Abstract

We present an approach for multi-layer preparation to perform microstructure analysis of a Li-ion cell anode active material using synchrotron tomography. All necessary steps, from the disassembly of differently-housed cells (pouch and cylindrical), via selection of interesting layer regions, to the separation of the graphite-compound and current collector, are described in detail. The proposed stacking method improves the efficiency of synchrotron tomography by measuring up to ten layers in parallel, without the loss of image resolution nor quality, resulting in a maximization of acquired data. Additionally, we perform an analysis of the obtained 3D volumes by calculating microstructural characteristics, like porosity, tortuosity and specific surface area. Due to a large amount of measurable layers within one stacked sample, differences between aged and pristine material (e.g., significant differences in tortuosity and specific surface area, while porosity remains constant), as well as the homogeneity of the material within one cell could be recognized.

Highlights

  • In recent times, electrochemical energy storage has become more important, especially for usage in e-mobility applications, such as pure electrical, plug-in-hybrid or mild-hybrid vehicles

  • Synchrotron tomography is a useful tool to obtain the microstructural characteristics of the Li-ion anode material

  • The analysis addresses two main questions that play an important role in the investigation of Li-ion cells: 1. Can the microstructure of graphite be regarded as statistically homogeneous over the whole cell?

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Summary

Introduction

Electrochemical energy storage has become more important, especially for usage in e-mobility applications, such as pure electrical, plug-in-hybrid or mild-hybrid vehicles. During the lifetime of Li-ion cells, a lot of aging mechanisms [1,2] occur, which affect different components, like the anode or cathode active material, separator, current-collector or electrolyte. These analysis methods allow a quantitative description of the samples and show the potential of synchrotron tomography in combination with refined preparation techniques as a valuable tool for the investigation and characterization of functional materials

Extraction of Samples
Cell Disassembly
Sample Selection
Separation of Graphite Layers
Surface Modification
Multilayer Preparation
Separation Materials
Layer Stacking
Stack Slicing and Final Setup
Discussion
Synchrotron Tomography
Data Post-Processing
Structural Analysis
Can the influence of aging on the microstructure of graphite be characterized?
Comparison of Structural Characteristics
Findings
Summary
Conclusions
Full Text
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