改性TiO_2光电复合材料制备及电荷输运特性
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摘要
近年来,半导体光催化氧化技术由于氧化能力强、耗能低、降解速度快、无二次污染、反应条件温和、应用范围广等优点而引起人们的广泛关注。但是由于存在半导体自身量子效率和太阳光利用率较低等不足,以及对应用基础理论知识如光催化剂结构与活性的关系、活性与界面电荷转移的关系、光催化剂改性机制等目前也不是十分清楚,在一定程度上限制了半导体光催化氧化技术的实用化进程。为了提高纳米TiO2在可见光区的光催化活性,能够充分利用太阳光,必须对其进行改性、修饰。本文试图通过贵金属Ag修饰、与ABO3型光催化剂复合等方法进一步改善TiO2光催化剂的性能,并重点揭示新型纳米结构材料表面界面光生电荷转移机制及其对光催化性能的影响规律。
利用溶胶-水热和溶胶-凝胶方法制备了TiO2纳米粒子,对样品进行表征并考察了样品的光催化活性。结果表明,具有和P25相似相组成的T550样品的SPS响应较强说明了此样品的光生电荷分离效率高,并且在405 nm还有一个较强的由表面态跃迁引起的SPS峰,显著地提高了可见光的光催化活性。
利用溶胶-水热法合成了TiO2水热粒子,同时在溶胶形成过程中引入了适量的DBS基团,并进一步通过旋涂法制备了不同的TiO2纳米粒子薄膜。重点考察了添加DBS基团对薄膜表面微观结构、光催化活性和润湿性能的影响,以及内在关系。结果表明:添加DBS使薄膜上的TiO2纳米粒子发生团聚而形成微米级的团簇,虽然减小了膜的有效表面积,使光催化活性降低,但改变了纳米TiO2薄膜的表面微结构,纳米-微米的复合结构使其具有很好的亲水性。添加DBS基团虽然降低了TiO2粒子膜的光催化活性,但是却显著提高了薄膜的亲水性能,甚至达到超亲水性,这主要与薄膜表面由TiO2纳米粒子所形成的微米级隆起有关。说明薄膜表面微观结构能够强烈影响材料的光催化和润湿性能。
半导体表面沉积贵金属被认为是可以捕获光生电子的有效改性方法之一,可以进一步提高半导体光催化剂的活性。以贵金属Ag为代表,对纳米TiO2薄膜进行了改性。主要考察了不同Ag沉积量对TiO2结构和性能等的影响,重点研究了贵金属Ag沉积对纳米TiO2薄膜光生载流子的分离以及光催化性能的影响。结果表明:适量Ag的沉积有利于TiO2薄膜中光生载流子的分离,从而减少电子-空穴的复合几率,进而提高纳米TiO2薄膜的光催化活性。硝酸银溶液的最佳浓度为1×10-3 mol·L-1。此外,沉积贵金属Ag的TiO2薄膜具有良好的光催化循环性能。
LaFeO3由于其独特的晶体结构和优良的性能,近年来在催化等领域显示了较好的应用前景。采用柠檬酸络合法制备了LaFeO3纳米粒子,并利用现代测试技术对样品进行了表征,重点考察了LaFeO3纳米粒子的最佳制备条件及其在可见光下光催化氧化罗丹明B的催化性能。结果表明:随着焙烧温度的升高,粒子尺寸逐渐增大,表面光电压谱(SPS)信号逐渐增强。在光催化实验中,500℃焙烧的LaFeO3纳米粒子表现出较高的光催化活性,随着焙烧温度的升高,样品的光催化活性降低,这与表面光电压谱(SPS)的表征结果是相符合的。样品的尺寸越大,能带弯曲越大,自建电场越强,所以其表面光电压信号增强。样品的尺寸越大,光生载流子从粒子内部到达表面的迁移时间越长,这样使光生载流子在复合前到达半导体表面的数目减少,以至于被捕获的机会减少,进而引发氧化还原反应的几率减小,使其光催化活性降低。此外,与比表面积也有关。随着焙烧温度的升高,粒子尺寸越大,比表面积越小,小的比表面积不利于光催化反应的进行,使其光催化活性降低。
柠檬酸络合法是一种经常被采用的合成方法,但是所制备的样品易团聚、粒径大、比表面积小,以至于在应用中存在许多不足,因此探索新的合成方法是非常有必要的。以SBA-16中孔分子筛为硬模板合成了纳米LaFeO3,利用N2气吸附-脱附和SPS等现代测试技术对样品进行了表征,并利用可见光下光催化降解亚甲基蓝为模型反应对样品的光催化性能进行评价。同时,对模板法与柠檬酸法合成的纳米LaFeO3进行了比较研究。结果表明,利用模板法制得的LaFeO3纳米粒子具有多孔结构,而且在高温条件下可以得到比表面积较大的纳米LaFeO3,其在可见光下的光催化性能与柠檬酸络合法制备的LaFeO3相比有很大的提高。
考虑到TiO2是一种紫外光光催化剂,而LaFeO3是一种可见光光催化剂。若将二者进行复合,在光谱吸收方面将会产生互补,进而会提高对太阳光的利用率。也可能会发生耦合作用或者发生载流子的注入过程,进而导致光生电荷的有效分离,以至于提高光量子效率。在前期研究工作基础上,构建了一系列的TiO2-LaFeO3的纳米复合膜,并利用PL和SPS等测试技术深入地揭示和探讨界面电荷转移行为及其机制,同时以光催化降解亚甲基蓝为模型反应对样品的光催化性能进行评价。结果表明,复合膜的光催化活性明显优于单一组成膜的光催化活性。LaFeO3/TiO2纳米复合膜光催化活性的提高是由于LaFeO3与TiO2之间发生了耦合作用,而TiO2/LaFeO3膜光催化活性的提高是因为发生了光生电荷从TiO2向LaFeO3的注入过程,进而促进了光生电荷的有效分离。
本论文能够使纳米半导体材料的基础理论知识得以丰富,从而有效地推动纳米材料在光催化领域的实用化进程。也将为半导体材料在其它领域的应用如光电转换及光诱导合成等提供理论依据。
In recent years, semiconductor photocatalytic oxidation technology has attracted widely attentions mainly due to its characteristics such as strong oxidation capability, low energy consumption, moderate reaction conditions, quick degrading speed, no-secondly pollution and large application range, and is a new promising practical technology for degrading environmental pollutions. However, the practical application step of the semiconductor photocatalytic oxidation technology is held back to a certain extent by the some shortcoming like the low quantum efficiency of semiconductor material in itself and the lower efficiency for utilizing the solar light. Moreover, the involving the photocatalytic reaction, the relationships between structure and activity, the relationships between activity and interface-charge transferring, the modification mechanism, are not well understood up to date. These problems are needed to solve.In order to improve the photocatalytic activity under visible light and make full use of the solar light, the nano-sized titanium dioxide must be modified. With these in mind, the main purpose of the paper is to prepare nano-sized TiO2 modified with noble metal Ag and ABO3-type perovskite photocatalyst and improve the photocatalytic activity under visible light, and the interface-charge transferring mechanism and the photocatalytic activity of composite film photocatalysts were also principally investigated.
TiO2 nanoparticles were prepared by a sol-hydrothermal process and by a sol-gel method and were characterized by several testing techniques. The photocatalytic activity was principally investigated. The results show that the stronger SPS response of T550 attributes to the efficient photoinduced electron transferring, the surface states related to oxygen vacancies can induce photocatalytic reactions under visible irradiation, especially in the resulting biphasic TiO2 due to the electron transfer from anatase surface states to rutile.
Nanosized anatase TiO2 film on the ITO glass has been fabricated via spin coat process, with sodium dodecylbenzenesulfonate modified TiO2 nanoparticles, which is synthesized by a sol-hydrothermal method, and also characterized mainly by means of several testing techniques. It can be suggested that the superhydrophilic performance is mainly attributed to the high roughness resulting from hierarchical surface structure. The formation of characteristic surface structure is close related to the DBS addition. This will be useful to fabricate other newly nanostructured semiconductor film materials, and promote the practical application in the wetting areas of TiO2 films.
Noble metal depositing has been considered as an effective method to hinder the photogenerated electron/hole pair recombination and accelerate the photoexcitation and formation of oxidizing species, consequently to enhance the photocatalytic activity. TiO2 nanoparticles and TiO2 film were prepared by a sol-hydrothermal process, and were characterized by several testing techniques. The photocatalytic activity for degrading Rhodamine B was principally investigated. Nano-sized TiO2 film deposited with the noble metal Ag was prepared by the sol-gel method. The influences of different Ag content on the TiO2 structure and properties were studied and the effect of Ag-depositing on photo-induced charge separation and photocatalytic activity were principally investigated. The results show that the appropriate Ag-depositing content can improve the photo-indcued charge separation and decrease the chance of the combination efficiencies of the photo-induced electrons and holes, which are responsible for the enhancement of TiO2 photocatalytic performance. The optimum silver nitrate concentration of was found to be 1×10?3 mol·L-1. Moreover, reproducibility tests proved that the photocatalytic activity of the silver-modified films remains intact even after eight consecutive experiments of new added pollutant quantities.
ABO3-type perovskite LaFeO3 shows a variety of unusual and interesting structure and properties, which was applied in catalytic field. LaFeO3 nano-sized photocatalysts were synthesized by a sol-gel method, using citric acid as complexing reagent and La(NO3)3·6H2O and Fe(NO3)3·9H2O as raw materials. The as-prepared samples also were characterized by several testing techniques, the optimum preparation conditions and the photocatalytic activity for degrading Rhodamine B under visible irradation were principally investigated. The results show that the crystallite size becomes larger and the SPS response becomes much stronger of LaFeO3 nanoparticles with increasing calcination temperature. The LaFeO3 sample calcined at 500℃exhibits higher activity, and the activity decreases with increasing calcination temperature, which is in good agreement with the characterization results. According to the results of XRD characterization, the crystallite size increases, the energy band bending upward becomes large, the built-in electric field becomes strong, resulting in the SPS intensity increases as the calcination temperature rises. The crystallite size is large, the migrating time of photoinduced charge carriers from the inner to surface is long. Thus, the less photoinduced charge carriers can reach to surfaces in advance of recombination, to fewer be captured to initiate photochemical reactions, resulting in the decrease in the activity.
The sol-gel method is an usual synthesized method. However, the practical application step of the method is hold back at a certain degree by the some shortcoming like small crystallite size and large surface area of the samples prepared by the sol-gel method. So it is necessary to explore new method. LaFeO3 nano-sized photocatalysts were synthesized by hard template method using SBA-16 as template and were characterized by several testing techniques such as nitrogen adsorption-desorption and surface photovoltage spectroscopy. The sample activity of LaFeO3 for degrading Methylene Blue solution under visible irradation was evaluated. We principally investigated the effects of the preparation method on the structure, the properties of LaFeO3. The results show that LaFeO3 prepared by hard template method is porous nano-materials and its surface area calcined at high temperature still becomes larger. Compared with the photocatalytic activity of LaFeO3 prepared by a sol-gel method, its photocatalytic activity increases.
TiO2 is an untra-violet photocatalyst and LaFeO3 is a visible photocatalyst. If TiO2 was modified by LaFeO3, some properties would be gained. It will realize sensitized intention and improve the photocatalytic activity under visible light. It will happen coupling or inpouring of photo-induced electron and enhance photoinduced charage separation. A series of nano-structured film photocatalysts were prepared using TiO2 and LaFeO3 as semiconductor representatives, and were characterized by several testing techniques such as photoluminescence spectrum and surface photovoltage spectroscopy. The photocatalytic activity of LaFeO3 for degrading Methylene Blue solution under visible irradation was evaluated. The results show that the photocatalytic activity of the composite film increases. The coupling between LaFeO3 and TiO2 conduces the high photocatalytic activity of the LaFeO3-TiO2 film; the charge inpouring from TiO2 to LaFeO3 conduces the photoinduced charage separation.
This paper could effectively supplement the basic theories of nano-sized semiconductor material, which would greatly speed up the practical process of nanomaterial in photocatalysis and would offer potent foundation in photoelectron conversion and photoinduced synthesis.
利用溶胶-水热和溶胶-凝胶方法制备了TiO2纳米粒子,对样品进行表征并考察了样品的光催化活性。结果表明,具有和P25相似相组成的T550样品的SPS响应较强说明了此样品的光生电荷分离效率高,并且在405 nm还有一个较强的由表面态跃迁引起的SPS峰,显著地提高了可见光的光催化活性。
利用溶胶-水热法合成了TiO2水热粒子,同时在溶胶形成过程中引入了适量的DBS基团,并进一步通过旋涂法制备了不同的TiO2纳米粒子薄膜。重点考察了添加DBS基团对薄膜表面微观结构、光催化活性和润湿性能的影响,以及内在关系。结果表明:添加DBS使薄膜上的TiO2纳米粒子发生团聚而形成微米级的团簇,虽然减小了膜的有效表面积,使光催化活性降低,但改变了纳米TiO2薄膜的表面微结构,纳米-微米的复合结构使其具有很好的亲水性。添加DBS基团虽然降低了TiO2粒子膜的光催化活性,但是却显著提高了薄膜的亲水性能,甚至达到超亲水性,这主要与薄膜表面由TiO2纳米粒子所形成的微米级隆起有关。说明薄膜表面微观结构能够强烈影响材料的光催化和润湿性能。
半导体表面沉积贵金属被认为是可以捕获光生电子的有效改性方法之一,可以进一步提高半导体光催化剂的活性。以贵金属Ag为代表,对纳米TiO2薄膜进行了改性。主要考察了不同Ag沉积量对TiO2结构和性能等的影响,重点研究了贵金属Ag沉积对纳米TiO2薄膜光生载流子的分离以及光催化性能的影响。结果表明:适量Ag的沉积有利于TiO2薄膜中光生载流子的分离,从而减少电子-空穴的复合几率,进而提高纳米TiO2薄膜的光催化活性。硝酸银溶液的最佳浓度为1×10-3 mol·L-1。此外,沉积贵金属Ag的TiO2薄膜具有良好的光催化循环性能。
LaFeO3由于其独特的晶体结构和优良的性能,近年来在催化等领域显示了较好的应用前景。采用柠檬酸络合法制备了LaFeO3纳米粒子,并利用现代测试技术对样品进行了表征,重点考察了LaFeO3纳米粒子的最佳制备条件及其在可见光下光催化氧化罗丹明B的催化性能。结果表明:随着焙烧温度的升高,粒子尺寸逐渐增大,表面光电压谱(SPS)信号逐渐增强。在光催化实验中,500℃焙烧的LaFeO3纳米粒子表现出较高的光催化活性,随着焙烧温度的升高,样品的光催化活性降低,这与表面光电压谱(SPS)的表征结果是相符合的。样品的尺寸越大,能带弯曲越大,自建电场越强,所以其表面光电压信号增强。样品的尺寸越大,光生载流子从粒子内部到达表面的迁移时间越长,这样使光生载流子在复合前到达半导体表面的数目减少,以至于被捕获的机会减少,进而引发氧化还原反应的几率减小,使其光催化活性降低。此外,与比表面积也有关。随着焙烧温度的升高,粒子尺寸越大,比表面积越小,小的比表面积不利于光催化反应的进行,使其光催化活性降低。
柠檬酸络合法是一种经常被采用的合成方法,但是所制备的样品易团聚、粒径大、比表面积小,以至于在应用中存在许多不足,因此探索新的合成方法是非常有必要的。以SBA-16中孔分子筛为硬模板合成了纳米LaFeO3,利用N2气吸附-脱附和SPS等现代测试技术对样品进行了表征,并利用可见光下光催化降解亚甲基蓝为模型反应对样品的光催化性能进行评价。同时,对模板法与柠檬酸法合成的纳米LaFeO3进行了比较研究。结果表明,利用模板法制得的LaFeO3纳米粒子具有多孔结构,而且在高温条件下可以得到比表面积较大的纳米LaFeO3,其在可见光下的光催化性能与柠檬酸络合法制备的LaFeO3相比有很大的提高。
考虑到TiO2是一种紫外光光催化剂,而LaFeO3是一种可见光光催化剂。若将二者进行复合,在光谱吸收方面将会产生互补,进而会提高对太阳光的利用率。也可能会发生耦合作用或者发生载流子的注入过程,进而导致光生电荷的有效分离,以至于提高光量子效率。在前期研究工作基础上,构建了一系列的TiO2-LaFeO3的纳米复合膜,并利用PL和SPS等测试技术深入地揭示和探讨界面电荷转移行为及其机制,同时以光催化降解亚甲基蓝为模型反应对样品的光催化性能进行评价。结果表明,复合膜的光催化活性明显优于单一组成膜的光催化活性。LaFeO3/TiO2纳米复合膜光催化活性的提高是由于LaFeO3与TiO2之间发生了耦合作用,而TiO2/LaFeO3膜光催化活性的提高是因为发生了光生电荷从TiO2向LaFeO3的注入过程,进而促进了光生电荷的有效分离。
本论文能够使纳米半导体材料的基础理论知识得以丰富,从而有效地推动纳米材料在光催化领域的实用化进程。也将为半导体材料在其它领域的应用如光电转换及光诱导合成等提供理论依据。
In recent years, semiconductor photocatalytic oxidation technology has attracted widely attentions mainly due to its characteristics such as strong oxidation capability, low energy consumption, moderate reaction conditions, quick degrading speed, no-secondly pollution and large application range, and is a new promising practical technology for degrading environmental pollutions. However, the practical application step of the semiconductor photocatalytic oxidation technology is held back to a certain extent by the some shortcoming like the low quantum efficiency of semiconductor material in itself and the lower efficiency for utilizing the solar light. Moreover, the involving the photocatalytic reaction, the relationships between structure and activity, the relationships between activity and interface-charge transferring, the modification mechanism, are not well understood up to date. These problems are needed to solve.In order to improve the photocatalytic activity under visible light and make full use of the solar light, the nano-sized titanium dioxide must be modified. With these in mind, the main purpose of the paper is to prepare nano-sized TiO2 modified with noble metal Ag and ABO3-type perovskite photocatalyst and improve the photocatalytic activity under visible light, and the interface-charge transferring mechanism and the photocatalytic activity of composite film photocatalysts were also principally investigated.
TiO2 nanoparticles were prepared by a sol-hydrothermal process and by a sol-gel method and were characterized by several testing techniques. The photocatalytic activity was principally investigated. The results show that the stronger SPS response of T550 attributes to the efficient photoinduced electron transferring, the surface states related to oxygen vacancies can induce photocatalytic reactions under visible irradiation, especially in the resulting biphasic TiO2 due to the electron transfer from anatase surface states to rutile.
Nanosized anatase TiO2 film on the ITO glass has been fabricated via spin coat process, with sodium dodecylbenzenesulfonate modified TiO2 nanoparticles, which is synthesized by a sol-hydrothermal method, and also characterized mainly by means of several testing techniques. It can be suggested that the superhydrophilic performance is mainly attributed to the high roughness resulting from hierarchical surface structure. The formation of characteristic surface structure is close related to the DBS addition. This will be useful to fabricate other newly nanostructured semiconductor film materials, and promote the practical application in the wetting areas of TiO2 films.
Noble metal depositing has been considered as an effective method to hinder the photogenerated electron/hole pair recombination and accelerate the photoexcitation and formation of oxidizing species, consequently to enhance the photocatalytic activity. TiO2 nanoparticles and TiO2 film were prepared by a sol-hydrothermal process, and were characterized by several testing techniques. The photocatalytic activity for degrading Rhodamine B was principally investigated. Nano-sized TiO2 film deposited with the noble metal Ag was prepared by the sol-gel method. The influences of different Ag content on the TiO2 structure and properties were studied and the effect of Ag-depositing on photo-induced charge separation and photocatalytic activity were principally investigated. The results show that the appropriate Ag-depositing content can improve the photo-indcued charge separation and decrease the chance of the combination efficiencies of the photo-induced electrons and holes, which are responsible for the enhancement of TiO2 photocatalytic performance. The optimum silver nitrate concentration of was found to be 1×10?3 mol·L-1. Moreover, reproducibility tests proved that the photocatalytic activity of the silver-modified films remains intact even after eight consecutive experiments of new added pollutant quantities.
ABO3-type perovskite LaFeO3 shows a variety of unusual and interesting structure and properties, which was applied in catalytic field. LaFeO3 nano-sized photocatalysts were synthesized by a sol-gel method, using citric acid as complexing reagent and La(NO3)3·6H2O and Fe(NO3)3·9H2O as raw materials. The as-prepared samples also were characterized by several testing techniques, the optimum preparation conditions and the photocatalytic activity for degrading Rhodamine B under visible irradation were principally investigated. The results show that the crystallite size becomes larger and the SPS response becomes much stronger of LaFeO3 nanoparticles with increasing calcination temperature. The LaFeO3 sample calcined at 500℃exhibits higher activity, and the activity decreases with increasing calcination temperature, which is in good agreement with the characterization results. According to the results of XRD characterization, the crystallite size increases, the energy band bending upward becomes large, the built-in electric field becomes strong, resulting in the SPS intensity increases as the calcination temperature rises. The crystallite size is large, the migrating time of photoinduced charge carriers from the inner to surface is long. Thus, the less photoinduced charge carriers can reach to surfaces in advance of recombination, to fewer be captured to initiate photochemical reactions, resulting in the decrease in the activity.
The sol-gel method is an usual synthesized method. However, the practical application step of the method is hold back at a certain degree by the some shortcoming like small crystallite size and large surface area of the samples prepared by the sol-gel method. So it is necessary to explore new method. LaFeO3 nano-sized photocatalysts were synthesized by hard template method using SBA-16 as template and were characterized by several testing techniques such as nitrogen adsorption-desorption and surface photovoltage spectroscopy. The sample activity of LaFeO3 for degrading Methylene Blue solution under visible irradation was evaluated. We principally investigated the effects of the preparation method on the structure, the properties of LaFeO3. The results show that LaFeO3 prepared by hard template method is porous nano-materials and its surface area calcined at high temperature still becomes larger. Compared with the photocatalytic activity of LaFeO3 prepared by a sol-gel method, its photocatalytic activity increases.
TiO2 is an untra-violet photocatalyst and LaFeO3 is a visible photocatalyst. If TiO2 was modified by LaFeO3, some properties would be gained. It will realize sensitized intention and improve the photocatalytic activity under visible light. It will happen coupling or inpouring of photo-induced electron and enhance photoinduced charage separation. A series of nano-structured film photocatalysts were prepared using TiO2 and LaFeO3 as semiconductor representatives, and were characterized by several testing techniques such as photoluminescence spectrum and surface photovoltage spectroscopy. The photocatalytic activity of LaFeO3 for degrading Methylene Blue solution under visible irradation was evaluated. The results show that the photocatalytic activity of the composite film increases. The coupling between LaFeO3 and TiO2 conduces the high photocatalytic activity of the LaFeO3-TiO2 film; the charge inpouring from TiO2 to LaFeO3 conduces the photoinduced charage separation.
This paper could effectively supplement the basic theories of nano-sized semiconductor material, which would greatly speed up the practical process of nanomaterial in photocatalysis and would offer potent foundation in photoelectron conversion and photoinduced synthesis.
引文
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