Analytical Sciences

Abstract − Analytical Sciences, 36(1), 47 (2020).

Development of Simultaneous Measurement System for X-ray Absorption Spectra at Two Absorption Edges
Misaki KATAYAMA,* Hirona YAMAGISHI,* Yusaku YAMAMOTO,** and Yasuhiro INADA**
*Synchrotron Radiation Center, Ritsumeikan University, 1-1-1 Noji-Higashi, Kusatsu 525-8577, Japan
**Department of Applied Chemistry, College of Life Sciences, Ritsumeikan University, 1-1-1 Noji-Higashi, Kusatsu 525-8577, Japan
Dispersive X-ray absorption fine structure (DXAFS) spectroscopy is a versatile measurement technique for analyzing chemical reactions in real time. We have developed a novel time-resolved DXAFS instrument based on two polychromators and a wide-range position-sensitive detector that permits direct observation of the synergistic effects of two elements. This system enables simultaneous acquisition of the X-ray absorption spectra for two different elements without any mechanical movement of the X-ray optics. The developed system was successfully applied to monitor both the synthesis of a Ni–Cu bimetallic catalyst, which revealed that the reduction of Ni occurred at a higher temperature than that of Cu, and the charge–discharge processes of a LixNi0.5Mn1.5O4-based lithium-ion battery, which demonstrated that the redox reactions of Ni and Mn occurred sequentially at specific electrode potentials.