Ramasundaram Subramaniyan, Jeevanandham Sampathkumar, Vijay Natarajan, Divya Sivasubramani, Jerome Peter, Oh Tae Hwan
School of Chemical Engineering, Yeungnam University, Gyeongsan 38541, Republic of Korea.
Molecular Science and Engineering Laboratory, Amity Institute of Click Chemistry Research and Studies, Amity University, Noida 201313, Uttar Pradesh, India.
Molecules. 2024 Sep 17;29(18):4411. doi: 10.3390/molecules29184411.
The field of energy storage and conversion materials has witnessed transformative advancements owing to the integration of advanced in situ characterization techniques. Among them, numerous real-time characterization techniques, especially in situ transmission electron microscopy (TEM)/scanning TEM (STEM) have tremendously increased the atomic-level understanding of the minute transition states in energy materials during electrochemical processes. Advanced forms of in situ/operando TEM and STEM microscopic techniques also provide incredible insights into material phenomena at the finest scale and aid to monitor phase transformations and degradation mechanisms in lithium-ion batteries. Notably, the solid-electrolyte interface (SEI) is one the most significant factors that associated with the performance of rechargeable batteries. The SEI critically controls the electrochemical reactions occur at the electrode-electrolyte interface. Intricate chemical reactions in energy materials interfaces can be effectively monitored using temperature-sensitive in situ STEM techniques, deciphering the reaction mechanisms prevailing in the degradation pathways of energy materials with nano- to micrometer-scale spatial resolution. Further, the advent of cryogenic (Cryo)-TEM has enhanced these studies by preserving the native state of sensitive materials. Cryo-TEM also allows the observation of metastable phases and reaction intermediates that are otherwise challenging to capture. Along with these sophisticated techniques, Focused ion beam (FIB) induction has also been instrumental in preparing site-specific cross-sectional samples, facilitating the high-resolution analysis of interfaces and layers within energy devices. The holistic integration of these advanced characterization techniques provides a comprehensive understanding of the dynamic changes in energy materials. This review highlights the recent progress in employing state-of-the-art characterization techniques such as in situ TEM, STEM, Cryo-TEM, and FIB for detailed investigation into the structural and chemical dynamics of energy storage and conversion materials.
由于先进的原位表征技术的整合，能量存储与转换材料领域取得了变革性进展。其中，众多实时表征技术，尤其是原位透射电子显微镜（TEM）/扫描透射电子显微镜（STEM）极大地增进了我们对能量材料在电化学过程中微小过渡态的原子级理解。先进形式的原位/操作中TEM和STEM显微技术还在最精细尺度上为材料现象提供了惊人的见解，并有助于监测锂离子电池中的相变和降解机制。值得注意的是，固体电解质界面（SEI）是与可充电电池性能相关的最重要因素之一。SEI严格控制着在电极-电解质界面发生的电化学反应。利用对温度敏感的原位STEM技术可以有效监测能量材料界面中复杂的化学反应，以纳米到微米级的空间分辨率解读能量材料降解途径中普遍存在的反应机制。此外，低温（Cryo）-TEM的出现通过保留敏感材料的原始状态增强了这些研究。Cryo-TEM还允许观察亚稳相和反应中间体，否则这些物质很难捕获。除了这些复杂技术，聚焦离子束（FIB）诱导在制备特定部位的横截面样品方面也发挥了作用，便于对能量装置内的界面和层进行高分辨率分析。这些先进表征技术的整体整合提供了对能量材料动态变化的全面理解。本综述重点介绍了采用原位TEM、STEM、Cryo-TEM和FIB等先进表征技术在详细研究能量存储与转换材料的结构和化学动力学方面的最新进展。
