Methods for operando coherent X-ray diffraction of battery materials at the Advanced Photon Source

Area of Science:

• Materials Science
• Crystallography
• Electrochemistry

Background:

• Operando characterization of battery electrode materials is crucial for understanding their performance and degradation.
• Bragg coherent X-ray diffraction imaging (BCXD) offers a powerful, non-destructive method for nanoscale visualization of crystal dynamics.
• Previous methods lacked the resolution to observe individual crystal behavior within complex electrode structures.

Purpose of the Study:

• To demonstrate the application of Bragg coherent X-ray diffraction imaging for operando analysis of battery electrode materials.
• To highlight the capabilities of the 34-ID-C beamline at the Advanced Photon Source for such measurements.
• To detail experimental protocols for sample handling, alignment, and data acquisition in BCXD studies.

Main Methods:

• Utilized Bragg coherent X-ray diffraction imaging (BCXD) to probe submicrometer-sized electrode material crystals.
• Employed two approaches: coherent multi-crystal diffraction for collective and individual crystal behavior, and Bragg coherent diffractive imaging for morphology and strain evolution.
• Conducted experiments on a sodium-ion cathode material (NaNi_1/3Fe_1/3Mn_1/3O₂) in a half-cell configuration.

Main Results:

• Successfully visualized the structural, morphological, and strain evolution of individual crystals within operando electrode materials.
• Demonstrated the ability of BCXD to provide both collective and single-crystal insights into phase transitions and dynamic processes.
• Established detailed experimental procedures for effective BCXD measurements on battery materials.

Conclusions:

• Bragg coherent X-ray diffraction imaging is a valuable technique for in-depth operando studies of battery electrode materials.
• The methodology allows for precise monitoring of crystal behavior at the nanoscale, crucial for battery development.
• The study provides a comprehensive guide for implementing BCXD experiments at synchrotron facilities.