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Title: An improved laboratory-based x-ray absorption fine structure and x-ray emission spectrometer for analytical applications in materials chemistry research

Journal Article · · Review of Scientific Instruments
DOI:https://doi.org/10.1063/1.5049383· OSTI ID:1542825

X-ray absorption fine structure (XAFS) and x-ray emission spectroscopy (XES) are advanced x-ray spectroscopies that impact a wide range of disciplines. Furthermore, 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 XAFS and XES spectrometer based on the general conceptual design of Seidler et al. [Rev. Sci. Instrum. 85, 113906 (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) measurement and analysis 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 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.

Research Organization:
Energy Frontier Research Centers (EFRC) (United States). Northeastern Center for Chemical Energy Storage (NECCES); Los Alamos National Lab. (LANL), Los Alamos, NM (United States)
Sponsoring Organization:
USDOE Office of Science (SC), Basic Energy Sciences (BES)
Grant/Contract Number:
89233218CNA000001
OSTI ID:
1542825
Report Number(s):
LA-UR-18-26355
Journal Information:
Review of Scientific Instruments, Vol. 90, Issue 2; ISSN 0034-6748
Publisher:
American Institute of Physics (AIP)Copyright Statement
Country of Publication:
United States
Language:
English
Citation Metrics:
Cited by: 55 works
Citation information provided by
Web of Science

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Cited By (6)

Interface Engineering V 2 O 5 Nanofibers for High‐Energy and Durable Supercapacitors journal June 2019
A wavelength‐dispersive X‐ray spectrometer for in/ex situ resonant inelastic X‐ray scattering studies journal April 2019
Laboratory EXAFS determined structure of the stable complexes in the ternary Ni( ii )–EDTA–CN system journal January 2019
In-house setup for laboratory-based x-ray absorption fine structure spectroscopy measurements journal July 2019
Laboratory-Based X-ray Absorption Spectroscopy on a Working Pouch Cell Battery at Industrially-Relevant Charging Rates journal January 2019
A Feasibility Investigation of Laboratory Based X-ray Absorption Spectroscopy in Support of Nuclear Waste Management journal January 2020

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