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Design and comparison of ex situ and in situ devices for Raman characterization of lithium titanate anode material
Authors:Jie Shu  Miao Shui  Dan Xu  Shan Gao  Tingfeng Yi  DongJie Wang  Xing Li  Yuanlong Ren
Institution:(1) Faculty of Materials Science and Chemical Engineering, Ningbo University, Ningbo, 315211, Zhejiang, People’s Republic of China;(2) School of Chemistry and Chemical Engineering, Anhui University of Technology, Maanshan, 243002, Anhui, People’s Republic of China
Abstract:In this paper, ex situ and in situ devices for Raman observations are designed and compared with each other by using lithium titanate as working electrode. In situ cell is made for Raman spectroscopy based on a confocal microscope Raman spectrometer. The instant evolutions of lithium titanate anode material during cycle can be recorded by in situ Raman in detail. Although the in situ technique is an important method to monitor the structure evolution of lithium titanate, it is difficult to conduct an in situ experiment in most laboratories. Moreover, the existence of electrolyte and surface deposits weakens the Raman signals of sample. Therefore, the structure evolution of Li4Ti5O12 cannot be described accurately. For comparison, air-free ex situ device is a simple and cheap tool to achieve the information from lithiated and delithiated samples. By removing the electrolyte and deposits on the sample with dimethyl carbonate, the ex situ Raman pattern shows higher signal to noise ratio than that of in situ Raman result. As a result, the shift and recovery of ex situ Raman bands confirms that the electrochemical reaction of Li4Ti5O12 with Li in 0.0–2.0 V is not a fully reversible process but a partially reversible process.
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