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Development of a Lithium Ion Cell Enabling In Situ Analyses of the Electrolyte by Gas Chromatography-Mass Spectrometry

机译:锂离子电池的气相色谱-质谱联用技术对电解质的原位分析

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Within the context of lithium ion batteries (LIB) the elucidation of occurring aging phenomena is of special interest. Therein the aging of the electrolyte, which is in contact with all parts of the LIB, typically represents a good indication of the overall cell status. Nevertheless, state of the art sample preparation for electrolyte analysis requires the mechanical opening of the cell and subsequent electrolyte extraction.Thus, the cells are destroyed during sample preparation and it is not possible to achieve data for multiple different states of health (SOHs) of one specific cell. In case of large cell formats the LIB has to be discharged prior to cell opening and electrolyte extraction further limiting the information to 0% state of charge (SOC). However, several analytical techniques are known, which do not rely on liquid samples, but may provide information about the electrolyte. In this case study an automated sample pretreatment was investigated, which was developed in the work group of Prof. Pawliszyn.The solid phase microextraction (SPME) in combination with gas chromatography mass spectrometry (GC-MS) provides several benefits with regard to the LIB environment - namely the headspace sampling option, the preconcentration of volatile organic compounds (VOCs) at room temperature and the small amount of removed sample. This work reports on the development of a prototype round cell (18650 format) for in situ investigations of the electrolyte. The consumption of vinylene carbonate (VC) and emerging decomposition products have been analyzed at different SOHs. Furthermore, the cell setup provides the possibility to investigate the electrolyte during the formation. In this context sampling was performed at different voltage steps throughout the formation protocol or online while the cell was formatted.
机译:在锂离子电池(LIB)的背景下,阐明发生的老化现象尤为重要。其中,与LIB的所有部分接触的电解质的老化通常很好地表明了整个电池的状态。然而,用于电解质分析的最新样品制备需要机械打开电池并随后进行电解质提取,因此,在样品制备过程中会破坏电池,并且无法获得多种不同健康状态(SOH)的数据一个特定的单元格。如果是大型电池,则必须在打开电池和提取电解液之前先将LIB放电,这样才能进一步将信息限制为0%电荷状态(SOC)。然而,已知几种分析技术,它们不依赖于液体样品,而是可以提供有关电解质的信息。在本案例研究中,研究了由Pawliszyn教授工作组开发的一种自动样品预处理方法。固相微萃取(SPME)与气相色谱质谱(GC-MS)的结合为LIB带来了许多好处环境-即顶空进样选项,室温下挥发性有机化合物(VOC)的预浓缩和少量去除的样品。这项工作报告了用于电解质原位研究的原型圆形电池(18650格式)的开发。碳酸亚乙烯酯(VC)和新兴分解产物的消耗量已在不同的SOH中进行了分析。此外,电池设置提供了在形成过程中研究电解质的可能性。在这种情况下,在整个形成方案中以不同的电压步长进行采样,或者在格式化单元格时在线进行采样。

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