Operando Freezing Cryogenic Electron Microscopy of Active Battery Materials

Area of Science:

• Materials Science
• Electrochemistry
• Microscopy

Background:

• Understanding battery material evolution is key for safer, more efficient energy storage.
• Cryogenic electron microscopy (cryo-EM) is valuable for battery characterization but sample prep can alter structures.
• Current methods lack the ability to preserve dynamic changes occurring during battery cycling.

Purpose of the Study:

• To develop and validate a method for operando freezing cryo-EM.
• To preserve and characterize native electrode and interfacial structures during battery cycling.
• To enable direct visualization of transient features in electrochemical systems.

Main Methods:

• Development of an operando plunge freezer and cold sample removal process.
• Application of the method to multiple electrode materials for validation.
• Quantification and discussion of the achieved freezing rates.

Main Results:

• Successful preservation of native electrode and interfacial structures during battery cycling.
• Demonstration of operando freezing cryo-EM's capability to visualize transient features.
• Validation of the method's effectiveness across various electrode materials.

Conclusions:

• Operando freezing cryo-EM provides a powerful tool for studying dynamic processes in batteries.
• This technique allows for a deeper understanding of structural evolution and interfacial chemistry.
• Enables advancements in the design of next-generation energy storage systems.