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. 2024 May 1;31(Pt 3):469-477.
doi: 10.1107/S1600577524001218. Epub 2024 Mar 22.

Development of the multiplex imaging chamber at PAL-XFEL

Junha Hwang  1 , Sejin Kim  2 , Sung Yun Lee  2 , Eunyoung Park  2 , Jaeyong Shin  2 , Jae Hyuk Lee  3 , Myong Jin Kim  3 , Seonghan Kim  3 , Sang Youn Park  3 , Dogeun Jang  3 , Intae Eom  1 , Sangsoo Kim  3 , Changyong Song  2 , Kyung Sook Kim  1 , Daewoong Nam  1
Affiliations

Development of the multiplex imaging chamber at PAL-XFEL

Junha Hwang et al. J Synchrotron Radiat. .

Abstract

Various X-ray techniques are employed to investigate specimens in diverse fields. Generally, scattering and absorption/emission processes occur due to the interaction of X-rays with matter. The output signals from these processes contain structural information and the electronic structure of specimens, respectively. The combination of complementary X-ray techniques improves the understanding of complex systems holistically. In this context, we introduce a multiplex imaging instrument that can collect small-/wide-angle X-ray diffraction and X-ray emission spectra simultaneously to investigate morphological information with nanoscale resolution, crystal arrangement at the atomic scale and the electronic structure of specimens.

Keywords: X-ray emission spectroscopy; XFELs; coherent diffraction imaging; ultrafast dynamics; wide-angle X-ray diffraction.

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Figures

Figure 1
Figure 1
Schematic of the multiplex imaging experiment. It enables collection of small-/wide-angle X-ray diffraction and X-ray emission spectra simultaneously to investigate morphological information with nanoscale resolution, crystal arrangement at the atomic scale and the electronic structure of specimens.
Figure 2
Figure 2
Bird’s eye-view of the multiplex imaging chamber including three JUNGFRAUs. Two detectors, JUNGFRAU 5M and JUNGFRAU 4M, are installed to collect X-ray diffraction signals. (Inset) Internal view of the multiplex imaging chamber. Two slit stages, a sample viewer stage and a sample stage are located for X-ray diffraction experiments. An in-vacuum JUNGFRAU 0.5M and a crystal stage are installed to collect X-ray emission spectra from specimens.
Figure 3
Figure 3
(a) Photograph of the JUNGFRAU 5M. Ten modular sensors are designed to collect wide-angle X-ray diffraction, and the diffracted X-rays at small angles pass through a central hole. (b) Single-shot diffraction pattern of LaB6 powder. The blue- and red-dotted lines indicate the minimum and the maximum 2θ angle covering the whole azimuthal direction, respectively. A central hole with a 20 mm diameter and dummy areas are indicated in white. (c) Intensity plot of the diffraction ring shown in (b). Debye–Scherrer rings can be measured in the range 6 nm−1 to 17.5 nm−1. Notably, whole signals of Debye–Scherrer rings spanning from 12.5 nm−1 to 17 nm−1 can be collected along the azimuthal.
Figure 4
Figure 4
(a) Top view of the spectrometer installed in the multiplex imaging chamber. Three components of the von Hamos spectrometer are indicated by arrows: (1) sample stage, (2) an Si crystal analyzer with a radius of curvature of 250 mm mounted on the stacked stages, (3) JUNGFRAU 0.5M. It is located next to the sample stage. The distance between the crystal plane and the detector plane is determined by the radius of curvature of the crystal analyzer. (b) Energy range measured by the spectrometer with Si(111) and Si(220) crystal analyzers. Because of the finite volume of the multiplex imaging chamber, the measurable energy range is restricted.
Figure 5
Figure 5
Kα1 and Kα2 emission lines of the Ge single crystal. Two peaks are clearly measured by the accumulation of 100 X-ray pulses.
Figure 6
Figure 6
Simultaneous measurements of small-angle X-ray diffraction, wide-angle X-ray diffraction and X-ray emission spectra of Au NPs. (a) Small-angle diffraction pattern of a single Au NP. (b) Au (111) and (200) Bragg peaks from the same particle measured in (a). (c) Intensity profiles of two peaks displayed by averaging the diffraction ring azimuthally. They were normalized with the maximum intensity. (d) Accumulated Lα1 (9.713 keV) and Lα2 (9.628 keV) emission lines of the Au NPs acquired using a von Hamos spectrometer. (e) Intensity profiles of two emission lines. More than 1000 X-ray pulses were accumulated to improve the SNR of the emission lines.
Figure 7
Figure 7
Static and time-resolved measurement of wide-angle X-ray diffraction and X-ray emission spectra of anatase TiO2 NPs. (a) Wide-angle diffraction intensity profile of the TiO2 (101) peak. (b) X-ray emission spectra of Ti Kα1 (4.510 keV) and Kα2 (4.504 keV). (c) Time-resolved X-ray diffraction of TiO2 NPs. At 40 ps, significant (101) peak broadening corresponding to a 70% increase in FWHM is presented. It implies melting of the crystalline domain after laser irradiation. (d) Time-resolved X-ray emission spectrum of TiO2 NPs. At 10 ps, the maximum energy shift, −0.6 eV, was observed. Compared with diffraction signals, the changes in the emission spectra were inappreciable after a 40 ps delay.
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