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. 2019 May 1;26(Pt 3):629-634.
doi: 10.1107/S1600577519002431. Epub 2019 Apr 2.

A high-throughput energy-dispersive tender X-ray spectrometer for shot-to-shot sulfur measurements

Baxter Abraham  1 , Stanislaw Nowak  2 , Clemens Weninger  1 , Rebecca Armenta  1 , Jim Defever  1 , David Day  2 , Gabriella Carini  3 , Kazutaka Nakahara  1 , Alessandro Gallo  4 , Silke Nelson  1 , Dennis Nordlund  2 , Thomas Kroll  2 , Mark S Hunter  1 , Tim van Driel  1 , Diling Zhu  1 , Tsu Chien Weng  2 , Roberto Alonso-Mori  1 , Dimosthenis Sokaras  2
Affiliations

A high-throughput energy-dispersive tender X-ray spectrometer for shot-to-shot sulfur measurements

Baxter Abraham et al. J Synchrotron Radiat. .

Abstract

An X-ray emission spectrometer that can detect the sulfur Kα emission lines with large throughput and a high energy resolution is presented. The instrument is based on a large d-spacing perfect Bragg analyzer that diffracts the sulfur Kα emission at close to backscattering angles. This facilitates the application of efficient concepts routinely employed in hard X-ray spectrometers towards the tender X-ray regime. The instrument described in this work is based on an energy-dispersive von Hamos geometry that is well suited for photon-in photon-out spectroscopy at X-ray free-electron laser and synchrotron sources. Comparison of its performance with previously used instrumentation is presented through measurements using sulfur-containing species performed at the LCLS. It is shown that the overall signal intensity is increased by a factor of ∼15. Implementation of this approach in the design of a tender X-ray spectroscopy endstation for LCLS-II is also discussed.

Keywords: X-ray absorption spectroscopy; X-ray emission spectroscopy; X-ray free-electron lasers; photon-in photon-out spectroscopy methods; tender X-rays.

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Figures

Figure 1
Figure 1
LiNbO3 formula image) von Hamos and Si(111) Johansson spectrometers acquired experimental data simultaneously. The dual instrument experimental scheme is depicted. X-ray emission induced by LCLS pulses incident on the flowing sample is collected by both crystal analyzers and recorded shot-to-shot by position-sensitive detectors. The off-Rowland circle sample leads to dispersion in the Johansson geometry, whereas the von Hamos dispersion provides focusing of spectra to a line.
Figure 2
Figure 2
Comparison of the sulfur Kα XES from (NH4)2SO4 using different detection schemes. The intensity of the signal measured by the lithium niobate von Hamos analyzer is ∼15 times greater than by the silicon-based Johansson analyzer.
Figure 3
Figure 3
(a) Comparison of the measured sulfur Kα spectrum using the lithium niobate von Hamos analyzer with spectra calculated by convolution of the natural Lorentzian lineshapes with Gaussian functions of varying widths to simulate the instrument response function. Best fit is obtained from a width of 0.29 eV. (b) Derivatives of the measured and best-fit simulated spectra show good agreement between their line shapes.
Figure 4
Figure 4
Normalized sulfur Kα spectra of ammonium sulfate, CdS quantum dots and thiophene measured using the new spectrometer. The Kα1 and Kα2 peaks are fully resolved and are observed to shift in energy with the oxidation state of the resident sulfur atoms.
See this image and copyright information in PMC

References

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