Abstract
Scanning electrochemical microscopy (SECM) used in the feedback mode is one of the most powerful versatile analytical tools used in the field of battery research. However, the application of SECM in the field of lithium-ion batteries (LIBs) faces challenges associated with the selection of a suitable redox mediator due to its high reactivity at low potentials at lithium metal or lithiated graphite electrodes. In this regard, the electrochemical/chemical stability of 2,5-di-tert-butyl-1,4-dimethoxybenzene (DBDMB) is evaluated and benchmarked with ferrocene. This investigation is systematically carried out in both linear and cyclic carbonates of the electrolyte recipe. Measurements of the bulk current with a microelectrode prove that while DBDMB decomposes in ethyl methyl carbonate (EMC)-containing electrolyte, bulk current remains stable in cyclic carbonates, ethylene carbonate (EC) and propylene carbonate (PC). Ferrocene was studied as an alternative redox mediator, showing superior electrochemical performance in ethyl methyl carbonate-containing electrolytes in terms of degradation. The resulting robustness of ferrocene with SECM is essential for a quantitative analysis of battery materials over extended periods. SECM approach curves depict practical problems when using the decomposing DBDMB for data acquisition and interpretation. This study sheds light towards the use of SECM as a probing tool enabled by redox mediators.
Highlights
Scanning electrochemical microscopy (SECM), among other scanning probe techniques, is one of the most powerful tools in the field of battery research [1]
This study presents the evaluation of DBDMB and ferrocene as potential redox mediators to enable SECM used in the feedback mode in different electrolyte solvents, enlisting linear and cyclic carbonates
Analysis of the current at a microelectrode over time showed that DBDMB decomposes in ethyl methyl carbonate (EMC)-containing electrolytes
Summary
Scanning electrochemical microscopy (SECM), among other scanning probe techniques, is one of the most powerful tools in the field of battery research [1]. SECM used in the feedback mode has received significant attention in the field of lithium-ion batteries (LIBs) [2]. SECM is a probing method that uses electrodes with a diameter of nano- or micrometers, usually made from platinum, referred to as the tip and is applied in a liquid medium. These microelectrodes are used in close proximity to the sample and a voltage is applied between the tip and counter electrode. In the so-called feedback mode, a redox mediator is added to the solution and a voltage is applied for oxidation. The redox mediator is oxidized at the tip according to Equation (1) and reduced again at the counter electrode
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