TiO aerogel is a unique three-dimensional porous nano-particle material with the characteristics of high specific surface area and good light transmittance. In this paper, a novel method involving ultrasonic-assisted sol-gel, solvent exchange, and vacuum drying was successfully developed to synthesis the TiO aerogel. The morphology and properties of the prepared TiO aerogels were characterized by the Brunauer-Emmett-Teller theory (BET), x-ray diffraction, field-emission scanning electron microscopy, energy dispersive spectroscopy, thermogravimetric analysis-differential thermal analysis, Fourier transform infrared spectroscopy, and Raman spectroscopy. The adsorption and photocatalytic activity of TiO aerogels was evaluated by monitoring the degradation of Rhodamine B solution. Our results indicated that: (1) with an optimum ratio of Ti:HO = 8:1 the BET surface area, average pore diameter, and total pore volume of TiO aerogel are enhanced to 563.6 m g, 3.01 nm, and 0.42 cm g, respectively; (2) the TiO aerogels possessed controllable crystal form depending on the thermal treatments conditions. The crystal face (101) of anatase, complete anatase, mixed state of anatase and rutile, and rutile were obtained by increasing the temperature from 200 °C-300 °C, from 400 °C-500 °C, 600 °C, and from 700 °C-1000 °C, respectively; and (3) the excellent catalytic activity of the as-prepared TiO aerogels for the ultraviolet photolytic degradation of Rhodamine B had attributed to the synergistic effect of adsorption and photoactivity.

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