Synthesis of Mesoporous Anatase TiO2 Sphere with High Surface Area and Enhanced Photocatalytic Activity

doi:10.1016/j.jmst.2016.03.019.

Abstract

Abstract:

Mesoporous anatase TiO₂ spheres with high surface area (119?m²?g^-1) were successfully synthesized via a facile and green template-free method. The prepared TiO₂ was characterized by X-ray diffraction (XRD), N₂ adsorption, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and UV-vis absorbance spectra. It was found that the prepared TiO₂ is characterized by pure anatase phase, which shows uniform spheres and has a typical mesostructure with a high specific surface area and a large pore volume. The effects of complexant (acetylacetone) amount, crystallization temperature and calcination temperature were also investigated. Based on the results, a sketch for the preparation of mesoporous TiO₂ was proposed. First, complex formed between tetrabutyl titanate and acetylacetone in ethanol. After introduction of aqueous of ammonia sulfate and urea, hydrolysis of tetrabutyl titanate would occur slowly, and sol of TiO₂ was formed. Then, crystallization proceeded under hydrothermal conditions. Calcination process favored the formation of bigger TiO₂ crystal through combining of the small crystals in TiO₂. This led to the formation of bigger mesopores between TiO₂ crystals. Photocatalytic activity of the prepared TiO₂ was evaluated by decomposition of methyl orange.

Key words: TiO2, Mesoporous, Template-free method, Photocatalysis

Lu Tianliang,Wang Youqiang,Wang Yingli,Zhou Lipeng,Yang Xiaomei,Su Yunlai. Synthesis of Mesoporous Anatase TiO₂ Sphere with High Surface Area and Enhanced Photocatalytic Activity[J]. J. Mater. Sci. Technol., 2017, 33(3): 300-304.

Figures/Tables 9

Fig.1. XRD patterns of TiO2 prepared with different acetylacetone amounts: (a) TiO2-0-95-450; (b) TiO2-1-95-450; (c) TiO2-2-95-450; (d) TiO2-4-95-450; (e) TiO2-6-95-450.

Fig.2. SEM images of TiO2 prepared with different acetylacetone amounts: (a) TiO2-0-95-450; (b) TiO2-1-95-450; (c) TiO2-2-95-450; and (d) TEM image of TiO2-2-95-450.

Fig.3. XRD patterns of TiO2 prepared under different crystallization temperatures: (a) TiO2-2-80-450; (b) TiO2-2-95-450; (c) TiO2-2-120-450; (d) TiO2-2-150-450.

Fig.4. XRD patterns of TiO2 prepared under different calcination temperatures: (a) TiO2-2-95-uncalcination; (b) TiO2-2-95-350; (c) TiO2-2-95-450; (d) TiO2-2-95-600; (e) TiO2-2-95-800.

Table 1 Physical property of TiO2 prepared under different calcination temperatures

Entry	Sample	BET surface area (m²?g^-1)	Total pore volume (mL?g^-1)
1	TiO₂-2-95-uncalcination	325	0.50
2	TiO₂-2-95-350	187	0.44
3	TiO₂-2-95-450	119	0.30
4	TiO₂-2-95-600	35	0.10

Fig.5. N2 sorption isotherms (a) and pore size distribution (b) of TiO2 prepared under different calcination temperatures.

Fig.6. Photodegradation of methylene orange (10?mg?L-1) over the TiO2 prepared under different calcination temperatures. Decomposition efficiency of η was calculated by η?=?(A0?-?At)/(A0?-?0.032)?×?100%, and A0and At are the initial absorbance before reaction and the absorbance after reaction for t h, respectively.

Fig.7. Photodegradation of methylene orange (10?mg?L-1) over the prepared mesoporous TiO2 spheres and that over Degussa P25. Decomposition efficiency of η was calculated by η?=?(A0?-?At)/(A0?-?0.032)?×?100%, and A0 and At are the initial absorbance before reaction and the absorbance after reaction for t h, respectively.

Fig.8. UV/Vis diffuse-reflectance spectra of Degussa P25 and the mesoporous anatase TiO2-2-95-450.

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Synthesis of Mesoporous Anatase TiO₂ Sphere with High Surface Area and Enhanced Photocatalytic Activity

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