Laboratory X-ray computed tomography imaging protocol allowing the operando investigation of electrode material evolution in various environments

A robust imaging protocol utilizing laboratory XCT is presented. Hybrid 2D/3D imaging at different scales with real-time monitoring allowed to assess, in operation, the evolution of zinc electrodes within three environments, namely alkaline, near-neutral, and mildly acidic. Different combinations of currents were used to demonstrate various scenarios exhibiting both dendritic and smooth deposition of active material. Directly from radiograms, the volume of the electrode and therefore its growth/dissolution rate was estimated and compared against tomographic reconstructions and theoretical values. The protocol combines simplistic cell design with multiple three-dimensional and two-dimensional acquisitions at different magnifications, providing a unique insight into electrode’s morphology evolution within various environments. [Display omitted] •Imaging protocol for investigation of electrode material evolution was developed•Radiographic data allowed to capture the dynamics of the process•Three environments were studied, namely alkaline, near-neutral and mildly acidic•Zinc plating and/or stripping rate could be estimated using only radiograms Materials science; Materials chemistry; Materials characterization