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. 2024 Jul 1;31(Pt 4):968-978.
doi: 10.1107/S1600577524004764. Epub 2024 Jun 25.

GIWAXS experimental methods at the NFPS-BL17B beamline at Shanghai Synchrotron Radiation Facility

Zhongjie Zhu  1 , Lanlu Lu  1 , Chunyu Li  1 , Qingjie Xiao  1 , Tingting Wu  1 , Jianchao Tang  1 , Yijun Gu  1 , Kangwen Bao  1 , Yupu Zhang  1 , Luozhen Jiang  1 , Yang Liu  1 , Weizhe Zhang  1 , Shuyu Zhou  1 , Wenming Qin  1
Affiliations

GIWAXS experimental methods at the NFPS-BL17B beamline at Shanghai Synchrotron Radiation Facility

Zhongjie Zhu et al. J Synchrotron Radiat. .

Abstract

The BL17B beamline at the Shanghai Synchrotron Radiation Facility was first designed as a versatile high-throughput protein crystallography beamline and one of five beamlines affiliated to the National Facility for Protein Science in Shanghai. It was officially opened to users in July 2015. As a bending magnet beamline, BL17B has the advantages of high photon flux, brightness, energy resolution and continuous adjustable energy between 5 and 23 keV. The experimental station excels in crystal screening and structure determination, providing cost-effective routine experimental services to numerous users. Given the interdisciplinary and green energy research demands, BL17B beamline has undergone optimization, expanded its range of experimental methods and enhanced sample environments for a more user-friendly testing mode. These methods include single-crystal X-ray diffraction, powder crystal X-ray diffraction, wide-angle X-ray scattering, grazing-incidence wide-angle X-ray scattering (GIWAXS), and fully scattered atom pair distribution function analysis, covering structure detection from crystalline to amorphous states. This paper primarily presents the performance of the BL17B beamline and the application of the GIWAXS methodology at the beamline in the field of perovskite materials.

Keywords: GIWAXS; X-ray; perovskite cells; synchrotron radiation.

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Figures

Figure 1
Figure 1
NREL shows the highest confirmed conversion efficiency for research cells used in a range of photovoltaic technologies from 1976 to the present.
Figure 2
Figure 2
(a) Schematic diagram of GIWAXS on the BL17B beamline at the SSRF. (b) The nucleation and crystallization process of perovskite films (Zhu et al., 2024 ▸). (c) Cs+ and Rb+ addition dictate the growth of perovskite films (Dang et al., 2019 ▸). (d) In situ GIWAXS measurements and schematic models showing the reduced-dimensional hybrid perovskite (RDP) formation for the three distinct fabrication conditions (Zhang et al., 2018 ▸).
Figure 3
Figure 3
The standard bending magnet front-end layout of SSRF.
Figure 4
Figure 4
Layout of the experimental station: (1) attenuator, (2) slit, (3) ion chamber, (4) fast shutter, (5) co-axis microscope, (6) robot, (7) goniometer, (8) fluorescence detector, (9) cryocooler, (10) Pilatus detector.
Figure 5
Figure 5
Schematic diagram of the MXCuBE software user interface.
Figure 6
Figure 6
Schematic illustration of different deposition methods (i.e. one-step spin-coating, two-step spin-coating, vapor deposition and anti-solvent engineering) (Choi et al., 2020 ▸).
Figure 7
Figure 7
(a) Photograph of the portable control station and (b) diagram of the software user interface. (c) An example of a diffraction pattern recorded in the GIWAXS experiment.
Figure 8
Figure 8
Schematic diagram of off situ and in situ. (a) Off-situ test, (b) in situ heating, (c) in situ spin coating and (d) in situ atmosphere environment.
Figure 9
Figure 9
Typical achievements in GIWAXS research at the BL17B beamline.
See this image and copyright information in PMC

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