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Characterization of Electrode Materials for Lithium Ion and Sodium Ion Batteries Using Synchrotron Radiation Techniques
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Note: Electrochemical cell for in operando X-ray diffraction measurements on a conventional X-ray diffractometer.

Steffen Hartung1, Nicolas Bucher1, Ramona Bucher1

  • 1TUM CREATE, Singapore 138602, Singapore.

The Review of Scientific Instruments
|September 3, 2015
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A new electrochemical in operando X-ray diffraction (XRD) cell uses thin aluminum windows for safer, high-quality analysis of sodium-ion battery materials during cycling.

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Area of Science:

  • Materials Science
  • Electrochemistry
  • Crystallography

Background:

  • Electrochemical in operando X-ray diffraction (XRD) is crucial for understanding structural dynamics in energy storage materials.
  • Conventional XRD cells often use toxic beryllium windows, necessitating safer alternatives.
  • Analyzing ion insertion/extraction requires in situ structural monitoring.

Purpose of the Study:

  • To design and present a novel electrochemical in operando XRD cell.
  • To demonstrate the cell's capability using aluminum foil as a non-toxic X-ray window.
  • To evaluate the structural changes in sodium-ion battery cathode materials.

Main Methods:

  • Development of a specialized XRD in operando cell incorporating a 6 μm thin aluminum foil X-ray window.
  • Electrochemical cycling of P2-Na(0.7)MnO2 and Na(2.55)V6O16 ⋅ 0.6H2O cathode materials in a half-cell configuration.
  • Acquisition and analysis of in operando XRD patterns during electrochemical charge/discharge processes.

Main Results:

  • The aluminum foil window provided excellent quality diffraction patterns, comparable to conventional cells.
  • High-resolution in operando XRD successfully captured structural evolution during ion insertion/extraction for both cathode materials.
  • The non-toxic aluminum window proved effective for studying sodium-ion battery cathode structural changes.

Conclusions:

  • The developed XRD in operando cell with an aluminum window is a safe and effective tool for materials research.
  • This method enables detailed structural analysis of energy storage materials during electrochemical cycling.
  • The findings facilitate the development of advanced sodium-ion battery technologies.