高性能SnO_2电极制备、表征及应用研究
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摘要
近二十年来，电催化氧化技术越来越受到国内外环境学者的关注。电催化氧化技术因具有适应性广，氧化性强，无二次污染，反应迅速，设备及其操作简单等优点而日益成为难降解有机废水处理领域的研究热点。
阳极材料是电催化氧化的核心，它决定了电催化氧化有机污染物的反应机理和电流效率等。理想的阳极材料一般需要满足：导电性好；稳定性好；电催化活性高等条件。然而目前正缺乏理想的阳极材料来满足电催化氧化技术的需要，这也大大限制了电化学催化氧化技术的工业化应用。因此，高效、廉价的阳极材料的研发是目前电催化氧化领域的研究重点。
本论文旨在研制适用于电催化氧化技术的高性能SnO_2阳极材料。主要研究工作包括三部分：SnO_2电极制备新方法探索；新型Sb-Ce双掺杂SnO_2电极的研制、表征及应用；新型Sb-Mn双掺杂SnO_2电极的研制、表征及应用。
成功开发了超声喷雾热解法制备钛基掺杂SnO_2电极新技术。研究结果表明，超声喷雾热解法不仅能将掺杂SnO_2膜均匀稳定地沉积在钛基上，而且成膜条件易操控，先驱物易选择，所得电极的电化学性能易调控。以SbCl_3和SnCl_4的盐酸溶液作为先驱物，采用超声喷雾热解法成功制得了钛基Sb掺杂SnO_2电极(Ti／SnO_2-Sb)。在同等条件下，该电极电催化降解苯酚的电流效率较常规法制得的Ti／SnO_2-Sb电极提高20-28％。
采用超声喷雾热解法成功制备了新型钛基Sb-Ce双掺杂SnO_2电极(Ti／SnO_2-Sb-Ce)。该电极适用于电化学降解，能有效地将废水中的难降解有机污染物分解成CO_2、H_2O等简单的无机物。物理化学表征表明，Ce掺杂可显著优化氧化物膜的微观结构，提高电极的比表面积，改善循环伏安特性。对比实验表明，与Ti／SnO_2-Sb电极相比，Ti／SnO_2-Sb-Ce电极降解橙黄Ⅱ的电流效率提高了22％，能耗降低了21％。
采用超声喷雾热解法还成功制备了新型钛基Sb-Mn双掺杂SnO_2电极(Ti／SnO_2-Sb-Mn)。该电极适用于难降解有机废水的电化学转化预处理，提高废水的可生化性。物理化学表征表明，Mn以固溶体的方式掺杂到氧化物膜中，显著改善了电极表面微观结构和循环伏安特性。电化学转化实验表明，Ti／SnO_2-Sb-Mn电极能明显改善橙黄Ⅱ废水和甲基橙废水的可生化性，使BOD_5与COD的比值分别由0.01与0.07提高到0.25与0.30。
In the past two decades, the electrochemical oxidation has been widelyinvestigated for wastewater treatment. Its good applicability, high oxidation efficiency,no secondary contamination, fast reaction rate, and easy operation make it a veryattractive alternative for degrading toxic and biologically refractory organicpollutants.
It is well known that the anodes assemble is the heart of the electrochemicaloxidation process. The efficiency and mechanism of pollutants oxidation dependhighly on the properties of the anodes used. A good anode should meet the followingrequirements: good conductivity, good stability, and high current efficiency. However,industrial application of electrochemical oxidation is restricted due to lack of idealanodes. The development of active anodes is therefore a hot research topic in thisfield.
This thesis systematically developed high-performance SnO_2 anodes for pollutantsdegradation. Major research works included: methological exploration for depositonof uniform oxide films on Ti substrates; preparation and characterization of novelTi/SnO_2-Sb-Ce anodes for pollutants degradation; and preparation andcharacterization of novel Ti/SnO_2-Sb-Mn anodes for pollutants conversion.
A new deposition method, i.e. ultrasonic spray pyrolysis, was developed forelectrodes preparation. Experimental results showed that the ultrasonic spraypyrolysis method could not only select the precursor and control the depositioncondition easily, but also deposite films uniformly. The Ti/SnO_2-Sb electrodes weresuccessfully fabricated using ultrasonic spray pyrolysis. Under the samilar condition,the current efficiency for phenol degradation obtained on the Ti/SnO_2-Sb electrodesprepared by ultrasonic spray pyrolysis was 20-28% higher than that obtained onelectrodes prepared by the conventional methods.
A novel Ti/SnO_2-Sb-Ce electrode for pollutants degradation was successfullyfabricated using ultrasonic spray pyrolysis, which could mineralized the pollutants into CO_2 and H_2O effectively. Physicochemical and electrochemical characterizationindicated the Ce doping could improve the microstructure, specific area and cyclicvoltammograms of electrodes. The orangeⅡdegradation experiments revealed thatthe Ce doping could enhance the current efficiency by 22% and save the energyconsumption by 21%.
A novel Ti/SnO_2-Sb-Mn electrode for pollutants electrochemical conversion wassuccessfully deposited using ultrasonic srpay pyrolysis, which could improve thebiodegradability of wastewater. Physicochemical and electrochemical examinationsdemonstrated that the solid-solution of Mn doping could improve the microstructureand cyclic voltammograms of electrodes effectively. The experimental resultsindicated that the biodegradability of wastewater containing orangeⅡ/Methyl orangewere greatly enhanced after electrochemical pretreatment, and the ratios ofBOD_5/COD of wastewater were increased from 0.01 and 0.07 to 0.25 and 0.30,repectively.
阳极材料是电催化氧化的核心，它决定了电催化氧化有机污染物的反应机理和电流效率等。理想的阳极材料一般需要满足：导电性好；稳定性好；电催化活性高等条件。然而目前正缺乏理想的阳极材料来满足电催化氧化技术的需要，这也大大限制了电化学催化氧化技术的工业化应用。因此，高效、廉价的阳极材料的研发是目前电催化氧化领域的研究重点。
本论文旨在研制适用于电催化氧化技术的高性能SnO_2阳极材料。主要研究工作包括三部分：SnO_2电极制备新方法探索；新型Sb-Ce双掺杂SnO_2电极的研制、表征及应用；新型Sb-Mn双掺杂SnO_2电极的研制、表征及应用。
成功开发了超声喷雾热解法制备钛基掺杂SnO_2电极新技术。研究结果表明，超声喷雾热解法不仅能将掺杂SnO_2膜均匀稳定地沉积在钛基上，而且成膜条件易操控，先驱物易选择，所得电极的电化学性能易调控。以SbCl_3和SnCl_4的盐酸溶液作为先驱物，采用超声喷雾热解法成功制得了钛基Sb掺杂SnO_2电极(Ti／SnO_2-Sb)。在同等条件下，该电极电催化降解苯酚的电流效率较常规法制得的Ti／SnO_2-Sb电极提高20-28％。
采用超声喷雾热解法成功制备了新型钛基Sb-Ce双掺杂SnO_2电极(Ti／SnO_2-Sb-Ce)。该电极适用于电化学降解，能有效地将废水中的难降解有机污染物分解成CO_2、H_2O等简单的无机物。物理化学表征表明，Ce掺杂可显著优化氧化物膜的微观结构，提高电极的比表面积，改善循环伏安特性。对比实验表明，与Ti／SnO_2-Sb电极相比，Ti／SnO_2-Sb-Ce电极降解橙黄Ⅱ的电流效率提高了22％，能耗降低了21％。
采用超声喷雾热解法还成功制备了新型钛基Sb-Mn双掺杂SnO_2电极(Ti／SnO_2-Sb-Mn)。该电极适用于难降解有机废水的电化学转化预处理，提高废水的可生化性。物理化学表征表明，Mn以固溶体的方式掺杂到氧化物膜中，显著改善了电极表面微观结构和循环伏安特性。电化学转化实验表明，Ti／SnO_2-Sb-Mn电极能明显改善橙黄Ⅱ废水和甲基橙废水的可生化性，使BOD_5与COD的比值分别由0.01与0.07提高到0.25与0.30。
In the past two decades, the electrochemical oxidation has been widelyinvestigated for wastewater treatment. Its good applicability, high oxidation efficiency,no secondary contamination, fast reaction rate, and easy operation make it a veryattractive alternative for degrading toxic and biologically refractory organicpollutants.
It is well known that the anodes assemble is the heart of the electrochemicaloxidation process. The efficiency and mechanism of pollutants oxidation dependhighly on the properties of the anodes used. A good anode should meet the followingrequirements: good conductivity, good stability, and high current efficiency. However,industrial application of electrochemical oxidation is restricted due to lack of idealanodes. The development of active anodes is therefore a hot research topic in thisfield.
This thesis systematically developed high-performance SnO_2 anodes for pollutantsdegradation. Major research works included: methological exploration for depositonof uniform oxide films on Ti substrates; preparation and characterization of novelTi/SnO_2-Sb-Ce anodes for pollutants degradation; and preparation andcharacterization of novel Ti/SnO_2-Sb-Mn anodes for pollutants conversion.
A new deposition method, i.e. ultrasonic spray pyrolysis, was developed forelectrodes preparation. Experimental results showed that the ultrasonic spraypyrolysis method could not only select the precursor and control the depositioncondition easily, but also deposite films uniformly. The Ti/SnO_2-Sb electrodes weresuccessfully fabricated using ultrasonic spray pyrolysis. Under the samilar condition,the current efficiency for phenol degradation obtained on the Ti/SnO_2-Sb electrodesprepared by ultrasonic spray pyrolysis was 20-28% higher than that obtained onelectrodes prepared by the conventional methods.
A novel Ti/SnO_2-Sb-Ce electrode for pollutants degradation was successfullyfabricated using ultrasonic spray pyrolysis, which could mineralized the pollutants into CO_2 and H_2O effectively. Physicochemical and electrochemical characterizationindicated the Ce doping could improve the microstructure, specific area and cyclicvoltammograms of electrodes. The orangeⅡdegradation experiments revealed thatthe Ce doping could enhance the current efficiency by 22% and save the energyconsumption by 21%.
A novel Ti/SnO_2-Sb-Mn electrode for pollutants electrochemical conversion wassuccessfully deposited using ultrasonic srpay pyrolysis, which could improve thebiodegradability of wastewater. Physicochemical and electrochemical examinationsdemonstrated that the solid-solution of Mn doping could improve the microstructureand cyclic voltammograms of electrodes effectively. The experimental resultsindicated that the biodegradability of wastewater containing orangeⅡ/Methyl orangewere greatly enhanced after electrochemical pretreatment, and the ratios ofBOD_5/COD of wastewater were increased from 0.01 and 0.07 to 0.25 and 0.30,repectively.
引文
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