Sulym Iryna, Goncharuk Olena, Sternik Dariusz, Skwarek Ewa, Derylo-Marczewska Anna, Janusz Wladyslaw, Gun'ko Vladimir M
Chuiko Institute of Surface Chemistry, NASU, 17 General Naumov Str., 03164, Kyiv, Ukraine.
Faculty of Chemistry, Maria Curie-Sklodowska University, 20-031, Lublin, Poland.
Nanoscale Res Lett. 2016 Dec;11(1):111. doi: 10.1186/s11671-016-1304-1. Epub 2016 Feb 29.
A series of TiO2-ZrO2/SiO2 nanocomposites were synthesized using a liquid-phase method and characterized by various techniques, namely, nitrogen adsorption-desorption, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, high-resolution transmission electron microscopy, and photon correlation spectroscopy (PCS). It was revealed that the component ratio and calcination temperature affect the phase composition of nanocomposites. Composites TiZrSi1 (TiO2:ZrO2:SiO2 = 3:10:87) and TiZrSi2 (10:10:80) calcined at 1100 °С demonstrate the presence of t-ZrO2 crystallites in TiZrSi1 and ZrTiO4 phase in TiZrSi2. The samples calcined at 550 °С were amorphous as it was found from XRD data. According to the Raman spectra, the bands specific for anatase are observed in TiZrSi2. According to XPS data, Zr and Ti are in the highest oxidation state (+4). Textural analysis shows that initial silica is mainly meso/macroporous, but composites are mainly macroporous. The particle size distributions in aqueous media showed a tendency of increasing particle size with increasing TiO2 content in the composites.
采用液相法合成了一系列TiO₂-ZrO₂/SiO₂纳米复合材料，并用多种技术对其进行了表征，即氮气吸附-脱附、X射线衍射（XRD）、X射线光电子能谱（XPS）、拉曼光谱、高分辨率透射电子显微镜和光子相关光谱（PCS）。结果表明，组分比例和煅烧温度会影响纳米复合材料的相组成。在1100℃煅烧的复合材料TiZrSi1（TiO₂:ZrO₂:SiO₂ = 3:10:87）和TiZrSi2（10:10:80）中，TiZrSi1中存在t-ZrO₂微晶，TiZrSi2中存在ZrTiO₄相。根据XRD数据，在550℃煅烧的样品为非晶态。根据拉曼光谱，在TiZrSi2中观察到了锐钛矿特有的谱带。根据XPS数据，Zr和Ti处于最高氧化态（+4）。织构分析表明，初始二氧化硅主要为介孔/大孔，但复合材料主要为大孔。水性介质中的粒径分布显示，随着复合材料中TiO₂含量的增加，粒径有增大的趋势。
