Optimizing Battery Development: Integrating Air-Controlled and Cryogenic Electron Microscopy Workflows
Authors: Kim Jae Jin 
Published: December 2024

The global energy landscape is undergoing a profound transformation, shifting from traditional fossil fuel-based systems to sustainable, renewable energy sources like wind, solar, bioenergy, hydroelectric, and tidal energy. This transition signifies a significant evolution in global energy generation and consumption patterns, necessitating advanced energy storage solutions to manage the intermittent nature of renewables and ensure a stable and reliable energy supply. Advanced energy storage technologies, including batteries, supercapacitors, and other innovative systems, play a pivotal role in this transition by enabling effective load balancing, supporting the electrification of transportation through electric vehicles and charging infrastructure, managing peak demand, and facilitating the seamless integration of renewable energy into the grid. This evolution not only advances sustainability goals but also enhances energy security and independence. [1]
Advanced analytical techniques are essential for developing energy storage systems, especially batteries, by providing critical insights into their complex chemical and physical processes. Battery materials' microstructure, composition, and operational dynamics can be explored using analytical techniques like scanning electron microscopy (SEM), focused ion beam (FIB), transmission electron microscopy (TEM), X-ray diffraction (XRD), and spectroscopy. The detailed analysis through these techniques is crucial for optimizing material properties, enhancing energy density, improving safety, and extending battery lifespan. By identifying degradation mechanisms and optimizing electrode and electrolyte materials, these techniques contribute to precise battery engineering. As demand grows for more efficient and higher-capacity batteries, these sophisticated tools are indispensable for advancing energy storage technology. [2]
At Shell Technology Center Houston, we have developed air-controlled and cryogenic electron microscopy (EM) workflows for studying advanced energy storage systems in preparation for the energy transition. The air-controlled EM workflow, employing SEM, FIB, TEM, and XRD, plays a pivotal role in battery research by providing a controlled environment that prevents exposure to atmospheric elements that could alter material properties. These techniques are essential for examining the fine structural details and chemical compositions of battery components under near-native conditions. The cryo-EM workflow using SEM, FIB, and TEM is vital in battery research for studying materials and interfaces sensitive to environmental conditions or rapid degradation upon exposure. These cryogenic techniques involve rapid freezing of battery components to preserve their structure in a close-to-native state and prevent deleterious effects of air exposure such as oxidation or moisture interaction. [3]
In our study, we present comprehensive results obtained using both air-controlled EM and cryogenic EM workflows to investigate advanced energy storage systems, including lithium-ion batteries (LIBs) and beyond-LIBs such as multivalent rechargeable batteries. The utilization of air-controlled EM techniques such as SEM, FIB, TEM, and XRD allows us to examine battery components under controlled environmental conditions, ensuring accurate analysis of structural details and chemical compositions without the risk of atmospheric contamination. Additionally, the use of cryo-EM techniques, including cryo-SEM, cryo-FIB, and cryo-TEM, enables the study of sensitive battery materials and interfaces in a preserved, near-native state. These cryogenic methods prevent degradation effects such as oxidation and moisture interaction, providing unprecedented insights into the ultrastructural properties and operational dynamics of battery materials at atomic or molecular levels. By leveraging both air-controlled and cryogenic EM workflows, we have achieved a comprehensive understanding of battery mechanics and chemistry, paving the way for improved battery design and enhanced performance in energy storage applications.
Reference
[1] International Renewable Energy Agent (IRENA) 2021 https://www.irena.org/publications/2021/Aug/Renewable-energy-statistics-2021
[2] Tarascon, J.-M., Armand, M., Nature 414, 359–367 (2001). https://doi.org/10.1038/35104644
[3] Cheng, D., Lu, B., Raghavendran, G., Zhang, M., and Meng, Y. S., Matter, Volume 5, Issue 1, p26-42, 2022 https://doi.org/10.1016/j.matt.2021.11.019