• Issue

    Journal of Synchrotron Radiation: Volume 29, Issue 2

    281-594
    March 2022

research papers

Open Access

SAXS study of the formation and structure of polynuclear thorium(IV) colloids and thorium dioxide nanoparticles

  • Pages: 281-287
  • First Published: 18 January 2022
SAXS study of the formation and structure of polynuclear thorium(IV) colloids and thorium dioxide nanoparticles

The study provides insight into the formation of thorium dioxide nanoparticles in solution using small-angle X-ray scattering.

Open Access

Effective coordination numbers from EXAFS: general approaches for lanthanide and actinide dioxides

  • Pages: 288-294
  • First Published: 27 January 2022
Effective coordination numbers from EXAFS: general approaches for lanthanide and actinide dioxides

New experimental EXAFS results for PuO2 and CeO2 nanoparticles in the size range of 2 nm were compared with published data for other lanthanide and actinide dioxides. A conceptual core-shell model with a calculated effective coordination number is proposed to fit the changes in EXAFS.

Open Access

X-ray spectroscopic study of chemical state in uranium carbides

  • Pages: 295-302
  • First Published: 27 January 2022
X-ray spectroscopic study of chemical state in uranium carbides

UC and UMeC2 (Me = Fe, Zr, Mo) carbides were studied by the high-energy-resolution fluorescence detected X-ray absorption technique at the U M4 and L3 edges. The data were analyzed using the Anderson impurity model.

Open Access

From EXAFS of reference compounds to U(VI) speciation in contaminated environments

  • Pages: 303-314
  • First Published: 08 February 2022
From EXAFS of reference compounds to U(VI) speciation in contaminated environments

Multiple EXAFS LIII-edge spectra of U(VI) model compounds were recorded at the STM beamline of KISI-Kurchatov (Moscow, Russia). The distinct parameters obtained for the U(VI) local structure were used to analyze the sample of radioactively contaminated soil.

Open Access

In situ beam reduction of Pu(IV) and Bk(IV) as a route to trivalent transuranic coordination complexes with hydroxypyridinone chelators

  • Pages: 315-322
  • First Published: 25 February 2022
In situ beam reduction of Pu(IV) and Bk(IV) as a route to trivalent transuranic coordination complexes with hydroxypyridinone chelators

X-ray absorption spectroscopy was used to probe the interactions between an octadentate hydroxypyridinone chelator and two transuranic elements in microgram quantities – plutonium and berkelium – within buffered solutions. Despite the precedence for chelation-driven stabilization of the tetravalent oxidation state of actinides with this ligand, in situ reductive decomposition yielded plutonium(III) and berkelium(III) coordination complexes.

Open Access

Quantifying electron cascade size in various irradiated materials for free-electron laser applications

  • Pages: 323-330
  • First Published: 15 February 2022
Quantifying electron cascade size in various irradiated materials for free-electron laser applications

Studying electron- and X-ray-induced electron cascades in solids is essential for various research areas at free-electron laser facilities, such as X-ray imaging, crystallography, pulse diagnostics or X-ray-induced damage. To better understand the fundamental factors that define the duration and spatial size of such cascades, this work investigates the electron propagation in ten solids relevant for the applications of X-ray lasers. Using classical Monte Carlo simulation in the atomic approximation, the dependence of the cascade size on the incident electron or photon energy and on the target parameters is studied.

Open Access

3D printed devices and infrastructure for liquid sample delivery at the European XFEL

  • Pages: 331-346
  • First Published: 15 February 2022
3D printed devices and infrastructure for liquid sample delivery at the European XFEL

Presented here are 3D printed sample delivery devices for precise control over fluids and the generation of micrometre-sized gas-focused liquid jets, high-viscosity streams and near-monodisperse droplets suitable for X-ray scattering experiments on X-ray free-electron laser (XFEL) instruments.

Open Access

Generating coherent and ultrashort X-ray pulses via HHG-seeding in storage rings

  • Pages: 347-354
  • First Published: 19 January 2022
Generating coherent and ultrashort X-ray pulses via HHG-seeding in storage rings

A method that utilizes the recent external light from high-harmonic generation (HHG) to coherent light at shorter wavelength is proposed. Numerical simulations with parameters of a diffraction-limited storage ring demonstrate the generation of coherent pulse trains with photon energy as high as 2 keV, pulse duration as short as ∼10 fs and high peak brightness directly from an HHG source at 13 nm.

Open Access

Synchrotron radiation transmission by two coupled flat microchannel plates: new opportunities to control the focal spot characteristics

  • Pages: 355-362
  • First Published: 19 January 2022
Synchrotron radiation transmission by two coupled flat microchannel plates: new opportunities to control the focal spot characteristics

Transmission properties and diffraction patterns generated by synchrotron radiation at the exit of an assembled couple of microchannel plates (MCPs) are inivestigated. A theoretical model to simulate the patterns and properties of the soft X-ray beam emerging from this couple of MCPs is presented and discussed.

Open Access

Vacuum joints of CuCrZr alloy for high-heat-load photon absorber

  • Pages: 363-368
  • First Published: 08 February 2022
Vacuum joints of CuCrZr alloy for high-heat-load photon absorber

A novel welded photon absorber with a total length of 600 mm has been successfully designed and manufactured, and will be applicable in the highest-heat-load front-end in the Shanghai Synchrotron Radiation Facility Phase-II beamline project.

Open Access

Using diffraction losses of X-rays in a single crystal for determination of its lattice parameters as well as for monochromator calibration

  • Pages: 369-376
  • First Published: 08 February 2022
Using diffraction losses of X-rays in a single crystal for determination of its lattice parameters as well as for monochromator calibration

Diffraction losses (glitches) at certain energies of the X-ray beam, transmitted through a single crystal, can be used for lattice parameters determination as well as for calibrating the monochromator (absolute pitch angle and the unit-cell parameter).

Open Access

Cryo-cooled silicon crystal monochromators: a study of power load, temperature and deformation

  • Pages: 377-385
  • First Published: 08 February 2022
Cryo-cooled silicon crystal monochromators: a study of power load, temperature and deformation

The heat-load effects on cryo-cooled Si crystals in synchrotron beamlines are investigated.

Open Access

Trapezoid-kinoform zone plate lens – a solution for efficient focusing in hard X-ray optics

  • Pages: 386-392
  • First Published: 15 February 2022
Trapezoid-kinoform zone plate lens – a solution for efficient focusing in hard X-ray optics

A new theoretical approach for computing the focusing performance of X-ray optics with circularly symmetry shape was developed. Greyscale electron beam lithography was applied to generate 3D kinoform zones in Au for hard X-rays for the first time. The novel trapezoid kinoform zone plate lens demonstrates significantly high diffraction efficiency well beyond that of conventional X-ray optics.

Open Access

Fast automated energy changes at synchrotron radiation beamlines equipped with transfocator or focusing mirrors

  • Pages: 393-399
  • First Published: 15 February 2022
Fast automated energy changes at synchrotron radiation beamlines equipped with transfocator or focusing mirrors

Procedures for fully automated X-ray energy changes at undulator-based synchrotron radiation beamlines with Kirkpatrick–Baez focusing mirrors or a long transfocator consisting of compound refractive lenses are presented. The procedures maintain beam intensity after the monochromator, beam position at the sample, beam attenuation, and the beam focusing distance.

Open Access

Beamline commissioning for microscopic measurements with ultraviolet and soft X-ray beam at the upgraded beamline BL-13B of the Photon Factory

  • Pages: 400-408
  • First Published: 16 February 2022
Beamline commissioning for microscopic measurements with ultraviolet and soft X-ray beam at the upgraded beamline BL-13B of the Photon Factory

Beamline BL-13B of the Photon Factory and the end-station have been upgraded, enabling microscopic XPS, XAS, and ARPES measurements with a spatial resolution that is comparable with the size of the focused beam. Beam profile evaluation and experimental demonstration of microscopic measurements are presented.

Open Access

Extreme conditions research using the large-volume press at the P61B endstation, PETRA III

  • Pages: 409-423
  • First Published: 22 February 2022
Extreme conditions research using the large-volume press at the P61B endstation, PETRA III

The operation of the P61B endstation large-volume press and optics of P61 are reviewed. The instrumentation at P61B, including the large-volume press, detection systems and data acquisition for in situ high-pressure experiments are described.

Open Access

A polycrystalline diamond micro-detector for X-ray absorption fine-structure measurements

  • Pages: 424-430
  • First Published: 16 February 2022
A polycrystalline diamond micro-detector for X-ray absorption fine-structure measurements

A polycrystalline diamond detector for XAFS measurement has been fabricated. Its volume is 2947 times smaller than a routine ion-chamber.

Open Access

A cell design for correlative hard X-ray nanoprobe and electron microscopy studies of catalysts under in situ conditions

  • Pages: 431-438
  • First Published: 15 February 2022
A cell design for correlative hard X-ray nanoprobe and electron microscopy studies of catalysts under in situ conditions

The development of an in situ gas/heating cell for X-ray nanoprobe studies is presented. The capabilities are demonstrated by an investigation of the redox behaviour of supported Pt nanoparticles on ceria.

Open Access

Implementation of wedged-serial protein crystallography at PROXIMA-1

  • Pages: 439-446
  • First Published: 17 January 2022
Implementation of wedged-serial protein crystallography at PROXIMA-1

The implementation of microfluidic-based wedged-serial protein crystallography at PROXIMA-1 opens new possibilities for in situ data collection experiments with low sample consumption.

Open Access

Diffuse X-ray scattering from polished silicon: application of the distorted wave Born approximation

  • Pages: 447-455
  • First Published: 08 February 2022
Diffuse X-ray scattering from polished silicon: application of the distorted wave Born approximation

Measurements of diffuse X-ray scattering from polished silicon were fit. The fits employed autocorrelation functions obtained from direct metrology of the surface roughness.

Open Access

Visualizing the valence states of europium ions in Eu-doped BaAl2O4 using X-ray nanoprobe mapping

  • Pages: 456-461
  • First Published: 18 January 2022
Visualizing the valence states of europium ions in Eu-doped BaAl2O4 using X-ray nanoprobe mapping

It is anticipated that X-ray nanoprobes will open new avenues with significant characterization ability for unravelling the emission mechanisms of phosphor materials.

Open Access

Wiggler radiation at a low-emittance storage ring and its usage for X-ray absorption spectroscopy

  • Pages: 462-469
  • First Published: 18 January 2022
Wiggler radiation at a low-emittance storage ring and its usage for X-ray absorption spectroscopy

Experimental and computational studies of wigglers on low-emittance storage rings are reported. EXAFS spectra for possible distortions originating from the source imperfection are also examined. It is concluded that wigglers are still an appropriate class of insertion devices, also on low-emittance synchrotrons.

Open Access

A new route to obtain fluorescence X-ray absorption spectra of compounds and to remove the self-absorption induced nonlinearity in the spectra

  • Pages: 470-479
  • First Published: 08 February 2022
A new route to obtain fluorescence X-ray absorption spectra of compounds and to remove the self-absorption induced nonlinearity in the spectra

This work describes an experimental method in tackling the self-absorption effect encountered in fluorescence X-ray absorption spectroscopy and its application to surface and subsurface.

Open Access

High-speed free-run ptychography at the Australian Synchrotron

  • Pages: 480-487
  • First Published: 17 January 2022
High-speed free-run ptychography at the Australian Synchrotron

The implementation of high-speed ptychography on the Australian Synchrotron XFM beamline in presented. It includes a free-run data collection mode where dead time is eliminated and scan time is optimized. This data collection mode is compatible with fast-scanning X-ray fluorescence mapping with extremely high data acquisition rates over large areas, demonstrated at up to 140 µm2 s−1 with 13× spatial resolution enhancement compared with the beam size.

Open Access

Fast and noise-tolerant determination of the center of rotation in tomography

  • Pages: 488-495
  • First Published: 19 January 2022
Fast and noise-tolerant determination of the center of rotation in tomography

A rapid phase symmetry method for finding the center of rotation in tomographic data using two images located 180° ± Δgθ apart is introduced. The method is more robust against photon noise than image correlation methods, and shows good tolerance to Δgθ ranging up to several degrees.

Open Access

Synchrotron radiation analysis of root dentin: the roles of fluoride and calcium ions in hydroxyapatite remineralization

  • Pages: 496-504
  • First Published: 19 January 2022
Synchrotron radiation analysis of root dentin: the roles of fluoride and calcium ions in hydroxyapatite remineralization

Early root carious lesions require an optimal amount of both free fluoride and calcium ions in the oral environment to initiate a hydroxyapatite remineralization on root dentin. This study elucidates the role of fluoride and calcium to maintain the abundance of hydroxyapatite on acid-challenged root dentin with a novel approach – using synchrotron radiation.

Open Access

A wide-field micro-computed tomography detector: micron resolution at half-centimetre scale

  • Pages: 505-514
  • First Published: 19 January 2022
A wide-field micro-computed tomography detector: micron resolution at half-centimetre scale

A custom wide-field lens and a new-generation megapixel camera enabled micro-CT scanning over a 3.5 mm × 5 mm field of view at 1 µm resolution/0.5 µm pixel size at Lawrence Berkeley Laboratory's Advanced Light Source and Argonne National Laboratory's Advanced Photon Source using a phantom with micron-scale features. This novel combination of resolution and field of view was designed for broad applicability to any setting in which micron-scale structures need to be characterized comprehensively in three dimensions over mm to cm.

Open Access

Environmental cell for in situ X-ray synchrotron micro-CT imaging with simultaneous acoustic measurements

  • Pages: 515-521
  • First Published: 27 January 2022
Environmental cell for in situ X-ray synchrotron micro-CT imaging with simultaneous acoustic measurements

A new environmental cell for simultaneous in situ dynamic X-ray imaging and measuring acoustic properties of geological samples is presented. The cell helps studying physical/chemical processes in geomaterials and their influence on the mechanical properties.

Open Access

In situ tomographic study of a 3D-woven SiC/SiC composite part subjected to severe thermo-mechanical loads

  • Pages: 522-531
  • First Published: 27 January 2022
In situ tomographic study of a 3D-woven SiC/SiC composite part subjected to severe thermo-mechanical loads

An in situ corner bending test under a high thermal gradient is followed by both computed tomography and thermography. Experimental procedure, image processing and preliminary conclusion are presented.

beamlines

Open Access

Operational status of the X-ray powder diffraction beamline at the SESAME synchrotron

  • Pages: 532-539
  • First Published: 17 January 2022
Operational status of the X-ray powder diffraction beamline at the SESAME synchrotron

The Materials Science (MS) beamline at SESAME, dedicated to the X-ray powder diffraction technique, started its operational phase in December 2020. A detailed description of the beamline components and the experimental characterization of the main instrumental parameters are presented.

Open Access

Scanning structural mapping at the Life Science X-ray Scattering Beamline

  • Pages: 540-548
  • First Published: 17 January 2022
Scanning structural mapping at the Life Science X-ray Scattering Beamline

Instrumentation and software for supporting microbeam structural mapping at the LiX beamline are presented.

Open Access

Fully automated measurement system for temperature-dependent X-ray total scattering at beamline BL04B2 at SPring-8

  • Pages: 549-554
  • First Published: 18 January 2022
Fully automated measurement system for temperature-dependent X-ray total scattering at beamline BL04B2 at SPring-8

The implementation of a new, fully automated X-ray total scattering system on beamline BL04B2 at SPring-8 is described.

Open Access

A setup for millisecond time-resolved X-ray solution scattering experiments at the CoSAXS beamline at the MAX IV Laboratory

  • Pages: 555-562
  • First Published: 16 February 2022
A setup for millisecond time-resolved X-ray solution scattering experiments at the CoSAXS beamline at the MAX IV Laboratory

A new experimental setup for millisecond time-resolved X-ray solution scattering has been developed and commissioned at the CoSAXS beamline at the MAX IV synchrotron. Results from T-jump experiments induced by infrared laser pulses in lysozyme in solution are presented for validation.

Open Access

I21: an advanced high-resolution resonant inelastic X-ray scattering beamline at Diamond Light Source

  • Pages: 563-580
  • First Published: 22 February 2022
I21: an advanced high-resolution resonant inelastic X-ray scattering beamline at Diamond Light Source

The design of the resonant inelastic X-ray scattering beamline at Diamond Light Source, I21, is presented. X-ray commissioning results are shown and compared with the optical simulations.

obituaries

Open Access

Kenneth C. Holmes (1934–2021)

  • Pages: 591-592
  • First Published: 25 February 2022
Kenneth C. Holmes (1934–2021)

Obituary for Kenneth C. Holmes