Publication date: 10th April 2024
Potential sweep methods involve measuring the current response while the applied potential is swept. In the most common technique, named cyclic voltammetry (CV), the sweep rate is kept constant up to a point where it is then reversed. These techniques are well established for probing redox reactions in liquid electrochemistry. More recently, potential sweep methods have also been widely utilized for studying redox reactions in both solid electrolytes and solid electrodes.
For an insertion reaction, however, the classic analysis must be modified to account for fundamental differences between solid-state and liquid-state storage. After a review of the decisive differences between typical liquid-state and solid-state, first, necessary modifications to the classical analysis are discussed. Numerical simulations are presented to illustrate how in intercalation systems the current response depends on the sweep rate and insertion thermodynamics. Second, CV measurements under wide range of sweep rates using TiO2 and Nb2O5 thin films (different thicknesses) are presented which allow for testing the proposed novel analysis. It is shown how reliably solid-state kinetic parameters (e.g., Li diffusivity in TiO2 thin films) can be obtained. The conventional practices of the common electrochemical methods (including CV) have produced drastically inconsistent chemical diffusion coefficients in the literature, which ranges over many orders of magnitude (e.g., seven orders of magnitude regarding Li in TiO2). To confirm the reliability of the extracted Li diffusivity, other electrochemical measurements (galvanostatic intermittent titration technique (GITT), electrochemical impedance spectroscopy (EIS), and battery cycling) of TiO2 thin films (well-defined geometry and of high quality) were also performed. Based on the careful and precise measurements and evaluations, all the methods give consistent results.
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