Quantitative manganese dissolution investigation in lithium-ion batteries by means of X-ray spectrometry techniques,Journal of Analytical Atomic Spectrometry

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Quantitative manganese dissolution investigation in lithium-ion batteries by means of X-ray spectrometry techniques
Journal of Analytical Atomic Spectrometry ( IF 3.1 ) Pub Date : 2021-08-26 , DOI: 10.1039/d0ja00491j
Claudia Zech ₁ , Marco Evertz ₂ , Markus Börner ₂ , Yves Kayser ₁ , Philipp Hönicke ₁ , Martin Winter _{2,

3} , Sascha Nowak ₂ , Burkhard Beckhoff ₁

Affiliation

Each battery suffers from degradation effects which lead to capacity fading and life cycle reduction. With electrochemical methods, the battery capacity decrease can easily be monitored, but they are inappropriate to comprehend the underlying chemical and physical properties responsible for the capacity fading. In the present paper, we demonstrate the power of X-ray spectrometry techniques to investigate the transition metal dissolution (TMD) fading process for manganese in Lithium Ion Batteries (LIBs). Regarding aging processes, quantitative analyses are important to evaluate the magnitude of a certain process for the total capacity decrease. The challenge for the investigation of aged battery materials is the lack of reference materials such that techniques based on them cannot be applied. With the use of reference sample-free quantitative X-ray fluorescence analysis (XRF), we investigated the total mass deposition of manganese deposited at the anode for an aged cell. For 50 full cycles with elevated cut-off voltage, the capacity decreased by 12.5%, while up to 1.6‰ of cathodic manganese was found deposited in the anode. Furthermore, the species of manganese deposited in the anode has been studied with near-edge X-ray absorption fine structure analysis (NEXAFS) at the manganese L-edges and K-edges. In addition to a different discrimination capability at L- and K-edges, the application of significantly different excitation energies provides sensitivity to different sample depths. We determined the manganese deposition to be in di- and tetra-valent states, whereby tetravalent manganese is solely found in the anode bulk. The combination of the different methods generates a clearer understanding of the chemical processes in the battery and can therefore help to improve the performance by exploring the absolute mass deposition and the electronic structure of elements contained in enhanced material combinations.

中文翻译：

基于 X 射线光谱技术的锂离子电池中锰溶解的定量研究

每个电池都会受到退化效应的影响，从而导致容量衰减和寿命周期缩短。使用电化学方法，可以很容易地监测电池容量的下降，但它们不适合理解导致容量衰减的潜在化学和物理特性。在本文中，我们展示了 X 射线光谱技术在研究锂离子电池 (LIB) 中锰的过渡金属溶解 (TMD) 褪色过程中的强大功能。关于老化过程，定量分析对于评估某个过程对总容量下降的幅度很重要。老化电池材料研究面临的挑战是缺乏参考材料，无法应用基于它们的技术。通过使用无参考样品的定量 X 射线荧光分析 (XRF)，我们研究了老化电池阳极上沉积的锰的总质量沉积。在截止电压升高的 50 个完整循环中，容量下降了 12.5%，同时发现高达 1.6‰的阴极锰沉积在阳极中。此外，已在锰 L 边和 K 边处使用近边 X 射线吸收精细结构分析 (NEXAFS) 研究了阳极中沉积的锰种类。除了在 L 和 K 边缘具有不同的辨别能力外，显着不同的激发能量的应用提供了对不同样品深度的灵敏度。我们确定锰沉积处于二价和四价状态，因此四价锰仅存在于阳极体中。

更新日期：2021-08-26

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