Cover ChemElectroChem | Enhancing Battery Reliability, Efficiency and Safety
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Enhancing Battery Reliability, Efficiency and Safety

X-ray microscopy (XRM) offers numerous advantages for the non-destructive characterization of batteries. Unlike traditional techniques that require the removal of components and risk contamination, XRM allows batteries to be studied intact, preserving their natural physical and chemical environment.

Non-Destructive Battery Investigation under Real-World Conditions

The technique provides real-time information on physical, electrochemical, and micro-to-nano structural changes during charge/discharge cycles, crucial for understanding battery dynamics under various operating conditions. With submicron and nanoscale resolution, XRM facilitates the detection of defects, cracks, and delamination events, impacting battery performance and lifetime. Its multiscale capability allows for a comprehensive investigation, from the macroscopic view of the entire device to the microscopic examination of individual components, helping to correlate phenomena at different length scales.

Additionally, in situ and in operando experiments provide valuable insights into battery behavior under real-world conditions. By eliminating destructive testing and sample preparation, XRM reduces the cost and time of investigation, allowing multiple batteries to be studied and extensive experiments to be conducted. It also provides multimodal information by simultaneously quantifying the morphology and composition of batteries for a holistic view of their internal structure and chemical makeup.

Flavio Cognigni | Sapienza University of Rome

X-ray microscopy has revolutionized battery research, facilitating the development of more efficient and reliable energy storage systems.

Flavio Cognigni | Sapienza University of Rome

Understanding the Inner Workings of Batteries

This work is a result from a collaboration between the Research Center on Nanotechnology Applied to Engineering (CNIS), Dept. of Basic and Applied Sciences to Engineering (SBAI) of Sapienza University of Rome and the ENEA Casaccia Research Center.

The research team at the ENEA Casaccia Research Center, composed by Dr. Pier Paolo Prosini, Dr. Claudia Paoletti and Dr. Annalisa Aurora (middle image), has been engaged in the fabrication and assembly of various types of batteries. The CNIS research team (left and right image), supported by SBAI and composed by Dr. Flavio Cognigni, Prof. Marco Rossi, Prof. Mauro Pasquali and Prof. Francesca Anna Scaramuzzo, focused on designing experiments to be conducted using sub-micron XRM, followed by image processing and 3D modelling. The SBAI research team was responsible for subjecting the cells to successive charge and discharge cycles to identify potential microstructural variations within the cells through XRM. The three institutions, working collaboratively, subsequently evaluated the experimental results presented in the scientific paper.

Dr. Flavio Cognigni (left) and Dr. Alessia Sanna, technologist from the CNIS lab (right).

Dr. Flavio Cognigni (left) and Dr. Alessia Sanna, technologist from the CNIS lab (right).

The ENEA research group (from left to right): Dr. Annalisa Aurora, Dr. Claudia Paoletti and Dr. Pier Paolo Prosini.

The ENEA research group (from left to right): Dr. Annalisa Aurora, Dr. Claudia Paoletti and Dr. Pier Paolo Prosini.

The SBAI-CNIS research group (from left to right): Prof. Marco Rossi (SBAI-CNIS), Prof. Mauro Pasquali (SBAI-CNIS) and Prof. Francesca Anna Scaramuzzo (SBAI)

Professors from the SBAI-CNIS research group (from left to right): Prof. Marco Rossi (SBAI-CNIS), Prof. Mauro Pasquali (SBAI-CNIS) and Prof. Francesca Anna Scaramuzzo (SBAI)

Flavio Cognigni | Sapienza University of Rome

XRM provided valuable insights into the morphology and composition of the batteries, allowing us to perform multiscale and multimodal 2D/3D experiments exploiting the radiation-matter interactions.

Flavio Cognigni | Sapienza University of Rome
ChemElectroChem Cover Battery Research
ChemElectroChem Cover Battery Research
Copyright: ChemElectroChem

The research of Dr. Cognigni & team made it to the cover of ChemElectroChem in July 2023.

Click enlarge to see full cover.

Copyright: ChemElectroChem

The research of Dr. Cognigni & team made it to the cover of ChemElectroChem in July 2023.

Click enlarge to see full cover.

Multi-Scale Imaging to Study the Inner Workings of Batteries

The focus of the paper was to demonstrate the advanced technical features of a submicron XRM system and its use for investigating the hidden and internal structures of diverse types of batteries. The team specifically looked at Na-ion coin cells, Li-ion pouch cells, and commercial VARTA NiMH cylindrical cells:

Investigating the Internal Structures of Various Battery Types

Na-Ion Coin Cell under the X-ray Microscope
Na-Ion Coin Cell under the X-ray Microscope
Copyright: Flavio Cognigni
Copyright: Flavio Cognigni

Na-ion Coin Cells

For the Na-ion coin cells, the researchers used XRM to verify the component positioning during the manufacturing process, locate damage that occurred during manufacturing, and identify critical manufacturing defects that caused the device to fail.

Pouch Cell under the X-ray Microscope
Pouch Cell under the X-ray Microscope

Li-ion Pouch Cells

For the Li-ion pouch cell, XRM allowed the team to digitally cross-section the subject’s layered structure and identify spherical voids that led to cracks in the electrode material, possibly formed after air bubbles in the electrolyte collapsed during manufacturing.

NiMH Cylindrical Cell under the X-ray Microscope
NiMH Cylindrical Cell under the X-ray Microscope

VARTA NiMH Cylindrical Cell

In the case of the commercial VARTA NiMH cylindrical cell, the group used low-resolution XRM to examine the general structure of the battery and high-resolution XRM to analyze specific components such as the negative electrode, positive electrode, and nickel foam. This allowed them to detect defects and delamination events that could lead to capacity fade and battery failure over time as well as charge/discharge cycles.

Towards a Sustainable and Circular Economy

Overall, the paper demonstrated the potential of multiscale in-situ XRM as a powerful tool for non-destructive battery investigation, providing insights into the inner workings of batteries and monitoring their behavior and evolution over time. This technique has significant implications for battery research and development, especially in the context of advancing European industry and transitioning towards a sustainable and circular economy.

Flavio Cognigni | Sapienza University of Rome

In our research, we benefited greatly from using the ZEISS Xradia 610 Versa microscope. The system provided us with advanced technical features and capabilities that allowed us to perform high-resolution imaging of batteries at various length scales. The system’s ability to perform multimodal and multiscale 2D/3D experiments was critical to their investigation of the hidden and internal structures of different types of batteries.

Flavio Cognigni | Sapienza University of Rome

Improving Battery Performance

The battery degradation process revealed through XRM provides critical insights that can pave the way for developing the battery of the future. By closely monitoring the degradation mechanisms, researchers can identify key factors that contribute to reduced battery performance and lifetime. This knowledge can be leveraged to design more durable and longer-lasting battery materials and architectures.

Understanding the root causes of defects, cracks, and delamination events enables the development of advanced electrode and separator materials with improved structural stability, mitigating these issues and enhancing battery reliability.

Moreover, the real-time operating information provided by X-ray microscopy provides valuable feedback on how batteries respond to various stressors and operating conditions. This information can be used to optimize battery management systems, improving the efficiency and safety of battery operation.

The high spatial resolution of X-ray microscopy allows researchers to investigate the micro- and nanoscale structure of battery components, providing insights into the interactions between active materials, electrolytes, and current collectors. This can lead to the design of tailored interfaces and coatings that optimize ion transport and minimize unwanted side reactions, ultimately improving battery performance and reducing degradation.

In Brief

  • The primary advantage of XRM is its ability to non-destructively characterize batteries while preserving their natural physical and chemical environment. Unlike traditional methods that require disassembly and risk contamination, XRM allows for real-time investigation of physical, electrochemical, and structural changes during charge/discharge cycles.

  • XRM enables researchers to investigate the hidden and internal structures of various battery types, such as Na-ion coin cells and Li-ion pouch cells. It allows for the detection of manufacturing defects, the identification of cracks and delamination events, and the examination of the layered structures of batteries, which is crucial for improving battery performance and reliability.

  • The research highlights the potential of XRM to provide insights into battery degradation mechanisms, which can inform the design of more durable and longer-lasting battery materials. This knowledge can lead to the development of advanced electrode and separator materials, ultimately enhancing battery reliability, efficiency, and safety, and contributing to a sustainable and circular economy.

  • Real-time information from XRM helps researchers understand how batteries respond to various stressors and operating conditions. This feedback can be utilized to optimize battery management systems, improve efficiency and safety, and design tailored interfaces that enhance ion transport and minimize unwanted side reactions, thereby improving overall battery performance.

  • XRM plays a pivotal role in the development of correlative microscopy workflows to solve multiscale materials challenges. Indeed, XRM can be used to investigate microstructures in macroscale samples to identify key regions of interest (ROIs). 3D localized region ROIs can be accessed using femtosecond (fs) laser on a FIB-SEM (ZEISS Crossbeam). The use of a fs-laser enables rapid material removal in the load lock and access large cross sections to pre-screen ROIs. High-quality surfaces and structures can be prepared using the Ion-sculptor Ga-FIB. The prepared samples can be investigated using a wide range of detectors including EDS, WDS, EBSD, ToF-SIMS or STEM.


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