TiO_2纳米管光电催化降解有机污染物耦合制氢研究
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摘要
随着工业化和城镇化进程的加快,环境问题和能源危机日益严重。由于氢能具有清洁高效、能量密度高、导热性好等特点必将成为人类未来能源发展的一个主要方向。利用太阳能为驱动,光催化剂为光电极来降解有机污染物制取氢,将光能、电能进行有机结合,实现了光能和电能到化学能(氢能)的转换,不但解决了严重的环境污染问题而且也为缓解能源危机提供有效途径。
作为该技术的关键,研制出具有光转化效率高的光电催化材料是重要的研究方向。本文利用电化学阳极氧化法成功制备出二氧化钛纳米管(TNT)并对其进行改性。探索了制备的主要影响因素对二氧化钛纳米管结构特征及其光电催化活性的影响。
探索二氧化钛纳米管阵列光电催化产氢性能的影响因素、掺杂改性及其光电催化降解有机污染物同时产氢的应用,并在此基础上对其光电催化降解有机污染物同时产氢的机理进行了初步探索,为开发高效能的二氧化钛纳米管阵列及其复合光催化剂提供了技术支持。主要结果如下：
1.在相同的氧化时间条件下,随着氧化电压(20V、30V、45V、60V)的升高,二氧化钛纳米管的管长、孔径、长径比、粗糙系数、生长速率逐渐增大,管壁厚度逐渐降低。在相同的氧化电压下,随着氧化时间(3h、4h、5h、6h)的延长,二氧化钛纳米管的管长、长径比和粗糙系数逐渐增大,孔径和壁厚基本不变。总之,氧化电压对二氧化钛纳米管阵列的形貌结构特征起着决定性影响,尤其是对其长径比。在氧化电压为60V,氧化时间为6h的条件下制备的二氧化钛纳米管具有最佳的长径比结构特征,其长径比为178,表现出优异的光电催化降解有机污染物同时产氢的性能,其光电流密度和光电催化降解甲基橙的动力学常数分别达到最大,其值分别为48×10-3mA/cm2和2.26×10-3min-1;在外加偏压为0.45V时表现出的最大光电流密度约为0.05mA/cm2。二氧化钛纳米管阵列经450℃煅烧后,其表现出锐钛矿和金红石的混合相；XPS测试表明,其含有一定量的C、N元素,成功实现了C、N元素的原位掺杂。
2.利用两步电化学氧化法制备的二氧化钛纳米管表现出较高的长径比和较薄的管壁厚度,其值分别为104.83和16.36nm,相比于一步阳极氧化制备的二氧化钛纳米管表现出更高的光电催化性能。一步阳极氧化和两步阳极氧化合成的二氧化钛纳米管的光电流密度和及其光-氢转化效率分别为0.2mA/cm2和0.4mA/cm2、0.14%和0.36%。当加入乙二醇作为有机电子供体时,一步阳极氧化和两步阳极氧化合成的二氧化钛纳米管的瞬时光电流密度分别为0.022mA/cm2和0.026mA/cm2。
3.以氧化电压分别为20V、30V、45V,氧化时间为1h的条件下制备二氧化钛纳米管为基体,利用电化学沉积法制备了ZnFe2O4/TiO2纳米管复合光电极,在氧化电压45V、氧化时间1h条件下制备的二氧化钛纳米管表现出最大光-氢转化效率为0.1%,而在氧化电压30V、氧化时间1h条件下制备的二氧化钛纳米管复合光电极znFe2O4/TiO2表现出的最大光-氢转化效率为0.18%。
4.以氧化电压45V、氧化时间5h制备的二氧化钛纳米管为基体,利用提拉-浸渍法合成的Pt/TiO2纳米管复合电极,其光-氢转化效率是YiO2纳米管的2.1倍。甲基橙光电催化降解实验表明,Pt/TNT的光电催化降解速率为TNT的2.7倍,且具有较好的的机械强度和化学稳定性,是一种极具应用潜力的环境友好材料。
5.采用三电极体系,在外加偏压为0.45V时,分别以0.1mol/L的KOH、 Na2SO4、Na2CO3溶液为支持电解质溶液,以0.5mol/L的乙二醇为目标污染物时,以KOH为电解质溶液的光电流密度最大；在pH值分别为2、6.8、10的条件下,以pH值为6.8时光电流最大。光电流密度随着乙二醇浓度的增大而增大。草酸作为目标污染物时的光电流密度最大。
With the rapid development of industrial and urbanization, environmental problems and energy crisis have been becoming increasingly serious. Because hydrogen energy possesses the characteristic with clear, high energy density, better heat conduction, it will become a main direction of energy for people in the near future. Photocatalyst was used as the photoanode to degrade organic pollutants and simultaneously produce hydrogen using solar energy as a drive, and combine optical energy and electrical energy, realize the conversion of optical energy and electrical energy into chemical energy(hydrogen energy), which not only solve serious environment pollution problems, but also provide an effective method to relieve energy cnsis.
As the key of photocatalytic technology, developing the photocatalytic materials with high photoconversion efficiency is the key study direction. Titania nanotube arrays (TNT) were fabricated by anodization method, and they were also modified to improve their photoelectrocatalytic performance. The main factors affecting preparation of TNT on its structural features and photoelectrocatalytic activity were investigated.
Effecting factors of TNT for the photoelectrocatalytic hydrogen generation performance, its modification and application in photoelectrocatalytic degradation of organic pollutants degradation and simultaneous hydrogen generation were also studied, and its mechanism of photoelectrocatalytic degradation organic pollutants and simultaneous hydrogen generation for TNT were preliminarily investigated, and provided a technical support to develop a high efficiency titania nanotube arrays and its multiplex photocatalyst. The main study results were listed as following:
Firstly, under the same conditions of anodization time, the tube length, pore size, aspect ratio, roughness factor, growth rate of TNT increased and the wall thickness decreased with the increase of anodization voltages (20V,30V,45V,60V). Under the same conditions of anodization voltages, the tube length, aspect ratio, roughness factor of TNT increased, and the wall thickness and pore size did not change with the increase of anodization time (3h,4h,5h,6h). In a word, anodization voltages decided the structural features of TNT, especially, it decisively affected the aspect ratio of TNT. TNT fabricated at60V for6h has an optimum aspect ratio, when the aspect ratio was178, TNT exhibited the maximum capacity for the photoelectrocatalytic degradation and simultaneous hydrogen generation. TNT that was annealed at450℃showed the mixture of anatase and rutile, and its XPS test indicated that TNT contained C, N, and successfully the in-situ modification of C, N. The aspect ratio of TNT has a decisive effect on its performance for the photoelectrocatalytic degradation and hydrogen generation. When TNT with the aspect ratio of178showed the maximum degradation kinetic constant of2.26x10-3min-1and the maximum photocurrent density of48×10-3mA/cm2. TNT showed the maximum photocurrent density of0.05mA/cm2under the bias potential of0.45V.
Secondly, TNT fabricated by two-step anodization demonstrated the higher aspect and thin wall thickness, which were104.83and16.36nm. TNT fabricated by two-step anodization showed higher photoelectrocatalytic activity than those prepared by one-step anodization, their photocurrent density and photo-hydrogen conversion efficiency were0.2mA/cm2and0.4mA/cm2,0.14%and0.36%. When ethylene glycol was used as organic electron donor, the photocurrent density of TNT fabricated by two-step anodization and one-step anodization were0.026mA/cm2and0.022mA/cm2.
Thirdly, TNT fabricated by anodization at20V,30V,45V for1h was used to dope ZnFe2O4nanoparticles using electrochemical deposition, and the results indicated that TNT prepared by anodization at45V for1h showed the maximum photo-hydrogen cinversion efficiency of0.18%.
Fourthly, TNT fabricated by anodization at45V for5h was utilized to prepare Pt/TiO2electrode using dipping-pulling method, the results indicate that the uniform dispersion of platinum successfully broadens the absorption spectrum of TiO2nanotube arrays to visible light region and the photocurrent density of Pt/TNT is18times that of TNT. The degradation of methyl orange on Pt/TNT conforms to pseudo first-order kinetics and the reaction rate constant is about3times that of TNT. The photo-hydrogen conversion efficiency of Pt/TiO2photoelectrode is2.1times that of TNT, it also demonstrates the highest mechanical and chemical stability.
Fifth, Using three-electrode system,0.1mol/L KOH, Na2SO4, Na2CO3solution were used as supporting electrolyte solution under the condition of bias potential of0.45V, TNT shows the highest photocurrent density in KOH solution. Na2SO4solution of0.1mol/L was used as supporting electrolyte solution under the condition of bias potential of0.45V, pH was2,6.8,10, TNT exhibits the maximum photocurrent density when pH of Na2SO4solution is6.8. Under the conditions of ethylene glycol of0mol/L,0.1mol/L,0.25mol/L,0.5mol/L, the photocurrent density increases with the increase of concentration of ethylene glycol. At the presence of ethylene glycol and oxalic acid, TNT in the electrolyte of ethylene glycol shows the higher photocurrent density than oxalic acid without the bias potential. And TNT in the electrolyte of oxalic acid demonstrates the higher photocurrent with the increase of the bias potential from0V to0.9V.
作为该技术的关键,研制出具有光转化效率高的光电催化材料是重要的研究方向。本文利用电化学阳极氧化法成功制备出二氧化钛纳米管(TNT)并对其进行改性。探索了制备的主要影响因素对二氧化钛纳米管结构特征及其光电催化活性的影响。
探索二氧化钛纳米管阵列光电催化产氢性能的影响因素、掺杂改性及其光电催化降解有机污染物同时产氢的应用,并在此基础上对其光电催化降解有机污染物同时产氢的机理进行了初步探索,为开发高效能的二氧化钛纳米管阵列及其复合光催化剂提供了技术支持。主要结果如下：
1.在相同的氧化时间条件下,随着氧化电压(20V、30V、45V、60V)的升高,二氧化钛纳米管的管长、孔径、长径比、粗糙系数、生长速率逐渐增大,管壁厚度逐渐降低。在相同的氧化电压下,随着氧化时间(3h、4h、5h、6h)的延长,二氧化钛纳米管的管长、长径比和粗糙系数逐渐增大,孔径和壁厚基本不变。总之,氧化电压对二氧化钛纳米管阵列的形貌结构特征起着决定性影响,尤其是对其长径比。在氧化电压为60V,氧化时间为6h的条件下制备的二氧化钛纳米管具有最佳的长径比结构特征,其长径比为178,表现出优异的光电催化降解有机污染物同时产氢的性能,其光电流密度和光电催化降解甲基橙的动力学常数分别达到最大,其值分别为48×10-3mA/cm2和2.26×10-3min-1;在外加偏压为0.45V时表现出的最大光电流密度约为0.05mA/cm2。二氧化钛纳米管阵列经450℃煅烧后,其表现出锐钛矿和金红石的混合相；XPS测试表明,其含有一定量的C、N元素,成功实现了C、N元素的原位掺杂。
2.利用两步电化学氧化法制备的二氧化钛纳米管表现出较高的长径比和较薄的管壁厚度,其值分别为104.83和16.36nm,相比于一步阳极氧化制备的二氧化钛纳米管表现出更高的光电催化性能。一步阳极氧化和两步阳极氧化合成的二氧化钛纳米管的光电流密度和及其光-氢转化效率分别为0.2mA/cm2和0.4mA/cm2、0.14%和0.36%。当加入乙二醇作为有机电子供体时,一步阳极氧化和两步阳极氧化合成的二氧化钛纳米管的瞬时光电流密度分别为0.022mA/cm2和0.026mA/cm2。
3.以氧化电压分别为20V、30V、45V,氧化时间为1h的条件下制备二氧化钛纳米管为基体,利用电化学沉积法制备了ZnFe2O4/TiO2纳米管复合光电极,在氧化电压45V、氧化时间1h条件下制备的二氧化钛纳米管表现出最大光-氢转化效率为0.1%,而在氧化电压30V、氧化时间1h条件下制备的二氧化钛纳米管复合光电极znFe2O4/TiO2表现出的最大光-氢转化效率为0.18%。
4.以氧化电压45V、氧化时间5h制备的二氧化钛纳米管为基体,利用提拉-浸渍法合成的Pt/TiO2纳米管复合电极,其光-氢转化效率是YiO2纳米管的2.1倍。甲基橙光电催化降解实验表明,Pt/TNT的光电催化降解速率为TNT的2.7倍,且具有较好的的机械强度和化学稳定性,是一种极具应用潜力的环境友好材料。
5.采用三电极体系,在外加偏压为0.45V时,分别以0.1mol/L的KOH、 Na2SO4、Na2CO3溶液为支持电解质溶液,以0.5mol/L的乙二醇为目标污染物时,以KOH为电解质溶液的光电流密度最大；在pH值分别为2、6.8、10的条件下,以pH值为6.8时光电流最大。光电流密度随着乙二醇浓度的增大而增大。草酸作为目标污染物时的光电流密度最大。
With the rapid development of industrial and urbanization, environmental problems and energy crisis have been becoming increasingly serious. Because hydrogen energy possesses the characteristic with clear, high energy density, better heat conduction, it will become a main direction of energy for people in the near future. Photocatalyst was used as the photoanode to degrade organic pollutants and simultaneously produce hydrogen using solar energy as a drive, and combine optical energy and electrical energy, realize the conversion of optical energy and electrical energy into chemical energy(hydrogen energy), which not only solve serious environment pollution problems, but also provide an effective method to relieve energy cnsis.
As the key of photocatalytic technology, developing the photocatalytic materials with high photoconversion efficiency is the key study direction. Titania nanotube arrays (TNT) were fabricated by anodization method, and they were also modified to improve their photoelectrocatalytic performance. The main factors affecting preparation of TNT on its structural features and photoelectrocatalytic activity were investigated.
Effecting factors of TNT for the photoelectrocatalytic hydrogen generation performance, its modification and application in photoelectrocatalytic degradation of organic pollutants degradation and simultaneous hydrogen generation were also studied, and its mechanism of photoelectrocatalytic degradation organic pollutants and simultaneous hydrogen generation for TNT were preliminarily investigated, and provided a technical support to develop a high efficiency titania nanotube arrays and its multiplex photocatalyst. The main study results were listed as following:
Firstly, under the same conditions of anodization time, the tube length, pore size, aspect ratio, roughness factor, growth rate of TNT increased and the wall thickness decreased with the increase of anodization voltages (20V,30V,45V,60V). Under the same conditions of anodization voltages, the tube length, aspect ratio, roughness factor of TNT increased, and the wall thickness and pore size did not change with the increase of anodization time (3h,4h,5h,6h). In a word, anodization voltages decided the structural features of TNT, especially, it decisively affected the aspect ratio of TNT. TNT fabricated at60V for6h has an optimum aspect ratio, when the aspect ratio was178, TNT exhibited the maximum capacity for the photoelectrocatalytic degradation and simultaneous hydrogen generation. TNT that was annealed at450℃showed the mixture of anatase and rutile, and its XPS test indicated that TNT contained C, N, and successfully the in-situ modification of C, N. The aspect ratio of TNT has a decisive effect on its performance for the photoelectrocatalytic degradation and hydrogen generation. When TNT with the aspect ratio of178showed the maximum degradation kinetic constant of2.26x10-3min-1and the maximum photocurrent density of48×10-3mA/cm2. TNT showed the maximum photocurrent density of0.05mA/cm2under the bias potential of0.45V.
Secondly, TNT fabricated by two-step anodization demonstrated the higher aspect and thin wall thickness, which were104.83and16.36nm. TNT fabricated by two-step anodization showed higher photoelectrocatalytic activity than those prepared by one-step anodization, their photocurrent density and photo-hydrogen conversion efficiency were0.2mA/cm2and0.4mA/cm2,0.14%and0.36%. When ethylene glycol was used as organic electron donor, the photocurrent density of TNT fabricated by two-step anodization and one-step anodization were0.026mA/cm2and0.022mA/cm2.
Thirdly, TNT fabricated by anodization at20V,30V,45V for1h was used to dope ZnFe2O4nanoparticles using electrochemical deposition, and the results indicated that TNT prepared by anodization at45V for1h showed the maximum photo-hydrogen cinversion efficiency of0.18%.
Fourthly, TNT fabricated by anodization at45V for5h was utilized to prepare Pt/TiO2electrode using dipping-pulling method, the results indicate that the uniform dispersion of platinum successfully broadens the absorption spectrum of TiO2nanotube arrays to visible light region and the photocurrent density of Pt/TNT is18times that of TNT. The degradation of methyl orange on Pt/TNT conforms to pseudo first-order kinetics and the reaction rate constant is about3times that of TNT. The photo-hydrogen conversion efficiency of Pt/TiO2photoelectrode is2.1times that of TNT, it also demonstrates the highest mechanical and chemical stability.
Fifth, Using three-electrode system,0.1mol/L KOH, Na2SO4, Na2CO3solution were used as supporting electrolyte solution under the condition of bias potential of0.45V, TNT shows the highest photocurrent density in KOH solution. Na2SO4solution of0.1mol/L was used as supporting electrolyte solution under the condition of bias potential of0.45V, pH was2,6.8,10, TNT exhibits the maximum photocurrent density when pH of Na2SO4solution is6.8. Under the conditions of ethylene glycol of0mol/L,0.1mol/L,0.25mol/L,0.5mol/L, the photocurrent density increases with the increase of concentration of ethylene glycol. At the presence of ethylene glycol and oxalic acid, TNT in the electrolyte of ethylene glycol shows the higher photocurrent density than oxalic acid without the bias potential. And TNT in the electrolyte of oxalic acid demonstrates the higher photocurrent with the increase of the bias potential from0V to0.9V.
引文
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