For the analysis of the structural transformation, electrodes were prepared by mixing the 3D-ZnSb or 2D-ZnSb [70 weight % (wt %)] as an active material, super P (15 wt %) as a conductor, and polyvinylidene fluoride dissolved in N-methyl pyrrolidinone (15 wt %) as a binder on copper foil substrates. These materials were dried under vacuum at 80°C for 8 hours. The coin cell was assembled in a dry room. Electrochemical discharge-charge reactions of 3D-ZnSb and 2D-ZnSb were performed with a potential range between 3.0 to ~0.63 V (3D-ZnSb) and 3.0 to ~0.6 V (2D-ZnSb) at a current density of 100 mAh g−1. In situ XRD measurement during the electrochemical reaction for 3D-ZnSb and 2D-ZnSb was carried out at the 5A beamline of the Pohang Accelerator Laboratory. The wavelength of the x-ray beam was 0.69265 Å, and XRD patterns were collected on a mar345 image plate detector in the transmission mode for every 3-min interval with 3 s of exposure time.

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