Beamline Endstation Research Articles

VerSoX B07-B: a high-throughput XPS and ambient pressure NEXAFS beamline at Diamond Light Source.

The beamline optics and endstations at branch B of the Versatile Soft X-ray (VerSoX) beamline B07 at Diamond Light Source are described. B07-B provides medium-flux X-rays in the range 45-2200 eV from a bending magnet source, giving access to local electronic structure for atoms of all elements from Li to Y. It has an endstation for high-throughput X-ray photoelectron spectroscopy (XPS) and near-edge X-ray absorption fine-structure (NEXAFS) measurements under ultrahigh-vacuum (UHV) conditions. B07-B has a second endstation dedicated to NEXAFS at pressures from UHV to ambient pressure (1 atm). The combination of these endstations permits studies of a wide range ofinterfaces and materials. The beamline and endstation designs are discussed in detail, as well as their performance and the commissioning process.

X-ray absorption fine structure (XAFS)-based radionuclide research at the KIT Light Source

Abstract. In the past two decades, X-ray absorption spectroscopy (XAS) and related synchrotron-based radionuclide speciation techniques have become indispensable, supporting open issues in fundamental radiochemistry and nuclear waste disposal alike. Physicochemical structure information – encoded in the element-specific X-ray absorption fine structure (XAFS) – is obtained by the precise determination of the linear mass absorption coefficient μ(E) of a specimen in an X-ray energy window ΔE encompassing an electronic bonding level of a selected atom type. The characteristic modulations of μ(E) in the vicinity of an “absorption edge” (i.e., the steeply rising absorption probability of photons tuned to the binding energy of inner shell “core” electrons) are attributed to electronic transitions into unoccupied states due to the photoelectric effect. While absorption features close to the edge (arising from excitations into molecular orbitals or empty band structure levels close to the Fermi level) are generally denoted as an X-ray absorption near-edge structure (XANES), the scattering states at higher excitation energies are causing the well-known extended X-ray absorption fine structure (EXAFS). EXAFS oscillations of the post-edge μ(E) are caused by the periodicity of the constructive and destructive interference of outbound and backscattered inbound photoelectron waves (superimposing at the absorbing atom site) when continuously increasing the excitation energy. Quantitative analysis of EXAFS data based on electron scattering theory is a well-established short-range structural probe, providing precise values of interatomic distances (between the absorber atom and its neighbors) and additional information on the type, number, and ordering of neighbor atoms within a local cluster. Recent significant advancements in the quantum theoretical description of core-excited final states have been successful in overcoming persisting ambiguities in XANES data interpretation. Meanwhile, although there are more than 50 synchrotron radiation centers operational in the world, facilities with specialized beamline infrastructure and safety protocols to allow experiments on radioactive samples with activities beyond the exemption limits are still scarce. At the KIT Light Source (at the Karlsruhe Institute of Technology, Karlsruhe, Germany), the Institute for Nuclear Waste Disposal (Institut für Nukleare Entsorgung, INE) operates two beamline end-stations dedicated to the investigation of radionuclide materials by XAFS spectroscopy and related techniques, i.e., the INE-Beamline (operational since 2005) and the ACT station of the CAT-ACT (CATalysis and ACTinide) wiggler beamline (operational since 2016). Samples with total activities amounting to 1.0×106 times the isotope specific exemption limits and 200 mg of fissile isotopes 235U and 239Pu are feasible at both beamlines. Highly versatile detection systems and sample holders – generally avoiding extensive shielding or sample handling in a glove box – have been conceived since the initial commissioning of the beamlines and have enabled unique XAFS measurements such as the first ever investigation of aqueous technetium species at the Tc L3 edge. Investigations of highly radioactive specimens (e.g., spent nuclear fuel or nuclear waste glass fragments) are feasible, regardless of the actual contact dose rate if the radiation field is limited to a few microsieverts per hour at the edge of the experimental table.

ALBA Synchrotron and its future

The ALBA Synchrotron light source is the Spanish national facility, providing extended research capabilities and a wide range of state-of-the-art instrumentation to academic and industrial users of the Spanish and European Research Area since 2012. It includes ten operating beamlines, two beamlines in commissioning and two more in construction. JEMCA (Joint Electron Microscopy Center at ALBA), a center including advanced electron microscopes, developed in collaboration with partner institutions, has recently been inaugurated. The next years will be dedicated to exploit the existing instrumentation, and in parallel prepare the upgrade toward a fourth generation synchrotron source, by combining the partial substitution of the accelerators with the upgrade of the existing instrumentation, the addition of new cutting-edge beamlines, the development of further capabilities for automatization, simulation, prototyping, nanotechnology and advanced optics, and the extension of the infrastructure in the nearby plots, which will host the new long beamline end-stations and aim at being the seed of a science, technology and innovation park. The 2-year dark period is foreseen for the end of this decade. The status of the facility, few scientific highlights, and the plans for the future are described.

In situ and operando study of catalysts during high-temperature high-pressure catalysis in a fixed-bed plug flow reactor with x-ray absorption spectroscopy.

Numerous important catalytic reactions, such as Fischer-Tropsch synthesis (FTS), are performed under harsh conditions in terms of high temperature of a catalyst in a mixture of reactants at a high pressure. There has been a lack of an intrinsic correlation between a catalytic performance and its corresponding catalyst structure due to the unavailable information on the authentic structure of the catalyst during catalysis under a high-temperature high-pressure (HTHP) condition. Here, we report in situ/operando studies of Co catalysts during catalysis under HTHP conditions using x-ray absorption spectroscopy (XAS). A high-temperature high-pressure catalysis-XAS (HTHP Catalysis-XAS) system using a thin, small quartz or beryllium tube as the reactor was built for in situ/operando characterization of high-energy absorption edges of 4d transition metals or low-energy absorption edges of 3d/4d transition metals under high-temperature high-pressure conditions, respectively. This reactor can be used for HTHP catalysis performed at a temperature of up to 550 °C and a gas pressure of up to 60 bars for uncovering the chemical states and coordination environments of metal atoms of these catalysts during HTHP catalysis. The capability of collecting XAS data during HTHP catalysis was confirmed through tests at 400oC in the mixture of 20 bar mixture of reactants at beamline endstation. The operando studies of Ru catalyst particles under Fischer-Tropsch catalytic conditions with extended x-ray absorption fine structure spectroscopy revealed a restructuring of the Ru catalyst at 250 °C in the mixture of 6 bars CO and 12 bars H2 during FTS (30 ml/min), which was not observed at 300 °C in 1bar H2 (20 ml/min). This observation suggests new chemistry for metal catalysts under HTHP condition inaccessible due to a lack of applicable characterizations. These tests confirmed the function of this HTHP Catalysis-XAS system for in situ/operando characterizations of catalysts during HTHP catalysis.

Commissioning of a gas monitor detector for an undulator beamline in the VUV and EUV wavelength range

A gas detector system was implemented to monitor the absolute photon flux at the insertion device beamline of the Metrology Light Source. This system should overcome the drawbacks in the use of traceably calibrated semiconductor photodiodes, which are prone to radiation-induced degradation and not qualified for permanent real-time monitoring during the measurements at the beamline endstation. Gas monitor detectors are based on atomic photoionization. They do not suffer from radiation-induced degradation, and their transparency makes them suitable for real-time monitoring of the photon flux. We calibrated and commissioned such a monitor at the insertion device beamline in the vacuum- and extreme ultraviolet spectral range from 14 eV to 111 eV photon energy. The resulting photon flux measurement was compared to measurements made with a photodiode and shows deviations below 5 %, which agrees well with the calculated relative uncertainty of 4.7 %.

Introduction of the liquid nitrogen transfer line for TPS beamline endstation

At Taiwan Photon Source (TPS), the main liquid-nitrogen (LN2) transfer line of length 600 m for beamline endstations was installed in 2015. It formerly supplied LN2 to maximum 24 beamline endstations. Beamline endstation 13A, of which the aim is advanced and general studies of biological structures and structural kinetics in solution or condensed forms under environmental simulations, from atomic to micrometre scale and time resolution from microsecond to minute, was installed during 2018 and 2019. We designed and self-manufactured one LN2 transfer line according to the requirement of beamline endstation 13A, to supply LN2 into the double-crystal monochromator (DCM), to solve the problem of thermal deformation of the crystal. Otherwise the keep-full device was designed to replace the phase separator of the chiller. In this paper we present the pipeline design, performance testing, keep-full device, pressure reducer, noise reduction and heat-load measurement.

Size and structure of hexanuclear plutonium oxo-hydroxo clusters in aqueous solution from synchrotron analysis.

The size and shape of a water-soluble hexanuclear plutonium cluster were probed by combining synchrotron small-angle X-ray scattering (SAXS) and extended X-ray absorption fine structure (EXAFS). A specific setup coupling both techniques and dedicated to radioactive samples on the MARS beamline endstation at Synchrotron SOLEIL is described. The plutonium hexanuclear cores are well stabilized by the 1,4,7,10-tetraazacyclododecane-1,4,7,10-tetraacetic acid ligands and this allows a good evaluation of the setup to probe the very small plutonium core. The results show that, in spite of the constrained conditions required to avoid any risk of sample dispersion, the flux and the sample environment are optimized to obtain a very good signal-to-noise ratio, allowing the detection of small plutonium aggregates in an aqueous phase. The structure of the well defined hexanuclear cluster has been confirmed by EXAFS measurements in solution and correlated with SAXS data processing and modelling. An iterative comparison of classical fit models (Guinier or sphere form factor) with the experimental results allowed a better interpretation of the SAXS signal that will be relevant for future work under environmentally relevant conditions.

A UHV MOKE magnetometer complementing XMCD-PEEM at the Elettra Synchrotron

We report on a custom-built UHV-compatible Magneto-Optical Kerr Effect (MOKE) magnetometer for applications in surface and materials sciences, operating in tandem with the PhotoEmission Electron Microscope (PEEM) endstation at the Nanospectroscopy beamline of the Elettra synchrotron. The magnetometer features a liquid-nitrogen-cooled electromagnet that is fully compatible with UHV operation and produces magnetic fields up to about 140 mT at the sample. Longitudinal and polar MOKE measurement geometries are realized. The magneto-optical detection is based on polarization analysis using a photoelastic modulator. The sample manipulation system is fully compatible with that of the PEEM, making it possible to exchange samples with the beamline endstation, where complementary X-ray imaging and spectroscopy techniques are available. The magnetometer performance is illustrated by experiments on cobalt ultra-thin films, demonstrating close to monolayer sensitivity. The advantages of combining in situ growth, X-ray Magnetic Circular Dichroism imaging (XMCD-PEEM) and MOKE magnetometry into a versatile multitechnique facility are highlighted.

Development of basic theory and application of cryogenic X-ray spectrometer in light sources and X-ray satellite

Cryogenic X-ray spectrometers are advantageous in the spectrum research for weak and diffusive X-ray source due to their high energy resolution, high detection efficiency, low noise level and non-dead-layer properties. Their energy resolution independent of the incident X-ray direction also makes them competitive in diffusion source detection. The requirements for X-ray spectrometers have heightened in recent years with the rapid development of large scientific facilities where X-ray detection is demanded, including beamline endstations in synchrotron and X-ray free electron laser facilities, accelerators, highly charged ion traps, X-ray space satellites, etc. Because of their excellent performances, cryogenic X-ray detectors are introduced into these facilities, typical examples of which are APS, NSLS, LCLS-II, Spring-8, SSNL, ATHENA, HUBS. In this paper, we review the cryogenic X-ray spectrometers, from the working principle and classification, system structure, major performance characteristics to the research status and trend in large scientific facilities in the world.

An optimized 19F (p, αγ)16O elemental mapping facility

A new target stage that allows a close positioning of a large 5in × 5in NaI(Tl) detector was implemented at the 45° beam-line end-station at the Centre for Ion Beam Applications (CIBA). Here we present preliminary results demonstrating the improvement in the F detection limit available in the new geometry. The reaction 19F(p, αγ)16O was used to map fluorine in untreated and fluorine/laser treated areas on human tooth samples.Proton Induced Gamma-Ray Emission (PIGE) was used in combination with Proton Induced X-Ray Emission (PIXE) and Rutherford Backscattering Spectrometry (RBS) for quantitative elemental mapping of fluorine. A 2 MeV proton beam focused to 5~10 μm spot size with a beam current of 0.5–1 nA was used along with a new in-vacuum piezo-driven three-axis target-stage at the nuclear microscopy beamline end-station. The new stage, which replaces the manual target positioning system, optimizes the solid angle subtended by factor of 13.

A setup for extreme-ultraviolet ultrafast angle-resolved photoelectron spectroscopy at 50-kHz repetition rate.

Time- and angle-resolved photoelectron spectroscopy (trARPES) is a powerful method to track the ultrafast dynamics of quasiparticles and electronic bands in energy and momentum space. We present a setup for trARPES with 22.3 eV extreme-ultraviolet (XUV) femtosecond pulses at 50-kHz repetition rate, which enables fast data acquisition and access to dynamics across momentum space with high sensitivity. The design and operation of the XUV beamline, pump-probe setup, and ultra-high vacuum endstation are described in detail. By characterizing the effect of space-charge broadening, we determine an ultimate source-limited energy resolution of 60 meV, with typically 80-100 meV obtained at 1-2 × 1010 photons/s probe flux on the sample. The instrument capabilities are demonstrated via both equilibrium and time-resolved ARPES studies of transition-metal dichalcogenides. The 50-kHz repetition rate enables sensitive measurements of quasiparticles at low excitation fluences in semiconducting MoSe2, with an instrumental time resolution of 65 fs. Moreover, photo-induced phase transitions can be driven with the available pump fluence, as shown by charge density wave melting in 1T-TiSe2. The high repetition-rate setup thus provides a versatile platform for sensitive XUV trARPES, from quenching of electronic phases down to the perturbative limit.

A reaction cell for ambient pressure soft x-ray absorption spectroscopy.

We present a new experimental setup for performing X-ray Absorption Spectroscopy (XAS) in the soft X-ray range at ambient pressure. The ambient pressure XAS setup is fully compatible with the ultra high vacuum environment of a synchrotron radiation spectroscopy beamline end station by means of ultrathin Si3N4 membranes acting as windows for the X-ray beam and seal of the atmospheric sample environment. The XAS detection is performed in total electron yield (TEY) mode by probing the drain current from the sample with a picoammeter. The high signal/noise ratio achievable in the TEY mode, combined with a continuous scanning of the X-ray energies, makes it possible recording XAS spectra in a few seconds. The first results show the performance of this setup to record fast XAS spectra from sample surfaces exposed at atmospheric pressure, even in the case of highly insulating samples. The use of a permanent magnet inside the reaction cell enables the measurement of X-ray magnetic circular dichroism at ambient pressure.

MX2: a high-flux undulator microfocus beamline serving both the chemical and macromolecular crystallography communities at the Australian Synchrotron.

MX2 is an in-vacuum undulator-based crystallography beamline at the 3 GeV Australian Synchrotron. The beamline delivers hard X-rays in the energy range 4.8-21 keV to a focal spot of 22 × 12 µm FWHM (H × V). At 13 keV the flux at the sample is 3.4 × 1012 photons s-1. The beamline endstation allows robotic handling of cryogenic samples via an updated SSRL SAM robot. This beamline is ideal for weakly diffracting hard-to-crystallize proteins, virus particles, protein assemblies and nucleic acids as well as smaller molecules such as inorganic catalysts and organic drug molecules. The beamline is now mature and has enjoyed a full user program for the last nine years. This paper describes the beamline status, plans for its future and some recent scientific highlights.

A first evaluation of the analytical capabilities of the new X-ray fluorescence facility at International Atomic Energy Agency-Elettra Sincrotrone Trieste for multipurpose total reflection X-ray fluorescence analysis

The aim of the work is to present a systematic evaluation of the analytical capabilities of the new X-ray fluorescence facility jointly operated between the International Atomic Energy Agency and the Elettra Sincrotrone Trieste for multipurpose total reflection X-ray fluorescence analysis.The analytical performance of the XRF beamline end-station (IAEAXspe) was systematically evaluated under TXRF excitation geometry by analyzing different types of aqueous (lake, waste and fresh water) and solid (soil, vegetal, biological) certified reference materials using an excitation energy of 13.0keV (for the purpose of multielemental analysis). The results obtained for both types of samples in terms of limits of detection and accuracy were also compared with those obtained using laboratory X-ray tube based TXRF systems with different features (including Mo and W X-ray tube systems). Taking advantage of the possibility to work under high vacuum, the IAEAXspe set-up instrumental sensitivity was also determined using an excitation energy of 6.2keV to explore the possibilities for light elements determination.A clear improvement of the element detection limits is achieved when comparing this facility to conventional X-ray tube based TXRF systems highlighting the benefits of using the monoenergetic synchrotron exciting radiation and the ultra-high vacuum chamber in comparison with conventional laboratory systems.The results of the present work are discussed in view of further exploitation of the facility for different environmental and biological related applications.

IBC - ION BEAM CENTER

In the Ion Beam Center (IBC), various set-ups – electrostatic accelerators, ion implanters, plasma-based ion implantation equipment, low-energy ion tools, an ion microscope etc. – are combined into a unique facility for research and applications using ion beams. Almost all ions from stable chemical nuclides are available in the ion energy range from 10 eV to about 60 MeV. In addition to broad beams, also focused (down to 1 nm) and highly-charged (charge state up to 45+) ion beams, or ions extracted from a plasma can be provided. In total, the IBC operates more than 30 dedicated tools or beamline end-stations. The specific expertise of IBC is the modification and analysis of solids by energetic ions aimed to develop novel materials for information technology, electronics or energy systems. In addition, ion beam analysis techniques became of increasing importance for interdisciplinary fields like geochemistry, climate or environmental research and resources technology. Special add-on services offered ensure a successful realization of user experiments. Based on a long-term expertise, specific equipment and common commercial procedures, the IBC is strongly active in the use of ion beam techniques for industrial applications aimed to initiate valuable product innovation.

Low Dose Photoelectron Spectroscopy at BESSY II: Electronic structure of matter in its native state

The implementation of a high-transmission, angular-resolved time-of-flight electron spectrometer with a 1.25MHz pulse selector at the PM4 soft X-ray dipole beamline of the synchrotron BESSY II creates unique capabilities to inquire electronic structure via photoelectron spectroscopy with a minimum of radiation dose. Solid-state samples can be prepared and characterized with standard UHV techniques and rapidly transferred from various preparation chambers to a 4-axis temperature-controlled measurement stage. A synchronized MHz laser system enables excited-state characterization and dynamical studies starting from the picosecond timescale. This article introduces the principal characteristics of the PM4 beamline and LowDosePES end-station. Recent results from graphene, an organic hole transport material for solar cells and the transition metal dichalcogenide MoS2 are presented to demonstrate the instrument performances.

A comparative study on the total reflection X-ray fluorescence determination of lowZelements using X-ray tube and synchrotron radiation as excitation sources

Detailed total reflection X-ray fluorescence (TXRF) studies for the detection and quantification of low atomic number elements were carried out by using a laboratory dual source TXRF spectrometer equipped with a vacuum chamber and at the International Atomic Energy Agency multi-purpose end-station facility, operated at the XRF beamline of Elettra Sincrotrone Trieste, Italy. Multi-elemental standard aqueous solutions of low Z elements (F, Na, Al, S, K, Sc, and Ti) with different elemental concentrations of 2, 10, 20, and 30 µg/ml were prepared and measured in both setups. The measurements at the synchrotron setup were performed in a scanning mode across the sample residue and perpendicular to the incident beam in order to account properly for a possible non-uniform deposition of certain elements. The accuracy and the detection limits obtained from the TXRF measurements in both setups were determined and comparatively evaluated and assessed. Significant improvement in the TXRF detection limits at the synchrotron beamline end-station was obtained for the elements with Z ≤ 13 (Al). Copyright © 2017 John Wiley & Sons, Ltd.

Mobile setup for synchrotron based in situ characterization during thermal and plasma-enhanced atomic layer deposition.

We report the design of a mobile setup for synchrotron based in situ studies during atomic layer processing. The system was designed to facilitate in situ grazing incidence small angle x-ray scattering (GISAXS), x-ray fluorescence (XRF), and x-ray absorption spectroscopy measurements at synchrotron facilities. The setup consists of a compact high vacuum pump-type reactor for atomic layer deposition (ALD). The presence of a remote radio frequency plasma source enables in situ experiments during both thermal as well as plasma-enhanced ALD. The system has been successfully installed at different beam line end stations at the European Synchrotron Radiation Facility and SOLEIL synchrotrons. Examples are discussed of in situ GISAXS and XRF measurements during thermal and plasma-enhanced ALD growth of ruthenium from RuO4 (ToRuS™, Air Liquide) and H2 or H2 plasma, providing insights in the nucleation behavior of these processes.

Pushing the limits of a beamline endstation

Pushing the limits of a beamline endstation

LabVIEW interface with Tango control system for a multi-technique X-ray spectrometry IAEA beamline end-station at Elettra Sincrotrone Trieste

A new synchrotron beamline end-station for multipurpose X-ray spectrometry applications has been recently commissioned and it is currently accessible by end-users at the XRF beamline of Elettra Sincrotrone Trieste. The end-station consists of an ultra-high vacuum chamber that includes as main instrument a seven-axis motorized manipulator for sample and detectors positioning, different kinds of X-ray detectors and optical cameras. The beamline end-station allows performing measurements in different X-ray spectrometry techniques such as Microscopic X-Ray Fluorescence analysis (µXRF), Total Reflection X-Ray Fluorescence analysis (TXRF), Grazing Incidence/Exit X-Ray Fluorescence analysis (GI-XRF/GE-XRF), X-Ray Reflectometry (XRR), and X-Ray Absorption Spectroscopy (XAS). A LabVIEW Graphical User Interface (GUI) bound with Tango control system consisted of many custom made software modules is utilized as a user-friendly tool for control of the entire end-station hardware components. The present work describes this advanced Tango and LabVIEW software platform that utilizes in an optimal synergistic manner the merits and functionality of these well-established programming and equipment control tools.