The crystal structures of all 3D-ZnSb, 2D-AZnSb, and 2D-ZnSb samples were investigated by x-ray diffractometry (SmartLab, Rigaku) and probe-corrected scanning TEM (JEM-ARM200F, JEOL). We measured the XRD patterns of all samples under high-quality Ar atmosphere using an atmosphere separator for SmartLab to prevent the oxidation during measurements. The TEM sample preparation was carried out using a dual-beam focused ion beam (FIB) (AURIGA CrossBeam Workstation, Carl Zeiss) slicing and lift-out technique. STEM-EDS and STEM–EELS (electron energy-loss spectroscopy) were used for the atomic scale–resolved chemical mapping and the lithium detection, respectively. The simulation of diffraction pattern was performed by using the CrystalMaker software with the parameters experimentally gained by XRD measurement. To prevent the oxidation of samples, an Ar-purged glove bag was attached to the entrance of FIB and TEM chambers during the loading and unloading processes. The chemical compositions of 3D-ZnSb, 2D-AZnSb, and A-etched 2D-ZnSb samples were analyzed by ICP-MS. The XPS of the samples was carried out using micro x-ray photoelectron spectrometer with a monochromatic Al Kα (1486.7 eV) x-ray source. The chamber pressure was maintained below 5.0 × 10−10 torr during the measurements. XPS spectra of single crystalline 2D-LiZnSb were obtained by cleaving in ultrahigh vacuum to prevent oxidation. XPS spectra of 3D-ZnSb and 2D-ZnSb were obtained after removing the surface contamination by using Ar gas cluster ion beam sputtering (32). To monitor any abnormality in the sample during the sputtering, a full survey spectrum and high-resolution XPS spectra measurements were made. The shift in the binding energy due to the relative surface charging was calibrated using the C 1s level at 284.6 eV as an internal standard.

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