以硫酸钛和氟硅酸水热法制备花状多级TiO2微球

doi:10.15541/jim20140114

摘要/Abstract

摘要：

以廉价的硫酸钛为原料和氟硅酸为结构控制剂, 用成本低效益好的水热法制备暴露{001}面纳米片组装的花状多级TiO₂微球。这些多级微球是由许多交联的纳米片组装。通过调变氟硅酸根离子的浓度可以容易地控制多级微球的精细结构。通过XRD和SEM表征来检测微球的生长过程, 并提出了可能的形成机理。与其他溶解热合成法相比, 这种成本低效益好的水热合成法有望应用于大批量生产花状多级TiO₂微球。这种精制的花状多级TiO₂微球展现了很好的光催化降解甲基橙的能力。

关键词: 花状, 水热合成, 晶体生长, 多级结构

Abstract:

Flower-like hierarchical TiO₂ microspheres assembled by nanosheets with exposed {001} facets were prepared through a cost-effective hydrothermal synthesis method, using cheap Ti(SO₄)₂ as the feedstock and hexafluorosilicic acid as the capping agent. These hierarchical microspheres were assembled by numerous and cross-linked nanosheets. The fine structure of hierarchical microspheres could be easily controlled by adjusting the concentration of hexafluorosilicic ions. The growth process of the microspheres was examined through XRD and SEM characterizations, and a possible formation mechanism was proposed. Compared with other solvothermal synthesis methods, this cost-effective hydrothermal synthesis route is attractive and can be potentially applied in the production of flower-like TiO₂ hierarchical microspheres in large scale. The as-prepared flower-like TiO₂ hierarchical microspheres exhibit good photocatalytic ability to degrade methyl orange dye.

Key words: flower-like, hydrothermal synthesis, crystal growth, hierarchical structure

中图分类号:

TQ174

施国栋, 宋军, 杨柳柳, 张利雄. 以硫酸钛和氟硅酸水热法制备花状多级TiO₂微球[J]. 无机材料学报, 2014, 29(8): 891-896.

SHI Guo-Dong, SONG Jun, YANG Liu-Liu, ZHANG Li-Xiong. Hydrothermal Synthesis of Flower-like Hierarchical TiO₂ Microspheres from Titanium Sulfate and Hexafluorosilicic Acid[J]. Journal of Inorganic Materials, 2014, 29(8): 891-896.

图/表 6

Fig. 1 XRD pattern (a), FESEM images with low (b) and high (c) magnifications, FESEM image (d) of a broken sample, <br/> low-magnification (e) and high-resolution (f) TEM image of the flower-like TiO2 microspheres The insets in (e) and (f) show the TEM image of the nanosheet at high magnification and FFT pattern, respectively

Fig. 2 FESEM images of the samples prepared with precursor hydrogel of different n(Ti4+): n(F-): n(H2O) (a) 1: 0.3: 15; (b) 1: 1.5: 15; (c) 1:3: 15; (d) 1: 6: 15; (e) 1: 9: 15; (f) 1: 0: 15

Fig. 3 XRD pattern of the samples prepared with a molar composition of 1Ti4+: 4.5F-: 15H2O at 180℃ for different time (1)2 h; (b) 3 h; (c) 4 h; (d) 5 h; (e) 12 h

Fig. 4 FESEM images of the samples prepared with a molar composition of 1Ti4+: 4.5F-: 15H2O at 180℃ for different time (a) 2 h; (b) 3 h; (c) 4 h; (d) 5 h; (e) 12 h

Fig. 5 N2 adsorption-desorption isotherm and pore size distribution curve (a) and UV-visible absorption spectra (b) of hierarchical flower-like TiO2 (1) As-prepared; (2) From the literature[8]

Fig. 6 UV-Vis spectra of MO aqueous solution in the presence of hierarchical flower-like TiO2 under UV light irradiation (a) and the fitting of absorbance maximum plot vs time over the hierarchical flower-like TiO2 (b)

参考文献 15

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以硫酸钛和氟硅酸水热法制备花状多级TiO₂微球

Hydrothermal Synthesis of Flower-like Hierarchical TiO₂ Microspheres from Titanium Sulfate and Hexafluorosilicic Acid

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