Development of Combined Small-Angle X-Ray Scattering and Fluorescence Yield X-Ray Absorption Spectroscopy Measurement Systems for Characterization of Structural and Chemical Information of Pt Alloy Nanoparticle Catalyst

Abstract

The understanding of the structural and the chemical properties of Pt catalysts in polymer electrolyte fuel cells (PEFCs) is necessary to improve the activity for the durability of the catalysts. The small-angle X-ray scattering (SAXS) and the X-ray absorption spectroscopy (XAS) measurements are widely used to investigate the properties of Pt catalysts. Recently, Povia et al developed a powerful tool by combining the SAXS and XAS measurements for the characterization of the Pt nanoparticle catalysts [1]. However, this technique is difficult to investigate the chemical states of the low-concentrated catalysts. In this study, we developed the combined SAXS and the fluorescence-yield (FY) XAS measurement systems to investigate the structural and the chemical properties of low-concentrated catalysts. The combined SAXS-FYXAS measurement system was developed at BL19B2 in SPring-8. For the XAS measurements, the Pt LⅢ edge was used. The ionization chamber and a single-element Ge solid state detector were used to obtain the FYXAS spectra. For the SAXS measurements, the X-ray energy was set to 11.5 keV and 11.55 keV, which are below and near to the Pt LⅢ absorption edge, respectively. The scattered X-ray was detected using an area detector (PILATUS 2M). The PtCo alloy nanoparticle for the oxygen reduction reaction was used as the sample in this experiment. As the result, we could demonstrate the combined SAXS-FYXAS measurement systems. We will discuss the degradation mechanism of the PtCo alloy nanoparticle catalyst from both SAXS and FYXAS data. [1] M. Povia et al. ACS. Catal., 8, 7000 (2018).