Valtsifer Viktor A, Sivtseva Anastasia V, Kondrashova Natalia B, Shamsutdinov Artem S, Averkina Anastasia S, Valtsifer Igor V, Feklistova Irina N, Strelnikov Vladimir N
Institute of Technical Chemistry, Ural Branch, Russian Academy of Sciences, Perm Federal Research Center, Russian Academy of Sciences, 614013 Perm, Russia.
The Faculty of Biology, Belarusian State University, 220045 Minsk, Belarus.
Nanomaterials (Basel). 2023 Sep 11;13(18):2537. doi: 10.3390/nano13182537.
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(OH)(NO)∙2HO. 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(OH)(NO)∙2HO) 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 ions in the supernatant of ZnO samples with different particle sizes and shapes. It was shown that the residual amount of Zn 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 ions was 10.22 mg/L.
本研究考察了合成条件的影响,包括使用具有不同分子量(400 - 12,600 g/mol)和各种亲水/疏水特性的非离子结构形成化合物(表面活性剂),以及使用玻璃基板和水热暴露对ZnO样品的织构和结构性能的影响。通过X射线分析确定,在所有情况下合成中间体都是化合物Zn(OH)(NO)∙2HO。结果表明,该化合物在600℃下热解,无论表面活性剂的物理化学性质如何,都会导致形成具有纤锌矿结构和球形或椭圆形颗粒的ZnO。随着表面活性剂分子量和粘度的增加,颗粒尺寸略有增大,从使用Pluronic F - 127(MM = 12,600)时的30 nm增加到使用Pluronic L - 31(MM = 1100)、PE - block - PEG(MM = 500)和PEG(MM = 400)时的80 nm。将预洗涤的合成中间体(Zn(OH)(NO)∙2HO)在水热条件下保持会导致形成各种尺寸的六方ZnO棒状晶体结构。结果表明,在使用Pluronic P - 123(MM = 5800)进行水热暴露期间获得的样品中观察到最大的ZnO颗粒(10 - 15μm)。原子吸收光谱法对不同粒径和形状的ZnO样品上清液中的残留锌离子进行了比较定量分析。结果表明,在检测具有30 - 80 nm球形颗粒的ZnO样品时,锌离子的残留量更高。例如,在粒径为30 nm的ZnO样品的上清液中,锌离子的定量含量为10.22 mg/L。