An Improved Laboratory-Based XAFS and XES Spectrometer for Analytical Applications in Materials Chemistry Research

TL;DR

This paper presents an improved laboratory-based XAFS and XES spectrometer that offers higher flux, wider angle range, and enables routine applications previously limited to synchrotron facilities, expanding analytical chemistry capabilities.

Contribution

The authors develop a novel laboratory XAFS and XES spectrometer with enhanced performance, allowing broader and more routine applications in materials chemistry research.

Findings

Successful measurement of battery electrode materials

Validation of monochromator performance with Ni and V EXAFS

Analysis of uranium oxidation states using XANES and XES

Abstract

X-ray absorption fine structure (XAFS) and x-ray emission spectroscopy (XES) are advanced x-ray spectroscopies that impact a wide range of disciplines. However, unlike the majority of other spectroscopic methods, XAFS and XES are accompanied by an unusual access model, wherein; the dominant use of the technique is for premier research studies at world-class facilities, i.e., synchrotron x-ray light sources. In this paper we report the design and performance of an improved spectrometer XAFS and XES based on the general conceptual design of Seidler, et al., Rev. Sci. Instrum. 2014. New developments include reduced mechanical degrees of freedom, much-increased flux, and a wider Bragg angle range to enable extended x-ray absorption fine structure (EXAFS) for the first time with this type of modern laboratory XAFS configuration. This instrument enables a new class of routine applications that are incompatible with the mission and access model of the synchrotron light sources. To illustrate this, we provide numerous examples of x-ray absorption near edge structure (XANES), EXAFS, and XES results for a variety of problems and energy ranges. Highlights include XAFS and XES measurements of battery electrode materials, EXAFS of Ni and V with full modeling of results to validate monochromator performance, valence-to-core XES for 3d transition metal compounds, and uranium XANES and XES for different oxidation states. Taken en masse, these results further support the growing perspective that modern laboratory-based XAFS and XES have the potential to develop a new branch of analytical chemistry.