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• High-aspect-ratio ZnO whiskers were hydrothermally synthesized in NaOH–Na2SO4 solutions.
• The influence of Na2SO4 on the formation of ZnO whiskers was investigated.
• Adsorption of SO42− mainly on (1 0 0) plane promoted 1D growth of ZnO whiskers along c-axis.
The influence of Na2SO4 on the formation of ZnO whiskers was investigated in this paper. ZnO whiskers with aspect ratios of up to 50 were synthesized by dissolving ɛ-Zn(OH)2 precursor in NaOH/Na2SO4 solution at room temperature, followed by aging of the resulting solution at 140 °C for 6 h. Fourier transform infrared spectroscopy, Raman spectroscopy, and X-ray photoelectron spectroscopy analyses revealed that SO42− ions were primarily adsorbed on the (1 0 0) plane of the ZnO whiskers via an outer-sphere complex configuration (O—H···O), thereby promoting the one-dimensional growth of ZnO whiskers along the c-axis.