In-House X-Ray Absorption Spectroscopy Measurement Using X-Ray Diffractometer: Comparison with Synchrotron Facilities

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Abstract:

X-ray Absorption Spectroscopy (XAS) experiments are usually performed at synchrotron facilities utilizing high-intensity X-ray sources produced by particle accelerators. However, this study showcases an in-house XAS experiment carried out using an X-ray Diffractometer (XRD) system that is typically available in material laboratories. The Rigaku SmartLab XRD was employed and configured for the Bragg-Brentano (BB) measurement mode. 20 keV electron energy is used to energize a molybdenum (Mo) target and produce high-intensity white X-rays via the Bremsstrahlung effect. Several crystals were tested as crystal analyzers for white X-ray dispersion to obtain optimal X-ray intensity and resolution. The detector energy filter is optimized to increase the peak-to-background ratio then the energy dispersion and resolution over the θ/2θ scanning range is determined and evaluated. The performance of the in-house XAS experiment is compared to theoretical calculations and synchrotron data from previous studies by observing resolution and spectrum shape and peak features of deposited Copper (Cu) and Copper Oxide (CuO) samples. Our findings showed that the absorption edges were clearly observed despite the peak broadening and shifting above absorption edge. Furthermore, some peaks were also observed in the XAS spectrum which originated from X-ray fluorescence of elements from both the samples and hardware components.

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Engineering Headway (Volume 15)

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107-113

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January 2025

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© 2025 Trans Tech Publications Ltd. All Rights Reserved

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[1] X. Shibo and C. Heaton, "XAFS analysis and applications to nanomaterials," Encyclopedia of Nanomaterials (First Edition). Elsevier, p.39–49, 2023.

DOI: 10.1016/b978-0-12-822425-0.00103-2

Google Scholar

[2] G. T. Seidler et al., "A laboratory-based hard x-ray monochromator for high-resolution x-ray emission spectroscopy and x-ray absorption near edge structure measurements," Rev. Sci. Instrum., vol. 85, no. 11, 2014.

DOI: 10.1063/1.4901599

Google Scholar

[3] C. Schlesiger, L. Anklamm, H. Stiel, W. Malzer, and B. Kanngießer, "XAFS spectroscopy by an X-ray tube based spectrometer using a novel type of HOPG mosaic crystal and optimized image processing," J. Anal. At. Spectrom., vol. 30, no. 5, p.1080–1085, 2015.

DOI: 10.1039/c4ja00303a

Google Scholar

[4] E. P. Jahrman et al., "Laboratory-Based X-ray Absorption Spectroscopy on a Working Pouch Cell Battery at Industrially-Relevant Charging Rates," J. Electrochem. Soc., vol. 166, no. 12, pp. A2549–A2555, 2019.

DOI: 10.1149/2.0721912jes

Google Scholar

[5] A. P. Honkanen, S. Ollikkala, T. Ahopelto, A. J. Kallio, M. Blomberg, and S. Huotari, "Johann-type laboratory-scale x-ray absorption spectrometer with versatile detection modes," Rev. Sci. Instrum., 2019.

DOI: 10.1063/1.5084049

Google Scholar

[6] "X-ray absorption spectroscopy," ANSTO Official Website. https://www.ansto.gov.au/facilities/australian-synchrotron/synchrotron-beamlines/x-ray-absorption-spectroscopy

DOI: 10.46427/gold2020.936

Google Scholar

[7] C. Glover et al., "Status of the X-ray Absorption Spectroscopy (XAS) beamline at the Australian synchrotron," AIP Conf. Proc., vol. 882, no. February, p.884–886, 2007.

DOI: 10.1063/1.2644692

Google Scholar

[8] J. L. Wedding, B. Lai, S. Vogt, and H. H. Harris, "Investigation into the intracellular fates, speciation and mode of action of selenium-containing neuroprotective agents using XAS and XFM," Biochim. Biophys. Acta - Gen. Subj., vol. 1862, no. 11, p.2393–2404, 2018.

DOI: 10.1016/j.bbagen.2018.03.031

Google Scholar

[9] X. Cheng et al., "Understanding Structure-Performance Relationships of Coox/Ceo2 Catalysts for No Catalytic Oxidation: Facet Tailoring and Bimetallic Interface Designing," SSRN Electron. J., vol. 451, no. February, p.131144, 2023.

DOI: 10.2139/ssrn.4326274

Google Scholar

[10] T. Williams et al., "Gnuplot 5.4," vol. 4, no. September, 2022.

Google Scholar

[11] A. Jain et al., "Commentary: The materials project: A materials genome approach to accelerating materials innovation," APL Materials. 2013.

DOI: 10.1063/1.4812323

Google Scholar

[12] K. Mathew et al., "Data descriptor: High-throughput computational X-ray absorption spectroscopy," Sci. Data, vol. 5, p.1–8, 2018.

Google Scholar

[13] L. K. H. K. Alwis, M. R. Mucalo, B. Ingham, and P. Kappen, " A Combined SNIFTIRS and XANES Study of Electrically Polarized Copper Electrodes in DMSO and DMF Solutions of Cyanate (NCO − ), Thiocyanate (NCS − ) and Selenocyanate (NCSe − ) Ions ," J. Electrochem. Soc., 2015.

DOI: 10.1149/2.0321507jes

Google Scholar