flux (1.6 × 10 photons s at 12.5 keV). The crystals are housed within a vacuum chamber to minimize background scatter from air. Crystals are plunge-cooled on cryo-electron microscopy grids, allowing much of the liquid surrounding the crystals to be removed. These factors improve the signal-to-noise during data collection and the lifetime of the microcrystals can be prolonged by exploiting photoelectron escape. A novel in vacuo sample environment has been designed which also houses a scanning electron microscope to aid with sample visualization. This combination of features at VMXm allows measurements at the physical limits of X-ray crystallography on biomacromolecules to be explored and exploited.
Five-analyzer Johann spectrometer for hard X-ray photon-in/photon-out spectroscopy at the Inner Shell Spectroscopy beamline at NSLS-II: design, alignment and data acquisition
Here, a recently commissioned five-analyzer Johann spectrometer at the Inner Shell Spectroscopy beamline (8-ID) at the National Synchrotron Light Source II (NSLS-II) is presented. Designed for hard X-ray photon-in/photon-out spectroscopy, the spectrometer achieves a resolution in the 0.5-2 eV range, depending on the element and/or emission line, providing detailed insights into the local electronic and geometric structure of materials. It serves a diverse user community, including fields such as physical, chemical, biological, environmental and materials sciences. This article details the mechanical design, alignment procedures and data-acquisition scheme of the spectrometer, with a particular focus on the continuous asynchronous data-acquisition approach that significantly enhances experimental efficiency.
distect: automatic sample-position tracking for X-ray experiments using computer vision algorithms
Soft X-ray spectroscopy is an important technique for measuring the fundamental properties of materials. However, for measurements of samples in the sub-millimetre range, many experimental setups show limitations. Position drifts on the order of hundreds of micrometres during thermal stabilization of the system can last for hours of expensive beam time. To compensate for drifts, sample tracking and feedback systems must be used. However, in complex sample environments where sample access is very limited, many existing solutions cannot be applied. In this work, we apply a robust computer vision algorithm to automatically track and readjust the sample position in the dozens of micrometres range. Our approach is applied in a complex sample environment, where the sample is in an ultra-high vacuum chamber, surrounded by cooled thermal shields to reach sample temperatures down to 2.5 K and in the center of a superconducting split coil. Our implementation allows sample-position tracking and adjustment in the vertical direction since this is the dimension where drifts occur during sample temperature change in our setup. The approach can be easily extended to 2D. The algorithm enables a factor of ten improvement in the overlap of a series of X-ray absorption spectra in a sample with a vertical size down to 70 µm. This solution can be used in a variety of experimental stations, where optical access is available and sample access by other means is reduced.
Green upgrading of SPring-8 to produce stable, ultrabrilliant hard X-ray beams
SPring-8-II is a major upgrade project of SPring-8 that was inaugurated in October 1997 as a third-generation synchrotron radiation light source. This upgrade project aims to achieve three goals simultaneously: achievement of excellent light source performance, refurbishment of aged systems, and significant reduction in power consumption for the entire facility. A small emittance of 50 pm rad will be achieved by (1) replacing the existing double-bend lattice structure with a five-bend achromat one, (2) lowering the stored beam energy from 8 to 6 GeV, (3) increasing the horizontal damping partition number from 1 to 1.3, and (4) enhancing horizontal radiation damping by installing damping wigglers in long straight sections. The use of short-period in-vacuum undulators allows ultrabrilliant X-rays to be provided while keeping a high-energy spectral range even at the reduced electron-beam energy of 6 GeV. To reduce power consumption, the dedicated, aged injector system has been shut down and the high-performance linear accelerator of SACLA, a compact X-ray free-electron laser (XFEL) facility, is used as the injector of the ring in a time-shared manner. This allows the simultaneous operation of XFEL experiments at SACLA and full/top-up injection of the electron beam into the ring. This paper overviews the concept of the SPring-8-II project, the system design of the light source and the details of the accelerator component design.
Upgraded front ends for SLS 2.0 with next-generation high-power diaphragms and slits
The upgrade of the Swiss Light Source, called SLS 2.0, necessitates comprehensive updates to all 18 user front ends. This upgrade is driven by the increased power of the synchrotron beam, reduced floor space, changing source points, new safety regulations and enhanced beam properties, including a brightness increase by up to a factor of 40. While some existing front-end components are being thoroughly refurbished and upgraded for safety reasons, other components, especially those designed to tailor the new synchrotron beam, are being completely rebuilt. These new designs feature innovative and enhanced cooling systems to manage the high-power load and meet new requirements such as mechanical stability and compact footprints.
Mirror-centered representation of a focusing hyperbolic mirror for X-ray beamlines
Conic sections are commonly used in reflective X-ray optics. Hyperbolic mirrors can focus a converging light source and are frequently paired with elliptical or parabolic mirrors in Wolter type configurations. This paper derives the closed-form expression for a mirror-centered hyperbolic shape, with zero-slope at the origin. Combined with the slope and curvature, such an expression facilitates metrology, manufacturing and mirror-bending calculations. Previous works consider ellipses, parabolas, magnifying hyperbolas or employ lengthy approximations. Here, the exact shape function is given in terms of the mirror incidence angle and the source and image distances.
Foreword to the special virtual issue on X-ray spectroscopy to understand functional materials: instrumentation, applications, data analysis
Foreword to the virtual focused issue of Journal of Synchrotron Radiation on X-ray spectroscopy to understand functional materials: instrumentation, applications, data analysis.
Correlative X-ray micro-nanotomography with scanning electron microscopy at the Advanced Light Source
Geological samples are inherently multi-scale. Understanding their bulk physical and chemical properties requires characterization down to the nano-scale. A powerful technique to study the three-dimensional microstructure is X-ray tomography, but it lacks information about the chemistry of samples. To develop a methodology for measuring the multi-scale 3D microstructure of geological samples, correlative X-ray micro- and nanotomography were performed on two rocks followed by scanning electron microscopy with energy-dispersive spectroscopy (SEM-EDS) analysis. The study was performed in five steps: (i) micro X-ray tomography was performed on rock sample cores, (ii) samples for nanotomography were prepared using laser milling, (iii) nanotomography was performed on the milled sub-samples, (iv) samples were mounted and polished for SEM analysis and (v) SEM imaging and compositional mapping was performed on micro and nanotomography samples for complimentary information. Correlative study performed on samples of serpentine and basalt revealed multiscale 3D structures involving both solid mineral phases and pore networks. Significant differences in the volume fraction of pores and mineral phases were also observed dependent on the imaging spatial resolution employed. This highlights the necessity for the application of such a multiscale approach for the characterization of complex aggregates such as rocks. Information acquired from the chemical mapping of different phases was also helpful in segmentation of phases that did not exhibit significant contrast in X-ray imaging. Adoption of the protocol used in this study can be broadly applied to 3D imaging studies being performed at the Advanced Light Source and other user facilities.
Development of hard X-ray photoelectron spectroscopy in liquid cells using optimized microfabricated silicon nitride membranes
We present first hard X-ray photoelectron spectroscopy (HAXPES) results of aqueous salt solutions and dispersions of gold nanoparticles in liquid cells equipped with specially designed microfabricated thin silicon nitride membranes, with thickness in the 15-25 nm range, mounted in a high-vacuum-compatible environment. The experiments have been performed at the HAXPES endstation of the GALAXIES beamline at the SOLEIL synchrotron radiation facility. The low-stress membranes are fabricated from 100 mm silicon wafers using standard lithography techniques. Platinum alignment marks are added to the chips hosting the membranes to facilitate the positioning of the X-ray beam on the membrane by detecting the corresponding photoemission lines. Two types of liquid cells have been used, a static one built on an Omicron-type sample holder with the liquid confined in the cell container, and a circulating liquid cell, in which the liquid can flow in order to mitigate the effects due to beam damage. We demonstrate that the membranes are mechanically robust and able to withstand 1 bar pressure difference between the liquid inside the cell and vacuum, and the intense synchrotron radiation beam during data acquisition. This opens up new opportunities for spectroscopic studies of liquids.
Formulation of perfect-crystal diffraction from Takagi-Taupin equations: numerical implementation in the crystalpy library
The Takagi-Taupin equations are solved in their simplest form (zero deformation) to obtain the Bragg-diffracted and transmitted complex amplitudes. The case of plane-parallel crystal plates is discussed using a matrix model. The equations are implemented in an open-source Python library crystalpy adapted for numerical applications such as crystal reflectivity calculations and ray tracing.