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ARTICLE NATURE COMMUNICATIONS | https://doi.org/10.1038/s41467-020-20334-6 Fig. 3 Zn plating dynamics on 3D Zn-Mn alloy imaged by in-situ optical microscope. a Schematic illustration of the experimental setup. b SEM image of 3D Zn-Mn alloy. c–e The early stage of Zn plating. Images were taken with a ×20 water immersion objective at 25 frames per second, and the experiment was performed at a current density of 80 mA cm−2. c shows the 3D Zn-Mn alloy before the experiment. d, e show the differential images at 10 s and 30 s, respectively, after the start of the experiment. f–h Zn plating on 3D Zn-Mn alloy. The experiment was performed at a current density of 80 mA cm−2 for 320 s. f, g are the images of 3D Zn-Mn alloy before and after Zn plating. h was calculated by (g–f)/f = (ΔI/I). i–q Evolution of Zn plating on the 3D Zn-Mn alloy. i–q are from the three different regions of interest labeled in f, where i–k, l–n, and o–q correspond to regions E, F, and G in f, respectively. The images were taken at 0 s (i, l, o), 160 s (j, m, p), and 320 s (k, n, q). The black dashed lines in (i–q) circle out the trench regions (i–n) and the protruding regions (o–q). Scale bars: 10 μm. The corresponding SEM and optical images of the 3D Zn-Mn alloy are shown in Fig. 3b, c, respectively. The optical image clearly shows the 3D structures of the Zn-Mn alloy with hierarchical pores on the surface. The contrast of the optical image originated from the morphologies and variations in reflectance at different locations. The brighter areas represent material protruding from the surface and high reflectivity, and the darker areas correspond to the trenches and low reflectivity. The shapes and sizes of the 3D structures match very well with those in the SEM images, demonstrating the feasibility of using optical microscopy to study the dynamic process of electrode reactions. To understand the Zn plating process on the 3D Zn-Mn alloy, a constant current was applied through the electrodes while the optical images were obtained at a certain framerate. The experimental conditions used in the in-situ optical microscopy study were identical to those in the Zn battery test. The entire Zn plating process was recorded, and the optical signal reflected the morphological changes during the charging and discharging processes. The spatial resolution in the optical imaging system could not resolve the initial nucleation sites that are smaller than the diffraction limit, however, it allows us to image and measure the entire Zn deposition process. This information provides critical evidence that we have utilized the morphology of 3D Zn- Mn alloy to control the reaction kinetics and minimize the dendrite formation. The pristine Zn anode was studied first using the in-situ optical microscope (Supplementary Fig. 27a). The Zn dendrites nucleated on the electrode surface after 60s of plating and continued to grow through the entire process (Supplementary Fig. 27b, c and Supplementary Movie 2). The results showed that the Zn plating on the pristine Zn surface was inhomogeneous, leading to both vertical and lateral growth of dendrites at a certain location (bottom right in Supplementary Fig. 27). To completely understand why the dendrite growth can be suppressed on the surface of this Zn-Mn alloy, we carefully studied the Zn plating dynamics using the in-situ optical microscopy and COMSOL 6 NATURE COMMUNICATIONS | (2021)12:237 | https://doi.org/10.1038/s41467-020-20334-6 | www.nature.com/naturecommunicationsPDF Image | high-performance dendrite-free seawater-based batteries
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