Beamline Instrumentation Research Articles

Vibrational stability improvement of a mirror system using active mass damping.

Addressing the demand for high stability of beamline instruments at the SHINE facility, a high stability mirror regulating mechanism has been developed for mirror adjustments. Active mass damping was adopted to attenuate pitch angle vibrations of mirrors caused by structural vibrations. An internal absolute velocity feedback was used to reduce the negative impact of spillover effects and to improve performance. The experiment was conducted on a prototype structure of a mirror regulating mechanism, and results showed that the vibration RMS of the pitch angle was effectively attenuated from 47 nrad to 27 nrad above 1 Hz.

A combination of soft X-ray and laser light sources offer 3D high content information on the native state of the cellular environment

Beamline B24 is a life sciences correlative cryo-imaging beamline at Diamond Light Source. B24 uses a combination of conventional and super-resolution visible-light fluorescence microscopy and soft X-ray tomography (cryoSXT) to provide 3D imaging of the cellular landscape at a resolution up to 25 nm in cryo-preserved biological samples up to 12 μm thick. B24 offers user-friendly, semi-automated 3D correlative cryo-imaging through an integrated platform of methods that encompass (a) sample preparation and evaluation, (b) data collection and processing and (c) data analysis and correlation. CryoSXT fills the current resolution gap between fluorescence and electron microscopy while cryo-structured illumination microscopy provides the additional dimension of chemical localization within the same cellular ultrastructure captured by cryoSXT. Beamline instruments can be accessed biannually by academics and industry globally through peer-reviewed standard and rapid access proposal processes. The B24 user base is primarily academic research groups studying cell function and cytopathology in biological systems ranging from viruses and algae to mammalian cells and proto-tissue complexes. Future work will consolidate development efforts and experiences gained thus far to enable high-throughput data collection. Special emphasis is placed on the delivery of other integrated advanced imaging methods such as X-ray absorption near-edge spectroscopy and phase contrast.

Status of LBNF/DUNE near site liquid argon proximity and external cryogenics systems development.

The Deep Underground Neutrino Experiment (DUNE) near site located at Fermilab will host the neutrino beam complex. It includes a high voltage liquid argon time projection chamber located 60-meter underground used as beamline instrumentation. The LAr cryogenic system provided by the Long-Baseline Neutrino Facility (LBNF) regulates thermohydraulic conditions of the membrane cryostat hosting the detector with 285 Ton purified LAr. The purification system uses molecular sieve and copper oxide pellets to manage the argon contamination below 100 ppt (parts per trillion) oxygen equivalent. The detector and its cryogenics are capable to move a stroke of 30 meters on/off beam. The cryogenic system modes of operation include the cryostat pressure test, purge in open loop, detector cooldown, cryostat fill, closed loop purification, liquid empty, and purification system activation/regeneration process. The system design status and schedule, and technical details such as operating modes and interfaces are reported in this paper.

Predictive modeling through Dynamic Error Budgeting applied to the High-Dynamic Double-Crystal Monochromator for Sirius light source

To address recent and more stringent nanometer-level requirements in positioning stability, the High-Dynamic Double-Crystal Monochromator (HD-DCM) has been in development since 2015 for X-ray beamlines of Sirius, the 4th-generation light source at the Brazilian Synchrotron Light Laboratory (LNLS). The unprecedented 10 nrad RMS (1Hz-2.5 kHz) inter-crystal parallelism in fixed and scanning modes represents improvements by factors of 5 and 100 with respect to state-of-the-art DCMs, respectively — which became possible only due to its innovative isolated mechatronic architecture with high closed-loop performance, rigorous precision engineering principles, and predictive design via Dynamic Error Budgeting (DEB). This work demonstrates the DEB methodology applied to the HD-DCM via a three-dimensional-space mechatronic model based on a lumped-mass system of 11 rigid bodies. Special attention is given to the disturbance models based on measurements and to performance prediction in fixed-energy operation mode, which is finally compared with experimental results in the real system. Hence, this article presents the step-by-step predictive modeling process of the HD-DCM as a successful case study on the efficient development of innovative high-performance mechatronic machines, which could be a game changer in synchrotron beamline instrumentation.

The "Historical Materials BAG": A New Facilitated Access to Synchrotron X-ray Diffraction Analyses for Cultural Heritage Materials at the European Synchrotron Radiation Facility.

The European Synchrotron Radiation Facility (ESRF) has recently commissioned the new Extremely Brilliant Source (EBS). The gain in brightness as well as the continuous development of beamline instruments boosts the beamline performances, in particular in terms of accelerated data acquisition. This has motivated the development of new access modes as an alternative to standard proposals for access to beamtime, in particular via the “block allocation group” (BAG) mode. Here, we present the recently implemented “historical materials BAG”: a community proposal giving to 10 European institutes the opportunity for guaranteed beamtime at two X-ray powder diffraction (XRPD) beamlines—ID13, for 2D high lateral resolution XRPD mapping, and ID22 for high angular resolution XRPD bulk analyses—with a particular focus on applications to cultural heritage. The capabilities offered by these instruments, the specific hardware and software developments to facilitate and speed-up data acquisition and data processing are detailed, and the first results from this new access are illustrated with recent applications to pigments, paintings, ceramics and wood.

A Sample Preparation Pipeline for Microcrystals at the VMXm Beamline.

The mounting of microcrystals (<10 µm) for single crystal cryo-crystallography presents a non-trivial challenge. Improvements in data quality have been seen for microcrystals with the development of beamline optics, beam stability and variable beam size focusing from submicron to microns, such as at the VMXm beamline at Diamond Light Source1. Further improvements in data quality will be gained through improvements in sample environment and sample preparation. Microcrystals inherently generate weaker diffraction, therefore improving the signal-to-noise is key to collecting quality X-ray diffraction data and will predominantly come from reductions in background noise. Major sources of X-ray background noise in a diffraction experiment are from their interaction with the air path before and after the sample, excess crystallization solution surrounding the sample, the presence of crystalline ice and scatter from any other beamline instrumentation or X-ray windows. The VMXm beamline comprises instrumentation and a sample preparation protocol to reduce all these sources of noise. Firstly, an in-vacuum sample environment at VMXm removes the air path between X-ray source and sample. Next, sample preparation protocols for macromolecular crystallography at VMXm utilize a number of processes and tools adapted from cryoTEM. These include copper grids with holey carbon support films, automated blotting and plunge cooling robotics making use of liquid ethane. These tools enable the preparation of hundreds of microcrystals on a single cryoTEM grid with minimal surrounding liquid on a low-noise support. They also minimize the formation of crystalline ice from any remaining liquid surrounding the crystals. We present the process for preparing and assessing the quality of soluble protein microcrystals using visible light and scanning electron microscopy before mounting the samples on the VMXm beamline for X-ray diffraction experiments. We will also provide examples of good quality samples as well as those which require further optimization and strategies to do so.

A Sample Preparation Pipeline for Microcrystals at the VMXm Beamline

The mounting of microcrystals (<10 µm) for single crystal cryo-crystallography presents a non-trivial challenge. Improvements in data quality have been seen for microcrystals with the development of beamline optics, beam stability and variable beam size focusing from submicron to microns, such as at the VMXm beamline at Diamond Light Source1. Further improvements in data quality will be gained through improvements in sample environment and sample preparation. Microcrystals inherently generate weaker diffraction, therefore improving the signal-to-noise is key to collecting quality X-ray diffraction data and will predominantly come from reductions in background noise. Major sources of X-ray background noise in a diffraction experiment are from their interaction with the air path before and after the sample, excess crystallization solution surrounding the sample, the presence of crystalline ice and scatter from any other beamline instrumentation or X-ray windows. The VMXm beamline comprises instrumentation and a sample preparation protocol to reduce all these sources of noise. Firstly, an in-vacuum sample environment at VMXm removes the air path between X-ray source and sample. Next, sample preparation protocols for macromolecular crystallography at VMXm utilize a number of processes and tools adapted from cryoTEM. These include copper grids with holey carbon support films, automated blotting and plunge cooling robotics making use of liquid ethane. These tools enable the preparation of hundreds of microcrystals on a single cryoTEM grid with minimal surrounding liquid on a low-noise support. They also minimize the formation of crystalline ice from any remaining liquid surrounding the crystals. We present the process for preparing and assessing the quality of soluble protein microcrystals using visible light and scanning electron microscopy before mounting the samples on the VMXm beamline for X-ray diffraction experiments. We will also provide examples of good quality samples as well as those which require further optimization and strategies to do so.

Combining X-rays, neutrons and electrons, and NMR, for precision and accuracy in structure-function studies.

The distinctive features of the physics-based probes used in understanding the structure of matter focusing on biological sciences, but not exclusively, are described in the modern context. This is set in a wider scope of holistic biology and the scepticism about `reductionism', what is called the `molecular level', and how to respond constructively. These topics will be set alongside the principles of accuracy and precision, and their boundaries. The combination of probes and their application together is the usual way of realizing accuracy. The distinction between precision and accuracy can be blurred by the predictive force of a precise structure, thereby lending confidence in its potential accuracy. These descriptions will be applied to the comparison of cryo and room-temperature protein crystal structures as well as the solid state of a crystal and the same molecules studied by small-angle X-ray scattering in solution and by electron microscopy on a sample grid. Examples will include: time-resolved X-ray Laue crystallography of an enzyme Michaelis complex formed directly in a crystal equivalent to in vivo; a new iodoplatin for radiation therapy predicted from studies of platin crystal structures; and the field of colouration of carotenoids, as an effective assay of function, i.e. their colouration, when unbound and bound to a protein. The complementarity of probes, as well as their combinatory use, is then at the foundation of real (biologically relevant), probe-artefacts-free, structure-function studies. The foundations of our methodologies are being transformed by colossal improvements in technologies of X-ray and neutron sources and their beamline instruments, as well as improved electron microscopes and NMR spectrometers. The success of protein structure prediction from gene sequence recently reported by CASP14 also opens new doors to change and extend the foundations of the structural sciences.

First results on ProtoDUNE-SP liquid argon time projection chamber performance from a beam test at the CERN Neutrino Platform

The ProtoDUNE-SP detector is a single-phase liquid argon time projection chamber with an active volume of 7.2× 6.1× 7.0 m3. It is installed at the CERN Neutrino Platform in a specially-constructed beam that delivers charged pions, kaons, protons, muons and electrons with momenta in the range 0.3 GeV/c to 7 GeV/c. Beam line instrumentation provides accurate momentum measurements and particle identification. The ProtoDUNE-SP detector is a prototype for the first far detector module of the Deep Underground Neutrino Experiment, and it incorporates full-size components as designed for that module. This paper describes the beam line, the time projection chamber, the photon detectors, the cosmic-ray tagger, the signal processing and particle reconstruction. It presents the first results on ProtoDUNE-SP's performance, including noise and gain measurements, dE/dx calibration for muons, protons, pions and electrons, drift electron lifetime measurements, and photon detector noise, signal sensitivity and time resolution measurements. The measured values meet or exceed the specifications for the DUNE far detector, in several cases by large margins. ProtoDUNE-SP's successful operation starting in 2018 and its production of large samples of high-quality data demonstrate the effectiveness of the single-phase far detector design.

The CLAS12 beamline and its performance

This paper describes the Hall B beamline and its performance during the first year of data-taking operation using the CLAS12 detector. We review the beamline instrumentation used to measure and monitor the beam. This instrumentation led to excellent beam quality for energies ranging from 2.2 to 10.6 GeV at the design luminosity of 1035 cm−2s−1. The instrumentation includes a Møller polarimeter, which can typically measure the beam polarization to an absolute precision of ∼2.5%.

The Heavy Ion Accelerator Facility: Research Achievements and Aspirations

An overview of Australia’s Heavy Ion Accelerator Facility (HIAF) is presented, including a survey of the accelerator infrastructure and its capabilities, as well as the beam-line instrumentation. Some recent research achievements are highlighted. Accelerator upgrades and instrumentation developments in progress are described, along with some aspirations for the longer-term development of the Facility and its associated research programs.

SEE Tests With Ultra Energetic Xe Ion Beam in the CHARM Facility at CERN

Taking advantage of the heavy ion acceleration program, tests on radiation effects with Ultrahigh Energy (UHE) xenon ion beams (with Energy > 5 GeV/nucleon) have been performed in several experimental areas of the CERN accelerator complex. Specifically, the outcomes of the first UHE heavy ion test campaign carried out at the CHARM facility are presented and discussed in this contribution. UHE ion beams have the advantage of not requiring a previous modification of the samples or testing in vacuum, owing to their large penetration range. The unique nature of the UHE ions motivated the study of their interaction with matter, with regard to the induction of SEE. To that end, great effort was paid on the calibration of the beam line instrumentation, typically prepared for the traditional proton runs. Electronic components sensitive to single event upset (SEU) and single-event latchup (SEL) were irradiated by an UHE xenon beam, with a particular interest in studying the sub-LET cross section region and benchmarking against the standard heavy ion test beams. Finally, the suitability of UHE ion testing for Radiation Hardness Assurance is also discussed in the contribution.

Fifteen Years of Radionuclide Research at the KIT Synchrotron Source in the Context of the Nuclear Waste Disposal Safety Case

For more than 120 years, systematic studies of X-ray interaction with matter have been the basis for our understanding of materials—both of natural or man-made origin—and their structure-function relationships. Beginning with simple radiographic imaging at the end of the 19th century, X-ray based analytical tools such as X-ray diffraction, X-ray fluorescence and photoemission or X-ray absorption techniques are indispensable in almost any field of chemical and material sciences—including basic and applied actinide and radionuclide studies. The advent of dedicated synchrotron radiation (SR) sources in the second half of the last century has revolutionized the analytical power of X-ray probes, while—with increasing number of SR facilities—beamline instrumentation followed a trend towards increasing specialization and adaption to a major research topic. The INE-Beamline and ACT station at the KIT synchrotron source belong to the exclusive club of a few synchrotron beamline facilities—mostly located in Europe—dedicated to the investigation of highly radioactive materials. Since commissioning of the INE-Beamline in 2005, capabilities for synchrotron-based radionuclide and actinide sciences at KIT have been continuously expanded, driven by in-house research programs and external user needs.

An integrated remote data collection system for macromolecular crystallography beamline at SSRF

Remote data collection is a rapidly growing area in many synchrotrons. With the increasing requirement for remote data collection from users of macromolecular crystallography beamline BL17U1 in Shanghai Synchrotron Radiation Facility (SSRF), an integrated remote data collection system based on Blu-Ice/DCS has been developed. Owing to the advances in the beamline instruments, the process of diffraction data collection which include the sample mount, crystal centering and data set collection can be executed full automatically on site. To let the external users access the intranet of SSRF, a VPN is set with authorization. The authorized user could login to the control computer and lunch the user graphic interface under the beam time management system. The remote users conduct their experiment from the virtual desktop by NoMachine client. To improve the efficiency on the high data-rate macromolecular crystallography beamline, data process pipeline display the results by web page.

Sample manipulation and data assembly for robust microcrystal synchrotron crystallography.

With the recent developments in microcrystal handling, synchrotron microdiffraction beamline instrumentation and data analysis, microcrystal crystallo-graphy with crystal sizes of less than 10 µm is appealing at synchrotrons. However, challenges remain in sample manipulation and data assembly for robust microcrystal synchrotron crystallography. Here, the development of micro-sized polyimide well-mounts for the manipulation of microcrystals of a few micrometres in size and the implementation of a robust data-analysis method for the assembly of rotational microdiffraction data sets from many microcrystals are described. The method demonstrates that microcrystals may be routinely utilized for the acquisition and assembly of complete data sets from synchrotron microdiffraction beamlines.

Current Status of Single Particle Imaging with X-ray Lasers

The advent of ultrafast X-ray free-electron lasers (XFELs) opens the tantalizing possibility of the atomic-resolution imaging of reproducible objects such as viruses, nanoparticles, single molecules, clusters, and perhaps biological cells, achieving a resolution for single particle imaging better than a few tens of nanometers. Improving upon this is a significant challenge which has been the focus of a global single particle imaging (SPI) initiative launched in December 2014 at the Linac Coherent Light Source (LCLS), SLAC National Accelerator Laboratory, USA. A roadmap was outlined, and significant multi-disciplinary effort has since been devoted to work on the technical challenges of SPI such as radiation damage, beam characterization, beamline instrumentation and optics, sample preparation and delivery and algorithm development at multiple institutions involved in the SPI initiative. Currently, the SPI initiative has achieved 3D imaging of rice dwarf virus (RDV) and coliphage PR772 viruses at ~10 nm resolution by using soft X-ray FEL pulses at the Atomic Molecular and Optical (AMO) instrument of LCLS. Meanwhile, diffraction patterns with signal above noise up to the corner of the detector with a resolution of ~6 Ångström (Å) were also recorded with hard X-rays at the Coherent X-ray Imaging (CXI) instrument, also at LCLS. Achieving atomic resolution is truly a grand challenge and there is still a long way to go in light of recent developments in electron microscopy. However, the potential for studying dynamics at physiological conditions and capturing ultrafast biological, chemical and physical processes represents a tremendous potential application, attracting continued interest in pursuing further method development. In this paper, we give a brief introduction of SPI developments and look ahead to further method development.

Coherence Length and Vibrations of the Coherence Beamline I13 at the Diamond Light Source

I13 is a 250 m long hard x-ray beamline for imaging and coherent diffraction at the Diamond Light Source. The beamline (6 keV to 35 keV) comprises two independent experimental endstations: one for imaging in direct space using x-ray microscopy and one for imaging in reciprocal space using coherent diffraction based imaging techniques [1]. In particular the coherence experiments pose very high demands on the performance on the beamline instrumentation, requiring extensive testing and optimisation of each component, even during the assembly phase. Various aspects like the quality of optical components, the mechanical design concept, vibrations, drifts, thermal influences and the performance of motion systems are of particular importance. In this paper we study the impact of the front-end slit size (FE slit size), which determines the horizontal source size, onto the coherence length and the detrimental impact of monochromator vibrations using in-situ x-ray metrology in conjunction with fringe visibility measurements and vibration measurements, based on centroid tracking of an x-ray pencil beam with a photon-counting detector.

SUT-NANOTEC-SLRI beamline for X-ray absorption spectroscopy.

The SUT-NANOTEC-SLRI beamline was constructed in 2012 as the flagship of the SUT-NANOTEC-SLRI Joint Research Facility for Synchrotron Utilization, co-established by Suranaree University of Technology (SUT), National Nanotechnology Center (NANOTEC) and Synchrotron Light Research Institute (SLRI). It is an intermediate-energy X-ray absorption spectroscopy (XAS) beamline at SLRI. The beamline delivers an unfocused monochromatic X-ray beam of tunable photon energy (1.25-10 keV). The maximum normal incident beam size is 13 mm (width) × 1 mm (height) with a photon flux of 3 × 108 to 2 × 1010 photons s-1 (100 mA)-1 varying across photon energies. Details of the beamline and XAS instrumentation are described. To demonstrate the beamline performance, K-edge XANES spectra of MgO, Al2O3, S8, FeS, FeSO4, Cu, Cu2O and CuO, and EXAFS spectra of Cu and CuOare presented.

SIRIUS: A new beamline for in situ X-ray diffraction and spectroscopy studies of advanced materials and nanostructures at the SOLEIL Synchrotron

We present a new beamline of Synchrotron SOLEIL dedicated to the study of thin films, nanostructures, and advanced materials via X-ray diffraction and spectroscopy in the energy range 1.4–12keV. This range covers most of the absorption edges of interest in the fields of semiconductors and functional oxides. In order to meet the increasing demand of advanced real-time characterization of nanoscale materials, the beamline optics and instrumentation have been designed with remarkable dynamic characteristics. SIRIUS presently ends in two experimental stations used for in situ X-ray characterization: a baby chamber and a chemical reactor, both mounted on a large seven-circle diffractometer. The rector is dedicated to atomic layer deposition and metal organic chemical vapor deposition of oxide materials. The third end-station, an in-vacuum diffractometer, will be operative by the end of 2016. SIRIUS offers several synchrotron radiation techniques which can be performed simultaneously or quasi-simultaneously on the same sample. We show here some examples of the first in situ results obtained at the beamline.

Radiation damage in polymer films from grazing‐incidence X‐ray scattering measurements

ABSTRACTGrazing‐incidence X‐ray scattering (GIXS) is widely used to analyze the crystallinity and nanoscale structure in thin polymer films. However, ionizing radiation will generate free radicals that initiate crosslinking and/or chain scission, and structural damage will impact the ordering kinetics, thermodynamics, and crystallinity in many polymers. We report a simple methodology to screen for beam damage that is based on lithographic principles: films are exposed to patterns of X‐ray radiation, and changes in polymer structure are revealed by immersing the film in a solvent that dissolves the shortest chains. The experiments are implemented with high throughput using the standard beam line instrumentation and a typical GIXS configuration. The extent of damage (at a fixed radiation dose) depends on a range of intrinsic material properties and experimental variables, including the polymer chemistry and molecular weight, exposure environment, film thickness, and angle of incidence. The solubility switch for common polymers is detected within 10–60 s at ambient temperature, and we verified that this first indication of damage corresponds with the onset of network formation in glassy polystyrene and a loss of crystallinity in polyalkylthiophenes. Therefore, grazing‐incidence X‐ray “patterning” offers an efficient approach to determine the appropriate data acquisition times for any GIXS experiment. © 2016 Wiley Periodicals, Inc. J. Polym. Sci., Part B: Polym. Phys. 2016, 54, 1074–1086