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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

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. 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 monochromatormore » 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.« less

Authors:
ORCiD logo [1]; ORCiD logo [1]; ORCiD logo [2];  [3]; ORCiD logo [1];  [4]; ORCiD logo [5]; ORCiD logo [6];  [6];  [7];  [7]
+ Show Author Affiliations
  1. Univ. of Washington, Seattle, WA (United States)
  2. Univ. of Washington, Seattle, WA (United States); Los Alamos National Lab. (LANL), Los Alamos, NM (United States)
  3. Univ. of Washington, Seattle, WA (United States); easyXAFS LLC, Renton, WA (United States)
  4. Argonne National Lab. (ANL), Lemont, IL (United States)
  5. Los Alamos National Lab. (LANL), Los Alamos, NM (United States)
  6. Binghamton Univ., Binghamton, NY (United States)
  7. The Univ. of Sheffield, Sheffield (United Kingdom)
Publication Date:
Research Org.:
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 Org.:
USDOE Office of Science (SC), Basic Energy Sciences (BES)
OSTI Identifier:
1542825
Report Number(s):
LA-UR-18-26355
Journal ID: ISSN 0034-6748
Grant/Contract Number:  
89233218CNA000001
Resource Type:
Accepted Manuscript
Journal Name:
Review of Scientific Instruments
Additional Journal Information:
Journal Volume: 90; Journal Issue: 2; Journal ID: ISSN 0034-6748
Publisher:
American Institute of Physics (AIP)
Country of Publication:
United States
Language:
English
Subject:
47 OTHER INSTRUMENTATION; Inorganic and Physical Chemistry; XAS; XAFS; XES

Citation Formats

Jahrman, Evan P., Holden, William M., Ditter, Alexander Scott, Mortensen, Devon R., Seidler, Gerald T., Fister, Timothy T., Kozimor, Stosh Anthony, Piper, Louis F. J., Rana, Jatinkumar, Hyatt, Neil C., and Stennett, Martin C. An improved laboratory-based x-ray absorption fine structure and x-ray emission spectrometer for analytical applications in materials chemistry research. United States: N. p., 2019. Web. doi:10.1063/1.5049383.
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Jahrman, Evan P., Holden, William M., Ditter, Alexander Scott, Mortensen, Devon R., Seidler, Gerald T., Fister, Timothy T., Kozimor, Stosh Anthony, Piper, Louis F. J., Rana, Jatinkumar, Hyatt, Neil C., & Stennett, Martin C. An improved laboratory-based x-ray absorption fine structure and x-ray emission spectrometer for analytical applications in materials chemistry research. United States. https://doi.org/10.1063/1.5049383
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Jahrman, Evan P., Holden, William M., Ditter, Alexander Scott, Mortensen, Devon R., Seidler, Gerald T., Fister, Timothy T., Kozimor, Stosh Anthony, Piper, Louis F. J., Rana, Jatinkumar, Hyatt, Neil C., and Stennett, Martin C. Wed . "An improved laboratory-based x-ray absorption fine structure and x-ray emission spectrometer for analytical applications in materials chemistry research". United States. https://doi.org/10.1063/1.5049383. https://www.osti.gov/servlets/purl/1542825.
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@article{osti_1542825,
title = {An improved laboratory-based x-ray absorption fine structure and x-ray emission spectrometer for analytical applications in materials chemistry research},
author = {Jahrman, Evan P. and Holden, William M. and Ditter, Alexander Scott and Mortensen, Devon R. and Seidler, Gerald T. and Fister, Timothy T. and Kozimor, Stosh Anthony and Piper, Louis F. J. and Rana, Jatinkumar and Hyatt, Neil C. and Stennett, Martin C.},
abstractNote = {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.},
doi = {10.1063/1.5049383},
journal = {Review of Scientific Instruments},
number = 2,
volume = 90,
place = {United States},
year = {Wed Feb 27 00:00:00 EST 2019},
month = {Wed Feb 27 00:00:00 EST 2019}
}
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Rapid Mapping of Lithiation Dynamics in Transition Metal Oxide Particles with Operando X-ray Absorption Spectroscopy
text, January 2016

  • Nowack, Lea; Grolimund, Daniel; Samson, Vallerie
  • Nature Publishing Group
  • DOI: 10.5167/uzh-128248
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