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Materials Characterization for Lithium Ion Battery Technology

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Materials Characterization for Lithium Ion Battery Technology

By AZoM

Table of Contents
Introduction Significance of Materials Characterization Pristine Materials Morphology and Uniformity Surface Chemistry and Composition Cycled Cell Characterization About Evans Analytical Group

Introduction
Dedicated characterization tools can be used to gain insight into material behavior during battery research and development, production and operation. Matching the measurement technique with both the data required and the dimensions of the feature or layer of interest is a key step in achieving desired goals. Evans Analytical Group provides analytical methods and expertise to better understand the materials utilized in the anodes, cathodes, and electrolytes of existing lithium ion batteries and next generation of batteries for automotive applications.

Significance of Materials Characterization

Since batteries have found use in new markets, gaining insight into material problems is imperative. The commercialization of new battery technologies demands a suite of mechanical, electrical and environmental stress testing. Moreover, gaining insight into the materials employed and their behavior throughout the life cycle of the battery system can provide useful data about the processes taking place within the battery systems and their potential failure mechanisms. Modern batteries consist of a variety of organic, inorganic and metallic components, with sizes in the range of between and cm. It is essential to use the appropriate tools to analyze these components. Evans Analytical Group has an extensive range of analytical instruments to tackle materials problems related to all stages of battery development.

Pristine Materials

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It is important to control the consistency of pristine electrode materials to ensure that lithium ion batteries have desirable energy, power and lifespan. Instrumental gas analysis (IGA) is used to study elements such as S, O, N, C, and H, while inductively coupled plasma-optical emission spectrometry (ICP-OES) enables measurement of the composition of major elements. Glow discharge mass spectrometry (GDMS) is suitable to monitor impurity levels for a complete mass range elemental analysis with lower detection limits or ppm. X-ray diffraction (XRD) is an ideal technique to measure the phase identification and crystallinity of pristine cathode materials. The analysis of a pristine NCA cathode is shown in Table 1. Table 1. Analysis of a pristine NCA cathode
Elements Measured Li O C N S Al Mn Co Ni Elemental Composition wt% 7.6 30.9 0.31 0.22 <0.001 1.2 <0.005 8.9 46.6

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Materials Characterization for Lithium Ion Battery Technology

Tab and electrode alignment is typically monitored using a real-time X-ray (RTX). An RTX image of a lithium ion 18650 cell is shown in Figure 1.

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Figure 1. RTX image of a lithium ion 18650 cell

Morphology and Uniformity

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Gaining insight into the materials employed in cell production is important to better understand the parameter that have an impact on the cycle life of a battery. Microscopy approaches such as transmission electron microscopy (TEM) and scanning electron microscopy (SEM) are ideal techniques to analyze particle size, morphology and particle agglomeration and shortcomings during materials acceptance, process development and actual production. An SEM image of a pristine LiFePO4 cathode is shown in Figure 2, demonstrating a good particle size distribution and the lack of excessive agglomeration of particles.

Figure 2. SEM image of an LiFePO4 cathode An SEM image of a pristine graphitic carbon anode that has significant difference in particle size and a non-uniform distribution of carbon black particles is shown in Figure 3.

Figure 3. SEM image of a graphitic anode A TEM image of a pristine LiFeP04 cathode particle is depicted in Figure 4, clearly showing the thin carbon coating which improve the electrical conductivity, with thickness measurements. The crystallinity of the particle is also illustrated in Figure 4, enabling to verify thickness consistency by surveying several particles.

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Materials Characterization for Lithium Ion Battery Technology

Figure 4. TEM image of an LiFePO4 cathode The combination of superior resolution of TEM and energy dispersive X-ray spectroscopy (EDS) or electron energy loss spectroscopy (EELS) enables obtaining compositional information from thin layers or very small areas, as shown in Figure 5.

Figure 5. An EELS linescan across the outer edge of the particle confirms the coating is composed of carbon only.

Surface Chemistry and Composition

The electrolyte utilized in lithium ion batteries forms a film called as the solid electrolyte interphase (SEI) on the surfaces of electrodes during battery cycling. Methods that provide elemental details and inorganic and molecular data are suitable to investigate the film growth process and decomposition chemistry. Auger Electron Spectroscopy (AES) is an ideal method for analyzing the surface of individual cathode or anode particles. The lateral distribution of elements of interest can be shown by elemental mapping with AES, as shown in Figure 6. With incremental sputtering utilizing an argon ion beam, it is possible to obtain elemental depth profiles through layers, such as the SEI.

Figure 6. SEM and AES images of battery electrode surfaces

Cycled Cell Characterization

The formation of SEI layer on electrode particles during cell cycling can be investigated using the superior lateral resolution of TEM. It is possible to obtain data on possible SEI growth mechanisms by detecting the composition of SEI layers using TEM-EELS or TEM-EDS. Gaining insight into the chemical state of elements on the surfaces of electrodes is important to understand the electrochemical processes taking place at different components of the battery, such as current collectors, electrolyte components, and electrodes. A TEM image of an SEI layer created on a cycled LiFeP04 cathode particle is shown in Figure 7.

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Figure 7. TEM image of an SEI layer on a cathode particle Phosphorus chemistry on a graphitic anode prior to and after cell cycling can be investigated using X-ray photoelectron spectroscopy (XPS), as shown in Figure 8, where the cycled cell demonstrates an increased phosphate bonding in relation to LiPF 6.

Figure 8. XPS analysis of graphitic anode An analysis of a particle on the surface of a graphitic anode film after removing from a cycled cell is shown in Figure 9. P is present from the electrolyte consisting of LiPF 6.

Figure 9. Graphite anode particle analysis A Time of Flight Secondary ion Mass Spectrometry (TOF-SIMS) spectrum that was obtained from a LiCoO2 cathode after its removal from a cycled cell is shown in Figure 10, enabling to identify a number of molecular species of interest. Applications and appropriate techniques for lithium ion batteries are listed in Figure 11.

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Figure 10. TOF-SIMS spectrum from a LiCoO2 cathode

Figure 11. Summary of analysis methods for Li ion cells

About Evans Analytical Group

Evans Analytical Group (EAG) has been a global leader in surface analysis and materials characterization for over 30 years, delivering innovative analytical services and solutions with uncompromising scientific integrity. Since our inception in 1978 as Charles Evans & Associates, our guiding principal has been innovative problem solving underscored by a commitment to excellence.

This information has been sourced, reviewed and adapted from materials provided by Evans Analytical Group. For more information on this source, please visit Evans Analytical Group. Date Added: May 21, 2013 | Updated: May 21, 2013

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