Herein, undoped and antimony (Sb)‐doped zinc oxide (ZnO) thin films are prepared by a sol–gel spin‐coating method. The influence of different annealing atmospheres including nitrogen and argon on pertinent properties of the prepared films is scrutinized. Structural, optical, morphological, and electrical properties of all annealed films are investigated by X‐ray diffraction (XRD), field emission scanning electron microscopy (SEM), transmission electron microscopy (TEM), X‐ray photoelectron spectroscopy (XPS), photoluminescence spectroscopy (PL), ultraviolet–visible spectroscopy, and current–voltage measurement. The XRD results exhibit that the films possess ZnO hexagonal wurtzite without impurity. The deterioration in the crystallinity of the film is highly influenced by Sb dopant and annealing atmosphere exhibiting the decrease in nanoparticle size after annealing in nitrogen, argon atmosphere, and upon doping. XPS results confirm that Sb3+ is well incorporated in ZnO lattice and the shift of XPS spectra in the films annealed in nitrogen atmosphere indicates nitrogen bonding with zinc. The PL spectra exhibit blueshift of near band edge emission due to the Sb dopant substituting in Zn site in ZnO lattice and red‐infrared emission induced by Sb dopant. The decrease in electrical resistance of ZnO film can be obtained by Sb doping and annealing in nitrogen atmosphere.

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In this work, morphological and physical properties of pyramid-like ZnO nanostructures fabricated on Sb-doped ZnO seeding films annealed under different atmospheres are extensively studied. The Sb-doped ZnO seeding films were first prepared by sol–gel spin coating technique onto glass substrate then annealed in nitrogen, air and argon followed by low-temperature hydrothermal process for ZnO nanostructures fabrication. The morphological results exhibit the growth of pyramid-like ZnO nanostructure with increasing density of the ZnO nanostructures. The crystal structure shows pyramid-like ZnO wurtzite hexagonal growth along the c-axis without any impurity phase. The growth of pyramid-like ZnO nanostructures is due to the high growth rate of (002) plane. Photoluminescence spectra exhibit the near-band-edge of all samples while the red emission appears in ZnO nanostructures after the hydrothermal process due to the imperfection in the crystal. The reflectance of ZnO nanostructures covers the visible region with the absorption edge of 375[Formula: see text]nm. The calculation shows the relevant energy band gaps in the range of 3.26–3.28[Formula: see text]eV. The difference in hydrothermally grown ZnO nanostructures is significantly affected by different annealing atmospheres.

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