| Summary: | This work investigated the influence of synthesis conditions, including the use of nonionic structure-forming compounds (surfactants) with different molecular weights (400–12,600 g/mol) and various hydrophilic/hydrophobic characteristics, as well as the use of a glass substrate and hydrothermal exposure on the texture and structural properties of ZnO samples. By X-ray analysis, it was determined that the synthesis intermediate in all cases is the compound Zn<sub>5</sub>(OH)<sub>8</sub>(NO<sub>3</sub>)<sub>2</sub>∙2H<sub>2</sub>O. It was shown that thermolysis of this compound at 600 °C, regardless of the physicochemical properties of the surfactants, leads to the formation of ZnO with a wurtzite structure and spherical or oval particles. The particle size increased slightly as the molecular weight and viscosity of the surfactants grew, from 30 nm using Pluronic F-127 (MM = 12,600) to 80 nm using Pluronic L-31 (MM = 1100), PE-block-PEG (MM = 500) and PEG (MM = 400). Holding the pre-washed synthetic intermediates (Zn<sub>5</sub>(OH)<sub>8</sub>(NO<sub>3</sub>)<sub>2</sub>∙2H<sub>2</sub>O) under hydrothermal conditions resulted in the formation of hexagonal ZnO rod crystal structures of various sizes. It was shown that the largest ZnO particles (10–15 μm) were observed in a sample obtained during hydrothermal exposure using Pluronic P-123 (MM = 5800). Atomic adsorption spectroscopy performed comparative quantitative analysis of residual Zn<sup>2+</sup> ions in the supernatant of ZnO samples with different particle sizes and shapes. It was shown that the residual amount of Zn<sup>2+</sup> ions was higher in the case of examining ZnO samples which have spherical particles of 30–80 nm. For example, in the supernatant of a ZnO sample that had a particle size of 30 nm, the quantitative content of Zn<sup>2+</sup> ions was 10.22 mg/L.
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