以SnCl2/SbCl3的乙二醇/乙腈混合液浸渍大孔SiO2载体，经多次水解沉积、高温煅烧制备大孔ATO/SiO2电极.SEM和XRD分析表明ATO（Sb-SnO2）微粒均匀负载在SiO2薄层上，4次水解沉积材料体积电阻率10 ?•cm，比表面77 m2•g-1.电化学测试表明，大孔ATO/SiO2电极在酸性条件下析氧电位2.5 V且对对氯苯酚的降解具有良好的电催化性能，而Fe2+的添加又可显著提高羟基自由基的产生率，从而进一步增大该电极的电流效率.
The macroporous ATO/SiO2 materials were prepared through multiple steps of hydrolysis deposition in ethylene glycol and acetonitrile mixed solutions of SnCl2/SbCl3 and subsequent calcination at high temperature. The structures of the obtained materials were characterized by means of SEM and XRD. The results showed that the nano-ATO chemically deposited on the SiO2 support underwent well-controlled aggregation and recrystallization to form a sandwich structure (ATO-SiO2-ATO). Through four times loading of ATO the volume resistivity and the specific surface area reached 10 ??cm and 77 m2?g-1, respectively. The oxygen evolution potential on macroporous ATO/SiO2 anode was 2.5 V in acidic condition and exhibited the electro-catalysis ability in degradation of 4-chlorophenol. It was also found that Fe2+ can significantly improve the current efficiency of ATO/SiO2 macroporous electrode in 4-chlorophenol solution by promoting the generation of OH radicals.
[1] Li-Choung Chiang, Juu-En Chang, Shu-Chuan Tseng. Electrochemical oxidation pretreatment of refractory organic pollutants [J]. J Water Science and Technology, 1997, 36(2-3): 123-130.
[2] Houk L L, Johnson S K, Feng J. Electrochemical incineration of benzoquinone in aqueous media using a quaternary metal oxide electrode in the absence of a soluble supporting electrolyte [J]. J Appl electrochem, 1998, 28(11): 1167-1177.
[3] Sarracco G, Solarino L, Aigotti R, et al. Electrochemical oxidation of organic pollutants at low electrolyte concentrations[J]. J Electrochim Acta, 2000, 46: 373-380.
[4] Elangovan E, Ramesh K, Ramamurthi K. Studies on the structural and electrical properties of spray deposited SnO2:Sb thin films as a function of substrate temperature [J]. J Solid State Commun, 2004, 130(8): 523-527.
[5] Stucki S, Kotz R, Carcer B, et al. Electrochemical waste water treatment using high overvoltage anodes Part II: Anode performance and applications [J]. J App1 Electrochem, 1991, 21(2): 99-104
[6] Hu Y, Hou S H. Preparation and characterization of Sb doped SnO2 thin films from colloidal precursors[J]. J Materials Chemistry and Physics, 2004, 86(1) : 21-25.
[7] Fockedey E, Van Lierde A. Coupling of anodic and cathodic reactions for phenol electro-oxidation using three-dimensional electrodes[J]. J Water Research, 2002, 36(16) : 4169-4175.
[8] Cui Yu-hong(崔玉红), Feng Yu-jie(冯玉杰), Liu Jun-feng(刘俊峰). Preparation and characterization on Sb doped Ti-base SnO2 electrocatalytic electrodes [J]. J Function Materials, 2005, 36(2) : 234-237
[9] Kong De-sheng(孔德生), Lv Wen-hua(吕文华), Feng Yuan-yuan(冯媛媛), et al. Advances and some problems in electrocatalysis of DSA electrodes[J]. J Progress In Chemistry(化学进展), 2009, 21(6):1108-1117.
[10] Feng Yu-jie(冯玉杰), Cui Yu-hong(崔玉红), Wang Jian-jun(王建军). Preparation and characterization of Dy doped Ti-base SnO2 / Sb electro-catalytic Electrodes [J]. J Inorg Chem (无机化学学报), 2005, 21(6) : 837-841.
[11] Li Shan-ping(李善评), Cao Han-lin(曹翰林), Hu Zhen(胡振). Preparation and performance of Ti / Sb-SnO2 electrodes doped with rare earth La [J]. J Inorg Chem (无机化学学报), 2008. 24(3) : 369-374.
[12] Zhang Rui-feng (张瑞丰), Long Neng-bing(龙能兵),Zhang Le-le(张乐乐). Preparation of 3-dimensional SiO2 structures via a templating method [J]. J Thin Solid Films,2009,517:6677-6680.
[13] Long Neng-bing(龙能兵), Zhang Rui-feng (张瑞丰). Preparation and photo-degradation of large-sized TiO2/SiO2 Macroporous materials [J]. J Inorg Chem (无机化学学报), 2009, 25(7) : 1153-1158.
[14] Tong S P, Ma C A, Feng H. A novel PbO2 electrode preparation and its application in organic degradation[J]. J Electrochim Acta, 2008, 53(6) : 3002-3006.
[15] Zhang J R, Gao L. Antimony-doped tin oxide nanocrystallites prepared by a combustion process[J]. J Material Letters, 2004, 58(22/23) : 2730-2734
[16] Comminellis C, Pulgarin C. Anodic oxidation of phenol for wastewater treatment [J]. J Appl Electrochem, 1991, 21(8) : 703-709.
[17] Rajkumar D, Palanivelu K. Electrochemical treatment of industrial wastewater [J]. J Hazard Mater, 2004, 113(1-3) :123-129.
[18] Chen Zhen(陈震), Chen Xiao(陈晓), Zheng Xi（郑曦), et al. Influence of pH and current concentration on electrochemical-generated hydroxyl radical for degradation and decolorization of dye wastewater[J]. J Research of Environmental Science, 2002, 15(3) : 42-44,52.
[19] Zhang Tie-Ming(张铁明), Wang Xun-hua(王勋华), Zhao Hao-feng(赵峰鸣), et al. Preparation of La2O3 doped ??PbO2 electrode and its application in electrochemical degradation of organic [J]. J Research of Environmental Science(化工学报) , 2008, 59(1) : 64-69.
