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TiO2光催化剂的微结构设计及应用
论文作者:童鞋论文网  论文来源:www.txlunwenw.com  发布时间:2019/10/18 14:22:51  

摘要:本文利用改进的水滴模板法和胶体碳球模板法制备出具有优异性能的TiO2薄膜和粉体,多孔TiO2薄膜、高比表面积TiO2微球、空心TiO2/SiO2光催化剂在疏水性和光催化方面有着优秀的表现,这为未来的工作提供了有价值的参考。

通过改进的水滴模板法和高温热处理方法合成具有分级结构的TiO2膜,其表面装饰有微米级的多层孔和亚微米级的TiO2中空结构。实验以通过乙酰丙酮稳定和未稳定的钛酸四正丁酯作钛源。在水滴模板法过程中分别产生前体凝胶薄膜和空心二氧化钛球体,沉积的水滴作为空心结构和孔隙结构形成的模板。通过扫描电子显微镜和透射电子显微镜对合成的TiO2薄膜进行了表征,并通过X-射线衍射和热重分析对热处理过程中凝胶薄膜的热行为和相变进行了分析。由于多层孔和中空结构的修饰,作为表面材料,TiO2薄膜表面经化学处理前后分别表现出较强的亲水性和疏水性。作为光催化剂,表面修饰有二氧化钛中空结构的薄膜表现出较高的光催化活性。

通过简单的水滴模板法制备出具有蜂窝结构的多孔TiO2薄膜。实验以乙酰丙酮稳定和未稳定的钛酸四正丁酯作钛源,氮气携带的饱和水蒸气作为水滴模板的来源。考察了湿气流速和蒸发时间对薄膜微结构的影响。实验结果表明,湿气流速达到3.5 mL/s以上,溶剂蒸发时间达到1.5 min以上时,薄膜表面形成较均匀且排列更紧密的气孔。通过扫描电子显微镜和透射电子显微镜对合成的TiO2薄膜微观形貌进行了观察,并通过X-射线衍射和热重分析对热处理过程中凝胶薄膜的相变和热行为进行了分析。作为表面材料,由于规则的气孔排列,用辛基三甲氧基硅烷处理后薄膜表面表现出较强的疏水性。作为光催化剂,经500 ℃热处理1 h,有着孔径大小均一且分布均匀的薄膜因其更大的表面积而显示出较高的光催化性能。

实验以钛酸四正丁酯为钛源,石油醚与乙酸乙酯的混合物作为溶剂,配制了溶液。利用水滴模板法形成水滴与溶液中的溶质反应。合成了具有高比表面积的TiO2微球。实验考察了混合溶剂的比例对产品微结构及光催化性能的影响。实验结果表明,随着混合溶剂中石油醚与乙酸乙酯体积比的增大,微球直径减小。当石油醚与乙酸乙酯的体积比为1:2时,所合成的TiO2微球因具有较大的比表面积而表现出较高的光催化活性。

以葡萄糖水溶液制备的胶体碳球为模板,通过水热法制备了具有空心结构的TiO2/SiO2粉体及薄膜光催化剂。所合成的TiO2/SiO2光催化剂采用SEM、XRD、IR进行了表征。考察了前驱液中钛酸四正丁酯的浓度对所制备TiO2/SiO2粉体及薄膜光催化剂活性的影响。由于优异的分散性和空心结构,前驱液未被稀释制得的产品经热处理后表现出较高的光催化活性。

In this paper, TiO2 film and powder withexcellent properties were prepared by improved droplet template method andcolloidal carbon sphere template method. Our porous TiO2 film, high specificsurface area TiO2 microsphere and hollow TiO2/SiO2 microstructure haveexcellent hydrophobicity and photocatalysis. This work provides a reference forfuture work.

Hierarchically structured TiO2 films,decorated with both multilayered pores in micron-scale and hollow TiO2 spheresin submicron-scale, were synthesized by a modified breath figure process and asubsequent calcinations process. Acetylaceton-stabilized and unstabilizedtetra-n-butyl titanate were used as titanium sources to produce the precursorgel films and TiO2 hollow structure respectively during the breath figureprocess, and the deposited water droplets were used as templates for theformation of both hollow and pore structures. The synthesized TiO2 films werecharacterized by scanning electron microscopy and transmission electronmicroscopy, and the thermal behavior and phase transformation of primary gelfilms during calcination were analyzed by X-ray diffraction andthermogravimetry. Due to the modification of the multilayer pores and thehollow structure, the surface of the TiO2 film showed strong hydrophilicity andhydrophobicity before and after chemical treatment, respectively. As aphotocatalyst, the thin film modified with TiO2 hollow structure exhibits highphotocatalytic activity.

A porous TiO2 film having a honeycombstructure was prepared by a simple water-droplet templating method. BothAcetylaceton-stabilized and unstabilized tetra-n-butyl titanate were used astitanium source. Saturated water vapor carried by nitrogen were used as asource of the template of water-droplet. The experiment result indicate thatwhen the velocity of moist flow reachs 3.5 mL/s ,and the evaporation time forsolvent reachs 1.5 min ,the pore formed on film surface were more uniform andarranged more closely. The synthesized TiO2 films were characterized byscanning electron microscopy and transmission electron microscopy. The phasetransition and thermal behavior of the gel films during calcination wereanalyzed by X-ray diffraction and thermogravimetric analysis. Due to theordered pores on the surface of the film,after being treated byoctyltrimethoxysilane, the film as a surface material exhibits stronghydrophobicity. After heat-treated at 500 ℃ for 1 h, the film with uniform poresize, as a photocatalyst, exhibits higher photocatalytic property, due to itslarger surface areat.

TiO2 microspheres with high specificsurface area were synthesized in a precursor solution through the reactionbetween prepared by tetra-n-butyl titanate and water droplets forme by breathfigure method. The precursor solution was prepared by using tetra-n-butyltitanate as titanium source and a mixture of petroleum ether and ethyl acetateas solvent. The effect of the volume ratio of petroleum ether to ethyl acetatewas investigated on the microstructure and photocatalytic property of thesynthesized TiO2 spheres. The experimental results suggests that the diameterof TiO2 sphere decreases with increases of the volume ratio of petroleum etherto ethyl acetate. TiO2 sphere synthesized at the volume ratio of petroleumether to ethyl acetate of 1:2 possess higher specific surface area and performhigher photocatalytic avtivity.

TiO2/SiO2 powder and film photocatalysthaving hollow structure was prepared by hydrothermal method, using colloidalcarbon sphere, derived from synthesized glucose solution, as template of hollowstructre. The synthesized TiO2/SiO2 photocatalysts were charactered by SEM, XRDand IR. The effect of the concentration of tetra-n-butyl titanate wasinvestigated on the photocatalytic property of synthesized TiO2/SiO2 powder andfilm. The concentration of tetra-n-butyl titanate was varied by diluting theprecursor solution.

关键词:二氧化钛;水滴模板法;水热法;润湿性能;光催化性

Titanium dioxide; Water droplet templatemethod; Hydrothermal method; Wettability; Photocatalysi

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