改性TiO_2纳米管阵列光阳极裂解水制氢的性能研究
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摘要
氢能源是未来的清洁能源之一,光电催化裂解水制氢是清洁、节能和经济可行的方法,该方法将太阳能通过光电化学转化为可贮存的氢能,其中催化剂光电极的研制是最关键的技术。目前光电催化裂解水催化剂的缺点首先是可见光光响应低,不能有效利用太阳光,其次是导带电位较正,光激发到导带的电子不足以还原水生成氢气,这需要对催化剂进行改性,来满足上述要求,提高光电催化产氢效率。
本文研究合适的金属及其氧化物半导体共同改性TiO2纳米管阵列,形成复合光催化剂,更好地改善TiO2纳米管阵列光催化剂的性能,此种光电极的制备、光电性质及其光电催化分解水产氢机理研究未见报道。本实验使用SEM、XRD和XPS表面分析方法研究了纳米管阵列及改性后纳米管的表面形貌和晶相组成,采用半导体光电流响应分析及电子结构分析方法研究了改性物质对TiO2纳米管阵列光电响应的作用结果,同时结合容抗分析(Mott-Schottky曲线和电化学阻抗谱EIS)研究改性TiO2纳米管阵列半导体特性和半导体/溶液界面的电荷传递动力学。
首先在含F-的乙二醇有机溶液中阳极氧化6h制备的TiO2纳米管阵列,经过450℃焙烧后呈锐钛矿晶型,表面和纵向分布整齐规则,光电响应最强；同时与纳米TiO2薄膜对比,TiO2纳米管阵列吸收光红移,最高光电流是纳米TiO2薄膜的4倍。
采用阴极还原和阳极氧化法制备过渡金属Ce及其氧化物(Ce2O3/CeO2)改性TiO2纳米管阵列。在10×10-3mo1/L硝酸铈乙醇溶液中制备的还原态铈和氧化态铈两种改性试样光催化效果最好,在此条件下,还原态铈以单质Ce和Ce2O3纳米线形式存在于TiO2纳米管阵列表面及管内,对比TiO2纳米管阵列,经还原态铈改性的TiO2纳米管阵列在可见光区光电响应增强,紫外光区光电响应减弱,平带电位向电负方向移动,同时改性TiO2纳米管阵列能带宽度减小至2.88eV；还原态铈经阳极氧化后,氧化态铈以单质Ce、Ce2O3和CeO2结晶态存在于TiO2纳米管阵列表面及管内,对比TiO2纳米管阵列,氧化态铈改性的TiO2纳米管阵列在可见光区和紫外光区光电响应都增强,平带电位向电负方向移动；随着氧化的不断深入,改性TiO2纳米管阵列在可见光区光电响应随之增强。同时光电流对光子能量谱分析发现,在还原态铈和氧化态铈中都存在能带宽度为Eg=2.4eV的氧化相Ce2O3。
通过电化学阻抗谱研究发现,在阳极电解液中添加供电子物质减小了光生载流子传递阻抗,其中添加有机物乙二醇效果最佳。经氧化态铈改性后的TiO2纳米管阵列,由于电极表面增加了新的界面而导致一个新的容抗圆弧,但改性减小了TiO2纳米管阵列空间电荷层阻抗,说明单质铈和氧化铈有助于提高TiO2纳米管阵列的电子传输性能,增加偏压主要有利于减小TiO2纳米管层的电荷传递阻抗。根据光电响应特性和电化学阻抗谱特点,讨论了氧化铈和单质铈加强TiO2纳米管阵列在可见和紫外光区光电流响应与促进光生载流子传输的机理：窄能带宽度半导体Ce2O3(Eg=2.4eV)和宽能带宽度半导体CeO2(Eg=3.16eV)分别加强TiO2纳米管阵列在可见光区和紫外光区的光电响应,同时这两种氧化铈导带电位负于TiO2纳米管的导带电位,有利于光生电子向TiO2导带移动,进而到达对电极裂解水产氢；单质铈一方面作为杂质能级位于TiO2的禁带之中,有利于光生电子和空穴的分离,促进可见光光电响应,另一方面可能单质铈掺杂进入TiO2晶格中,与Ti的3d轨道形成混合导带使其禁带宽度变窄,增加了对可见光的吸收。
铈及其氧化物改性有助于提高TiO2纳米管阵列的产氢光电转换效率,在水溶液中无外加偏压条件下,在450W氙灯光照反应5h期间,TiO2NTs电极无氢气生成,而单质铈和氧化铈共同改性的TiO2NTs-Ce-CeOx有0.092mL/h·cm2氢气生成。在阳极电解液中添加乙二醇后,TiO2NTs-Ce-CeOx的最高产氢光电转换效率为5.9%,是TiO2NTs的1.76倍,在0.4V偏压条件下,TiO2NTs-Ce-CeOx的平均产氢量为2.38mL/h·cm2;在大于370nm波长光照下,TiO2NTs-Ce-CeOx最高产氢光电转换效率为4.43%,是TiO2NTs的1.92倍,在0.4V偏压条件下,TiO2NTs-Ce-CeOx的平均产氢量为1.39mL/h·cm2。
金属铅及其氧化物改性有助于TiO2纳米管阵列的平带电位向电负方向移动,但降低了光电流响应；金属铜或铟及其氧化物改性有助于提高TiO2纳米管阵列在紫外和可见光区的光电流响应,但是平带电位都向正向移动,都不利于光电催化裂解水产氢。
Hydrogen is one of the clean energy in future. The hydrogen production from photoelectrocatalytic water spliting which transfers solar to hydrogen energy by photoelectrochemical cell is the cleanest, low energy and economical feasible technology, the preparation of catalyst photoelectrode is the key role of this work. At present, the shortcomings of catalyst for photoelectrocatalytic water spliting maily include two aspects. Firstly the low visible light response cannot effectively use the sunlight. Secondly the light electron from valence band exciting into the conduction band is not sufficient to split water molecular to generate hydrogen as the positive conduction band potential. So the catalyst needs modification to meet the above requirements, and increase photoconversion efficiency of hydrogen generation.
In this work, the TiO2nanotube arrays were modified by an appropriate metal and its oxide as semiconductor to improve the performance in water splitting hydrogen production. According to our knowledge, such photoelectrode preparation in photoelectrocatalytic splitting water to hydrogen production investigation has not been reported. The surface morphology and crystal phase of the modified TiO2nanotube arrays were analysised by SEM, XRD and XPS. The modified substances effect on TiO2nanotube arrays photoresponse were studied by semiconductor photocurrent response and electronic structure analysis. And the semiconductor characteristics and charge transfer kinetics on the TiO2nanotube arrays semiconductor/solution interface vere investigated by capacitance analysis of Mott-Schottky curves and electrochemistry impedance spectrum(EIS).
The optimal TiO2nanotube arrays(TiO2NTs) prepared by anodic oxidation6h in the glycol solution containing F", showed well-ordered surface and profile as anatase after calcination at450℃and indicated the highest photocurrent response. This sample absorbed light redshift and its photocurrent improved four times than that of TiO2thin film.
Reductive Cerium and oxidative Cerium were deposited on the TiO2nanotube arrays by electrochemical cathodic reduction and then anodic oxidation. The sample(TiO2NTs-Ce-CeOx) prepared in the10mmol/L cerium nitrate solution suggested an optimal deposition quantity. In this condition, the reductive Cerium was in the form of elementary Cerium and Ce2O3nanofibers dispersed both on the surface and inside of TiO2nanotubes. Compared with TiO2nanotubes without modification, reductive Cerium modification lowered the original bandgap energy from3.15eV to2.88eV and enhanced photocurrent response in visible spectra rather than in UV spectra. The flat band potentials also moved to negative direction. After anodic oxidation, the oxidative Cerium was in the form of elementary Cerium, Ce2O3and CeO2dispersed both on the surface and inside of TiO2nanotube. Comparred with TiO2nanotube, the photocurrent response of the sample was enhanced in visible spectra and in UV spectra region and the flat potentials moved to negative direction. As the anodic oxidation in depth, the photocurrent responses increased in visible light. The study of photocurrent on photon energy indicated that there was a band gap energy of2.4eV as Ce2O3oxidation phase in the reductive Cerium and oxidative Cerium.
The donor materials adding in the anode electrolyte significantly reduced the charge transfer impedance of TiO2nanotube to promote the photocatalytic spitting water for production hydrogen by EIS with adding organic glycol(C2H6O2) optimum. Although the oxidative Cerium modified TiO2nanotube arrays had a new capacitace arc by EIS as the TiO2nanotube arrays electrode surface increased the new interface, while reduced the space charge layer impedance of TiO2nanotube arrays. This indicated the elemental cerium and cerium oxide work to improve the electron transmission performance of TiO2nanotube arrays. The bias potential on working electrode reduces charge transfer impedance on TiO2nanotube layer. The mechanism of the Cerium and oxidative Cerium acting on TiO2nanotube arrays to improve photocurrent response and reduce charge transfer was discussed. The narrow bandgap semiconductor Ce2O3(Eg=2.4eV)and wide bandgap semiconductor CeO2(Eg=3.16eV) respectively enhanced the photocurrent responces of TiO2nanotube arrays in the visible and UV region. And two cerium oxides had negative conduction band potential than TiO2, which contributed that photoinduced electrons move to the conduction band of TiO2and then reach the counter electrode to split water for hydrogen production; On the one hand, elemental cerium as the impurity levels in the band gap of TiO2was conducive to the separation of photo-generated electrons and holes, and promote visible light photoresponce. On the other hand, elemental cerium was doped into TiO2crystal lattice to form a mixed conduction band with Ti3d. This new conduction band narrowed the energy bandgap to promote the absorption of visible light.
Cerium and oxidative Cerium increased TiO2nanotube arrays photoconversion efficiency for splitting water. In water TiO2NTs-Ce-CeOx photoelectrode without bias resulted in stable and consistent hydrogen generation throughout the5h reaction and the average hydrogen generation rate was0.092mL/h·cm2, but TiO2NTs photoelectrode without hydrogen generation. After adding C2H6O2in anode electrolyte, this optimized TiO2NTs-Ce-CeOx photoelectrode was found to split water with maximum photoconversion efficiency of5.9%under white light illumination, which was1.76times that of TiO2NTs and the average hydrogen generation rate was2.38mL/h·cm2with0.4V bias. In above370nm wavelength light illumination, TiO2NTs-Ce-CeOx photoelectrode was found to split water with maximum photoconversion efficiency of4.43%, which was1.92times that of TiO2NTs and the average hydrogen generation rate was1.39mL/h·cm2with0.4V bias.
Very experiments were taken out in different metal and its oxide as method discussed above. The flat band potentials of TiO2NTs modified by Lead(Pb) and its oxides moved to the negative direction while its photocurrent responses in visible spectra and UV spectra reduced by modification. As a contrast, the photocurrent responses of TiO2NTs modified by In or Cu, respectively, improved in visible spectra and UV spectra, while their flat band potentials moved to the positive direction, which played a negative effect in photoelectrocatalytic splitting water for hydrogen production.
本文研究合适的金属及其氧化物半导体共同改性TiO2纳米管阵列,形成复合光催化剂,更好地改善TiO2纳米管阵列光催化剂的性能,此种光电极的制备、光电性质及其光电催化分解水产氢机理研究未见报道。本实验使用SEM、XRD和XPS表面分析方法研究了纳米管阵列及改性后纳米管的表面形貌和晶相组成,采用半导体光电流响应分析及电子结构分析方法研究了改性物质对TiO2纳米管阵列光电响应的作用结果,同时结合容抗分析(Mott-Schottky曲线和电化学阻抗谱EIS)研究改性TiO2纳米管阵列半导体特性和半导体/溶液界面的电荷传递动力学。
首先在含F-的乙二醇有机溶液中阳极氧化6h制备的TiO2纳米管阵列,经过450℃焙烧后呈锐钛矿晶型,表面和纵向分布整齐规则,光电响应最强；同时与纳米TiO2薄膜对比,TiO2纳米管阵列吸收光红移,最高光电流是纳米TiO2薄膜的4倍。
采用阴极还原和阳极氧化法制备过渡金属Ce及其氧化物(Ce2O3/CeO2)改性TiO2纳米管阵列。在10×10-3mo1/L硝酸铈乙醇溶液中制备的还原态铈和氧化态铈两种改性试样光催化效果最好,在此条件下,还原态铈以单质Ce和Ce2O3纳米线形式存在于TiO2纳米管阵列表面及管内,对比TiO2纳米管阵列,经还原态铈改性的TiO2纳米管阵列在可见光区光电响应增强,紫外光区光电响应减弱,平带电位向电负方向移动,同时改性TiO2纳米管阵列能带宽度减小至2.88eV；还原态铈经阳极氧化后,氧化态铈以单质Ce、Ce2O3和CeO2结晶态存在于TiO2纳米管阵列表面及管内,对比TiO2纳米管阵列,氧化态铈改性的TiO2纳米管阵列在可见光区和紫外光区光电响应都增强,平带电位向电负方向移动；随着氧化的不断深入,改性TiO2纳米管阵列在可见光区光电响应随之增强。同时光电流对光子能量谱分析发现,在还原态铈和氧化态铈中都存在能带宽度为Eg=2.4eV的氧化相Ce2O3。
通过电化学阻抗谱研究发现,在阳极电解液中添加供电子物质减小了光生载流子传递阻抗,其中添加有机物乙二醇效果最佳。经氧化态铈改性后的TiO2纳米管阵列,由于电极表面增加了新的界面而导致一个新的容抗圆弧,但改性减小了TiO2纳米管阵列空间电荷层阻抗,说明单质铈和氧化铈有助于提高TiO2纳米管阵列的电子传输性能,增加偏压主要有利于减小TiO2纳米管层的电荷传递阻抗。根据光电响应特性和电化学阻抗谱特点,讨论了氧化铈和单质铈加强TiO2纳米管阵列在可见和紫外光区光电流响应与促进光生载流子传输的机理：窄能带宽度半导体Ce2O3(Eg=2.4eV)和宽能带宽度半导体CeO2(Eg=3.16eV)分别加强TiO2纳米管阵列在可见光区和紫外光区的光电响应,同时这两种氧化铈导带电位负于TiO2纳米管的导带电位,有利于光生电子向TiO2导带移动,进而到达对电极裂解水产氢；单质铈一方面作为杂质能级位于TiO2的禁带之中,有利于光生电子和空穴的分离,促进可见光光电响应,另一方面可能单质铈掺杂进入TiO2晶格中,与Ti的3d轨道形成混合导带使其禁带宽度变窄,增加了对可见光的吸收。
铈及其氧化物改性有助于提高TiO2纳米管阵列的产氢光电转换效率,在水溶液中无外加偏压条件下,在450W氙灯光照反应5h期间,TiO2NTs电极无氢气生成,而单质铈和氧化铈共同改性的TiO2NTs-Ce-CeOx有0.092mL/h·cm2氢气生成。在阳极电解液中添加乙二醇后,TiO2NTs-Ce-CeOx的最高产氢光电转换效率为5.9%,是TiO2NTs的1.76倍,在0.4V偏压条件下,TiO2NTs-Ce-CeOx的平均产氢量为2.38mL/h·cm2;在大于370nm波长光照下,TiO2NTs-Ce-CeOx最高产氢光电转换效率为4.43%,是TiO2NTs的1.92倍,在0.4V偏压条件下,TiO2NTs-Ce-CeOx的平均产氢量为1.39mL/h·cm2。
金属铅及其氧化物改性有助于TiO2纳米管阵列的平带电位向电负方向移动,但降低了光电流响应；金属铜或铟及其氧化物改性有助于提高TiO2纳米管阵列在紫外和可见光区的光电流响应,但是平带电位都向正向移动,都不利于光电催化裂解水产氢。
Hydrogen is one of the clean energy in future. The hydrogen production from photoelectrocatalytic water spliting which transfers solar to hydrogen energy by photoelectrochemical cell is the cleanest, low energy and economical feasible technology, the preparation of catalyst photoelectrode is the key role of this work. At present, the shortcomings of catalyst for photoelectrocatalytic water spliting maily include two aspects. Firstly the low visible light response cannot effectively use the sunlight. Secondly the light electron from valence band exciting into the conduction band is not sufficient to split water molecular to generate hydrogen as the positive conduction band potential. So the catalyst needs modification to meet the above requirements, and increase photoconversion efficiency of hydrogen generation.
In this work, the TiO2nanotube arrays were modified by an appropriate metal and its oxide as semiconductor to improve the performance in water splitting hydrogen production. According to our knowledge, such photoelectrode preparation in photoelectrocatalytic splitting water to hydrogen production investigation has not been reported. The surface morphology and crystal phase of the modified TiO2nanotube arrays were analysised by SEM, XRD and XPS. The modified substances effect on TiO2nanotube arrays photoresponse were studied by semiconductor photocurrent response and electronic structure analysis. And the semiconductor characteristics and charge transfer kinetics on the TiO2nanotube arrays semiconductor/solution interface vere investigated by capacitance analysis of Mott-Schottky curves and electrochemistry impedance spectrum(EIS).
The optimal TiO2nanotube arrays(TiO2NTs) prepared by anodic oxidation6h in the glycol solution containing F", showed well-ordered surface and profile as anatase after calcination at450℃and indicated the highest photocurrent response. This sample absorbed light redshift and its photocurrent improved four times than that of TiO2thin film.
Reductive Cerium and oxidative Cerium were deposited on the TiO2nanotube arrays by electrochemical cathodic reduction and then anodic oxidation. The sample(TiO2NTs-Ce-CeOx) prepared in the10mmol/L cerium nitrate solution suggested an optimal deposition quantity. In this condition, the reductive Cerium was in the form of elementary Cerium and Ce2O3nanofibers dispersed both on the surface and inside of TiO2nanotubes. Compared with TiO2nanotubes without modification, reductive Cerium modification lowered the original bandgap energy from3.15eV to2.88eV and enhanced photocurrent response in visible spectra rather than in UV spectra. The flat band potentials also moved to negative direction. After anodic oxidation, the oxidative Cerium was in the form of elementary Cerium, Ce2O3and CeO2dispersed both on the surface and inside of TiO2nanotube. Comparred with TiO2nanotube, the photocurrent response of the sample was enhanced in visible spectra and in UV spectra region and the flat potentials moved to negative direction. As the anodic oxidation in depth, the photocurrent responses increased in visible light. The study of photocurrent on photon energy indicated that there was a band gap energy of2.4eV as Ce2O3oxidation phase in the reductive Cerium and oxidative Cerium.
The donor materials adding in the anode electrolyte significantly reduced the charge transfer impedance of TiO2nanotube to promote the photocatalytic spitting water for production hydrogen by EIS with adding organic glycol(C2H6O2) optimum. Although the oxidative Cerium modified TiO2nanotube arrays had a new capacitace arc by EIS as the TiO2nanotube arrays electrode surface increased the new interface, while reduced the space charge layer impedance of TiO2nanotube arrays. This indicated the elemental cerium and cerium oxide work to improve the electron transmission performance of TiO2nanotube arrays. The bias potential on working electrode reduces charge transfer impedance on TiO2nanotube layer. The mechanism of the Cerium and oxidative Cerium acting on TiO2nanotube arrays to improve photocurrent response and reduce charge transfer was discussed. The narrow bandgap semiconductor Ce2O3(Eg=2.4eV)and wide bandgap semiconductor CeO2(Eg=3.16eV) respectively enhanced the photocurrent responces of TiO2nanotube arrays in the visible and UV region. And two cerium oxides had negative conduction band potential than TiO2, which contributed that photoinduced electrons move to the conduction band of TiO2and then reach the counter electrode to split water for hydrogen production; On the one hand, elemental cerium as the impurity levels in the band gap of TiO2was conducive to the separation of photo-generated electrons and holes, and promote visible light photoresponce. On the other hand, elemental cerium was doped into TiO2crystal lattice to form a mixed conduction band with Ti3d. This new conduction band narrowed the energy bandgap to promote the absorption of visible light.
Cerium and oxidative Cerium increased TiO2nanotube arrays photoconversion efficiency for splitting water. In water TiO2NTs-Ce-CeOx photoelectrode without bias resulted in stable and consistent hydrogen generation throughout the5h reaction and the average hydrogen generation rate was0.092mL/h·cm2, but TiO2NTs photoelectrode without hydrogen generation. After adding C2H6O2in anode electrolyte, this optimized TiO2NTs-Ce-CeOx photoelectrode was found to split water with maximum photoconversion efficiency of5.9%under white light illumination, which was1.76times that of TiO2NTs and the average hydrogen generation rate was2.38mL/h·cm2with0.4V bias. In above370nm wavelength light illumination, TiO2NTs-Ce-CeOx photoelectrode was found to split water with maximum photoconversion efficiency of4.43%, which was1.92times that of TiO2NTs and the average hydrogen generation rate was1.39mL/h·cm2with0.4V bias.
Very experiments were taken out in different metal and its oxide as method discussed above. The flat band potentials of TiO2NTs modified by Lead(Pb) and its oxides moved to the negative direction while its photocurrent responses in visible spectra and UV spectra reduced by modification. As a contrast, the photocurrent responses of TiO2NTs modified by In or Cu, respectively, improved in visible spectra and UV spectra, while their flat band potentials moved to the positive direction, which played a negative effect in photoelectrocatalytic splitting water for hydrogen production.
引文
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