Herein, the effect of the postannealing process on the structural properties of nitrogen‐doped Zinc oxide nanostructures (N‐ZnO) synthesized by a single‐step hydrothermal method is reported. Detailed structural and compositional characterizations are performed using X‐ray diffraction (XRD), X‐ray photoelectron spectroscopy (XPS), field emission scanning electron microscopy (FESEM), and energy‐dispersive spectroscopy (EDS). Also, the amount of nitrogen doping has been optimized using different concentrations of the precursor solutions and they are subjected to different postannealing environments. The postannealing process is found to alter the defect structure in ZnO significantly. The samples showing the highest nitrogen doping are further evaluated in detail to know their structural variations. The incorporation of nitrogen into the ZnO structure and the effects of the postannealing process substantially alter the electrochemical characteristics by changing the surface properties of ZnO nanosheets. The effect of these structural variations on the electrochemical performance of ZnO is also explored. Under optimized conditions, the highest conductivity of N‐ZnO nanostructures obtained suggests the material as an outstanding candidate for electrochemical applications.
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