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通过正交试验分析不同阳极氧化电压、氧化时间、氧化次数以及热处理温度对TiO2纳米管阵列电极性能的影响机理,使用电化学工作站测试电极光电化学性能,结合扫描电子显微镜、X射线衍射、紫外–可见漫反射光谱等表征手段着重研究影响电极催化性能的内在机理。结果表明:不同阳极氧化和热处理使电极获得不同的微观结构和晶型,导致电极光催化性能差异明显。60V恒压下1次阳极氧化1h的样品经500℃热处理后,保持规整的纳米管阵列结构和较大的活性面积,并获得了特殊的分层混晶结构,具有较好的催化活性。同时,使用同一电极进行多次光催化制氢反应。紫外光照下,在0.5mol/LNa2SO4+0.5 mol/L乙二醇水溶液中,0.5 V偏压下获得了5.3 mL/(h cm2)的稳定产氢速率,证明电极具有稳定的光催化制氢活性。
The effects of different anodic oxidation voltage, oxidation time, oxidation times and heat treatment temperature on the performance of TiO2 nanotube array electrode were analyzed by orthogonal test. The electrochemical performance of the electrode was tested by electrochemical workstation. The electrochemical and electrochemical properties of the electrode were investigated by scanning electron microscopy (SEM), X - ray diffraction Visible diffuse reflectance spectroscopy and other means of characterization focused on the intrinsic mechanism of the electrode catalytic performance. The results show that different anodic oxidation and heat treatment make the electrode get different microstructure and crystal form, which leads to obvious difference of the photocatalytic performance of the electrode. After the sample was heated at 500 ℃ for 1 hour at 60V, the regular nanotube array structure and the larger active area were maintained, and a special layered mixed crystal structure was obtained with good catalytic activity. At the same time, multiple photocatalytic hydrogen production reactions were performed using the same electrode. Under the UV light irradiation, a steady hydrogen production rate of 5.3 mL / (h cm2) was obtained at a bias voltage of 0.5 V in a 0.5 mol / L Na 2 SO 4 + 0.5 mol / L ethylene glycol aqueous solution, demonstrating that the electrode has a stable photocatalytic hydrogen production activity .