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

doi:10.15541/jim20140114

Abstract

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

CLC Number:

TQ174

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.

Figures/Tables 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)

References 15

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

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