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Effect of synthesis conditions on photocatalytic activities of nanoparticulate TiO2 thin films

机译:合成条件对纳米TiO2薄膜光催化活性的影响

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In the present study, design of experiments (DOE) was used to find an optimal combination for the factors affecting the preparation, morphology and catalytic activity of nano-crystalline TiO2 thin films synthesized by sol-gel method. Nine TiO2 thin films were prepared onto indium-tin oxide (ITO) substrates by changing four operating parameters at three levels. The four operating parameters are the volume of 20% acetic acid aqueous solution, the volume of co-solvent alcohol, the amount of template reagent (triblock copolymer Pluronic P123), and the calcination temperature. The resulting films were characterized by X-ray diffraction (XRD), field emission-scanning electron microscopy (FE-SEM), atomic force microscopy (AFM), and Fourier transform-infrared (FT-1R) spectra. The results of DOE are examined by both the direct observation analysis (also called range analysis) and the analysis of variance (ANOVA) with 90 or 95% confidence intervals. The parameter settings have been optimized as the combination of precursor solution constitution of Ti(OC4H9)4/20%HAC/EtOH/P123 (2 g/15 ml/8 ml/1.1 g), calcination temperature of 450 °C, calcination time of 3 h, and air reaction atmosphere. The thin film prepared under the optimal combination consists of ordered compact anatase nanoparticles with an average grain size of approximately 17.2 nm and an average roughness of 3.653 nm. The 1-h photodegradation efficiency of methyl orange (MO) in aqueous solution and toluene in gaseous phase is 98.9 and 100%, respectively. The factor analysis results of degradation efficiencies show that the calcinations temperature plays an important role in determining the photocatalytic activity of the prepared TiO2 thin film. Furthermore, the surface morphology-dependent photocatalytic activity of the prepared thin films was also found.
机译:在本研究中,通过实验设计(DOE)找到了影响溶胶-凝胶法合成纳米TiO2薄膜的制备,形貌和催化活性的因素的最佳组合。通过在三个级别上更改四个操作参数,在氧化铟锡(ITO)基板上制备了九个TiO2薄膜。四个操作参数是20%乙酸水溶液的体积,助溶剂醇的体积,模板试剂(三嵌段共聚物Pluronic P123)的数量和煅烧温度。通过X射线衍射(XRD),场发射扫描电子显微镜(FE-SEM),原子力显微镜(AFM)和傅立叶变换红外(FT-1R)光谱对所得膜进行表征。通过直接观察分析(也称为范围分析)和具有90%或95%置信区间的方差分析(ANOVA)来检查DOE的结果。优化了参数设置,结合了Ti(OC4H9)4/20%HAC / EtOH / P123(2 g / 15 ml / 8 ml / 1.1 g)的前体溶液组成,450°C的煅烧温度,煅烧时间3小时,和空气反应气氛。在最佳组合下制备的薄膜由有序的紧密锐钛矿纳米粒子组成,平均粒径约为17.2 nm,平均粗糙度为3.653 nm。水溶液中甲基橙(MO)和气相中甲苯的1-h光降解效率分别为98.9和100%。降解效率的因子分析结果表明,煅烧温度在决定所制备的TiO2薄膜的光催化活性中起着重要作用。此外,还发现了制备的薄膜的表面形态依赖性的光催化活性。

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