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Register a new userTEXS: in-vacuum tender X-ray emission spectrometer with 11 Johansson crystal analyzers
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We describe the design and show first results of a large solid angle X-ray emission spectrometer that is optimized for energies between 1.5 keV and 5.5 keV. The spectrometer is based on an array of 11 cylindrically bent Johansson crystal analyzers arranged in a non-dispersive Rowland circle geometry. The smallest achievable energy bandwidth is smaller than the core hole lifetime broadening of the absorption edges in this energy range. Energy scanning is achieved using an innovative design, maintaining the Rowland circle conditions for all crystals with only four motor motions. The entire spectrometer is encased in a high-vacuum chamber that allocates a liquid helium cryostat and provides sufficient space for in situ cells and operando catalysis reactors.
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We demonstrate that vacuum forming of 10-cm diameter silicon wafers of various crystallographic orientations under an x-ray permeable, flexible window can easily generate spherically bent crystal analyzers (SBCA) and toroidally bent crystal analyzers (TBCA) with ~1-eV energy resolution and a 1-m major radius of curvature. In applications at synchrotron light sources, x-ray free electron lasers, and laboratory spectrometers these characteristics are generally sufficient for many x-ray absorption fine structure (XAFS), x-ray emission spectroscopy (XES), and resonant inelastic x-ray scattering (RIXS) applications in the chemical sciences. Unlike existing optics manufacturing methods using epoxy or anodic bonding, vacuum forming without adhesive is temporary in the sense that the bent wafer can be removed when vacuum is released and exchanged for a different orientation wafer. Therefore, the combination of an x-ray compatible vacuum-forming chamber, a library of thin wafers, and a small number of forms having different secondary curvatures can give extreme flexibility in spectrometer energy range. As proof of this method we determine the energy resolution and reflectivity for several such vacuum-formed bent crystal analyzers (VF-BCA) in laboratory based XAFS and XES studies using a conventional x-ray tube. For completeness we also show x-ray images collected on the detector plane to characterize the resulting focal spots and optical aberrations.
A vacuum-compatible photon-counting hybrid pixel detector has been installed in the ultra-high vacuum (UHV) reflectometer of the four-crystal monochromator (FCM) beamline of the Physikalisch-Technische Bundesanstalt (PTB) at the electron storage ring BESSY II in Berlin, Germany. The setup is based on the PILATUS3 100K module. The detector can be used in the entire photon energy range accessible at the beamline from 1.75 to 10 keV. Complementing the already installed vacuum-compatible PILATUS 1M detector used for small-angle scattering (SAXS) and grazing incidence SAXS (GISAXS), it is possible to access larger scattering angles. The water-cooled module is located on the goniometer arm and can be positioned from -90{deg} to 90{deg} with respect to the incoming beam at a distance of about 200 mm from the sample. To perform absolute scattering experiments the linearity, homogeneity and the angular dependence of the quantum efficiency, including their relative uncertainties, have been investigated. In addition, first results of the performance in wide-angle X-ray scattering (WAXS), X-ray diffraction (XRD) and X-ray reflectometry (XRR) are presented.
We present the development, manufacturing and performance of spherically bent crystal analyzers (SBCAs) of 100 mm diameter and 0.5 m bending radius. The elastic strain in the crystal wafer is partially released by a strip-bent method where the crystal wafer is cut in strips prior to the bending and the anodic bonding process. Compared to standard 1 m SBCAs, a gain in intensity is obtained without loss of energy resolution. The gain ranges between 2.5 and 4.5, depending on the experimental conditions and the width of the emission line measured. This reduces the acquisition times required to perform high energy-resolution x-ray absorption and emission spectroscopy on ultra-dilute species, accessing concentrations of the element of interest down to, or below, the ppm (ng/mg) level.
The resolution function of a spectrometer based on a strongly bent single crystal (bending radius of 10 cm or less) is evaluated. It is shown that the resolution is controlled by two parameters, (i) the ratio of the lattice spacing of the chosen reflection to the crystal thickness and (ii) a single parameter comprising crystal thickness, its bending radius, and anisotropic elastic constants of the chosen crystal. Diamond, due to its unique elastic properties, can provide notably higher resolution than silicon. The results allow to optimize the parameters of bent crystal spectrometers for the hard X-ray free electron laser sources.
X-ray emission spectroscopy is emerging as an important complement to x-ray absorption fine structure spectroscopy, providing a characterization of the occupied electronic density of states local to the species of interest. Here, we present details of the design and performance of a compact x-ray emission spectrometer that uses a dispersive refocusing Rowland (DRR) circle geometry to achieve excellent performance for the 2 - 2.5 keV energy range. The DRR approach allows high energy resolution even for unfocused x-ray sources. This property enables high count rates in laboratory studies, comparable to those of insertion-device beamlines at third-generation synchrotrons, despite use of only a low-powered, conventional x-ray tube. The spectrometer, whose overall scale is set by use of a 10-cm diameter Rowland circle and a new small-pixel CMOS x-ray camera, is easily portable to synchrotron or x-ray free electron beamlines. Photometrics from measurements at the Advanced Light Source show somewhat higher overall instrumental efficiency than prior systems based on less tightly curved analyzer optics. In addition, the compact size of this instrument lends itself to future multiplexing to gain large factors in net collection efficiency, or its implementation in controlled gas gloveboxes either in the lab or in an endstation.
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