The New Beamline LISA at ESRF: Performances and Perspectives for Earth and Environmental Sciences

LISA (Linea Italiana per la Spettroscopia di Assorbimento di raggi X) is the new Italian Collaborating Research Group (CRG) beamline at the European Synchrotron Radiation Facility (ESRF) dedicated to X-ray absorption spectroscopy (XAS). The beamline covers a wide energy range, 4 < E < 90 keV, which offers the possibility for probe the K and L edges of elements that are heavier than Ca. A liquid He/N2 cryostat and a compact furnace are available for measurements in a wide temperature range (10–1000 K), allowing for in situ chemical treatments and measurements under a controlled atmosphere. The sub-millimetric beam size, the high photon flux provided, and the X-ray fluorescence detectors available (HP-Ge, SDD) allow for the study of liquid and highly diluted samples. Trace elements in geological or environmental samples can be analyzed, even for very small sample areas, gaining information on oxidation states and host phases.

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XAFS and X-MCD spectroscopies with undulator gap scan

Journal of Synchrotron Radiation ◽

10.1107/s0909049597014702 ◽

1998 ◽

Vol 5 (3) ◽

pp. 989-991 ◽

Cited By ~ 16

Author(s):

Andrei Rogalev ◽

Vincent Gotte ◽

Jose´ Goulon ◽

Christophe Gauthier ◽

Joel Chavanne ◽

...

Keyword(s):

Energy Range ◽

Absorption Spectroscopy ◽

Emission Peak ◽

Photon Statistics ◽

Wide Energy Range ◽

X Ray ◽

Polarization Rate ◽

Spin Polarized ◽

Wide Energy ◽

X Ray Absorption

The first experimental applications of the undulator gap-scan technique in X-ray absorption spectroscopy are reported. The key advantage of this method is that during EXAFS scans the undulator is permanently tuned to the maximum of its emission peak in order to maximize the photon statistics. In X-MCD or spin-polarized EXAFS studies with a helical undulator of the Helios type, the polarization rate can also be kept almost constant over a wide energy range.

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The materials science X-ray beamline BL8 at the DELTA storage ring

Journal of Synchrotron Radiation ◽

10.1107/s0909049509000508 ◽

2009 ◽

Vol 16 (2) ◽

pp. 264-272 ◽

Cited By ~ 28

Author(s):

Dirk Lützenkirchen-Hecht ◽

Ralph Wagner ◽

Ulrich Haake ◽

Anke Watenphul ◽

Ronald Frahm

Keyword(s):

Materials Science ◽

Photon Flux ◽

Acquisition Time ◽

Optical Components ◽

Time Resolved ◽

X Ray ◽

Heavy Loads ◽

Vacuum Systems ◽

X Ray Absorption

The hard X-ray beamline BL8 at the superconducting asymmetric wiggler at the 1.5 GeV Dortmund Electron Accelerator DELTA is described. This beamline is dedicated to X-ray studies in the spectral range from ∼1 keV to ∼25 keV photon energy. The monochromator as well as the other optical components of the beamline are optimized accordingly. The endstation comprises a six-axis diffractometer that is capable of carrying heavy loads related to non-ambient sample environments such as, for example, ultrahigh-vacuum systems, high-pressure cells or liquid-helium cryostats. X-ray absorption spectra from several reference compounds illustrate the performance. Besides transmission measurements, fluorescence detection for dilute sample systems as well as surface-sensitive reflection-mode experiments have been performed. The results show that high-quality EXAFS data can be obtained in the quick-scanning EXAFS mode within a few seconds of acquisition time, enabling time-resolved in situ experiments using standard beamline equipment that is permanently available. The performance of the new beamline, especially in terms of the photon flux and energy resolution, is competitive with other insertion-device beamlines worldwide, and several sophisticated experiments including surface-sensitive EXAFS experiments are feasible.

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Nanoscale determination of interatomic distance by ptychography-EXAFS method using advanced Kirkpatrick–Baez mirror focusing optics

Journal of Synchrotron Radiation ◽

10.1107/s1600577519017004 ◽

2020 ◽

Vol 27 (2) ◽

pp. 455-461

Author(s):

Makoto Hirose ◽

Kei Shimomura ◽

Takaya Higashino ◽

Nozomu Ishiguro ◽

Yukio Takahashi

Keyword(s):

Wide Energy Range ◽

X Rays ◽

Bulk Materials ◽

Interatomic Distances ◽

X Ray ◽

Combination Technique ◽

Wide Energy ◽

Diffraction Patterns ◽

X Ray Absorption

This work demonstrates a combination technique of X-ray ptychography and the extended X-ray absorption fine structure (ptychography-EXAFS) method, which can determine the interatomic distances of bulk materials at the nanoscale. In the high-resolution ptychography-EXAFS method, it is necessary to use high-intense coherent X-rays with a uniform wavefront in a wide energy range, hence a ptychographic measurement system installed with advanced Kirkpatrick–Baez mirror focusing optics is developed and its performance is evaluated. Ptychographic diffraction patterns of micrometre-size MnO particles are collected by using this system at 139 energies between 6.504 keV and 7.114 keV including the Mn K absorption edge, and then the EXAFS of MnO is derived from the reconstructed images. By analyzing the EXAFS spectra obtained from a 48 nm × 48 nm region, the nanoscale bond lengths of the first and second coordination shells of MnO are determined. The present approach has great potential to elucidate the unclarified relationship among the morphology, electronic state and atomic arrangement of inhomogeneous bulk materials with high spatial resolution.

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A new detector for sub-millisecond EXAFS spectroscopy at the European Synchrotron Radiation Facility

Journal of Synchrotron Radiation ◽

10.1107/s1600577514014805 ◽

2014 ◽

Vol 21 (6) ◽

pp. 1240-1246 ◽

Cited By ~ 18

Author(s):

Innokenty Kantor ◽

Jean-Claude Labiche ◽

Emmanuel Collet ◽

Laurent Siron ◽

Jean-Jacques Thevenin ◽

...

Keyword(s):

European Synchrotron Radiation Facility ◽

Low Noise ◽

Frame Rate ◽

Full Time ◽

Time Resolved ◽

Temperature Oxidation ◽

X Ray ◽

X Ray Absorption ◽

Exafs Spectra

A new FReLoN (Fast-Readout Low-Noise) high-frame-rate detector adopted for the fast continuous collection of X-ray absorption spectra is presented. The detector is installed on the energy-dispersive X-ray absorption beamline ID24 at the ESRF and is capable of full time-resolved EXAFS spectra collection with over 4 kHz repetition rate and 0.2 ms exposure time. An example of thein situkinetic study of the high-temperature oxidation of metallic iron is presented.

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The TES beamline (8-BM) at NSLS-II: tender-energy spatially resolved X-ray absorption spectroscopy and X-ray fluorescence imaging

Journal of Synchrotron Radiation ◽

10.1107/s1600577519012761 ◽

2019 ◽

Vol 26 (6) ◽

pp. 2064-2074 ◽

Cited By ~ 7

Author(s):

Paul Northrup

Keyword(s):

Energy Range ◽

Fluorescence Imaging ◽

Absorption Spectroscopy ◽

Small Sample ◽

Energy Calibration ◽

Helium Atmosphere ◽

X Ray ◽

Spatially Resolved ◽

X Ray Absorption

The tender-energy X-ray spectroscopy (TES) beamline at the National Synchrotron Light Source II (NSLS-II) is now operational for general users. Its scientific mission includes static and in situ X-ray fluorescence imaging and spatially resolved X-ray absorption spectroscopy for characterization of complex heterogeneous, structured and dynamic natural or engineered materials and systems. TES is optimized for the tender-energy range, offering routine operations from 2.0 to 5.5 keV, with capabilities to reach down to 1.2 or up to 8 keV with configuration change. TES is designed as an extended X-ray absorption fine-structure microprobe (EXAFS microprobe) for applications of micrometre-scale EXAFS spectroscopy to heterogeneous samples. Beam size is user-tunable from ∼2 to 25 µm. Energy may be scanned on-the-fly or in traditional step scanning. Importantly, the position of the microbeam at the sample location does not move significantly during energy scanning or when changing energy across the entire routine energy range. This enables full EXAFS of a particle or domain the same size as the probe beam, and measurement of the same spot at different energies. In addition, there is no measureable drift in energy calibration (repeatability) scan-to-scan and over 24 h. This is critical where simultaneous calibration measurements are generally not feasible, and for speciation mapping where precise and stable control of incident energy is essential. The sample environment is helium atmosphere at room pressure with infrastructure for in situ electrochemistry and catalysis in small sample cells or microreactors. As the first bend-magnet beamline at NSLS-II, noteworthy commissioning aspects are described. Example measurements are presented to illustrate its capabilities.

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A middle energy-bandwidth X-ray monochromator for high-flux synchrotron diffraction: revisiting asymmetrically cut silicon crystals

Journal of Synchrotron Radiation ◽

10.1107/s1600577519003473 ◽

2019 ◽

Vol 26 (3) ◽

pp. 750-755 ◽

Cited By ~ 6

Author(s):

Hiroo Tajiri ◽

Hiroshi Yamazaki ◽

Haruhiko Ohashi ◽

Shunji Goto ◽

Osami Sakata ◽

...

Keyword(s):

Atomic Plane ◽

Photon Flux ◽

Wide Energy Range ◽

Double Crystal ◽

X Ray ◽

Silicon Crystals ◽

Double Crystal Monochromator ◽

Diffraction Geometry ◽

Wide Energy ◽

Surface Diffraction

To supply the growing demand for high photon flux in synchrotron science including surface diffraction, a middle energy-bandwidth monochromator covering the 10−4 to 10−3 range has been adapted by applying an asymmetric diffraction geometry to a cryogenically cooled silicon 111 double-crystal monochromator used as a standard for the undulator source at SPring-8. The asymmetric geometry provides a great advantage with its ability to configure flux gains over a wide energy range by simply changing the asymmetry angle, while the angular divergence of the exit beam remains unchanged. A monolithic design with three faces has been employed, having one symmetrically cut and another two asymmetrically cut surfaces relative to the same atomic plane, maintaining cooling efficiency and the capability of quickly changing the reflection surface. With the asymmetric geometry, an X-ray flux greater than 1014 photons s−1 was available around 12 keV. A maximum gain of 2.5 was obtained relative to the standard symmetric condition.

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Absolute X-ray energy measurement using a high-accuracy angle encoder

Journal of Synchrotron Radiation ◽

10.1107/s1600577520014526 ◽

2021 ◽

Vol 28 (1) ◽

pp. 111-119

Author(s):

Takahiko Masuda ◽

Tsukasa Watanabe ◽

Kjeld Beeks ◽

Hiroyuki Fujimoto ◽

Takahiro Hiraki ◽

...

Keyword(s):

Photon Energy ◽

Wide Energy Range ◽

Energy Measurement ◽

X Ray ◽

Order Of Magnitude ◽

Single Crystal Plate ◽

Wide Energy ◽

Angle Encoder ◽

Potassium 40

This paper presents an absolute X-ray photon energy measurement method that uses a Bond diffractometer. The proposed system enables the prompt and rapid in situ measurement of photon energies over a wide energy range. The diffractometer uses a reference silicon single-crystal plate and a highly accurate angle encoder called SelfA. The performance of the system is evaluated by repeatedly measuring the energy of the first excited state of the potassium-40 nuclide. The excitation energy is determined as 29829.39 (6) eV, and this is one order of magnitude more accurate than the previous measurement. The estimated uncertainty of the photon energy measurement was 0.7 p.p.m. as a standard deviation and the maximum observed deviation was 2 p.p.m.

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Photon interference effect in x-ray absorption spectra over a wide energy range

Physical Review B ◽

10.1103/physrevb.66.113103 ◽

2002 ◽

Vol 66 (11) ◽

Cited By ~ 2

Author(s):

Y. Nishino ◽

T. Ishikawa ◽

M. Suzuki ◽

N. Kawamura ◽

P. Kappen ◽

...

Keyword(s):

Energy Range ◽

Absorption Spectra ◽

Interference Effect ◽

Wide Energy Range ◽

X Ray ◽

Wide Energy ◽

X Ray Absorption

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Energy-Resolving X-ray Fluorescence Detection Using Synthetic Multilayers

Journal of Synchrotron Radiation ◽

10.1107/s0909049597019535 ◽

1998 ◽

Vol 5 (4) ◽

pp. 1227-1234 ◽

Cited By ~ 7

Author(s):

K. Zhang ◽

G. Rosenbaum ◽

G. Bunker

Keyword(s):

Fluorescence Detection ◽

Detection System ◽

Array Detector ◽

Wide Energy Range ◽

Ionization Chambers ◽

X Ray ◽

Detection Systems ◽

Wide Energy ◽

Fluorescence Detection System ◽

X Ray Absorption

The potential of synthetic multilayers for energy-resolving the X-ray fluorescence in X-ray absorption fine structure (XAFS) experiments is discussed. Two detection systems, one using curved multilayers and the other using graded multilayers to select X-ray fluorescence photons, have been designed to cover a wide energy range with a usefully large solid angle. Such a detector will be more advantageous than the barrel-like crystal-array detector because of the unique properties of synthetic multilayers, such as larger horizontal acceptance angles and bandwidth. In addition, the detector should be much simpler to construct and readily accommodates energy changes, especially the detector using graded multilayers. Comparison of the multilayer array detector with conventional detectors, such as ionization chambers and conventional 13-element Ge detectors, shows that the proposed system will be superior, particularly with the increased photon fluxes available from insertion devices and with decreased sample concentration, since this detection system eliminates the `bad' photons before they enter any X-ray detector. Consequently, the X-ray detector proper for this system does not suffer from the incident-count-rate bottleneck common to current X-ray fluorescence detectors with energy resolution by signal processing. Thus, this new fluorescence detection system will provide tremendous opportunities for XAFS measurements on dilute systems, such as biological systems, at third-generation synchrotron sources.

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