多级结构单晶TiO_2的制备、修饰与光催化性能研究
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摘要
单晶Ti02材料在光催化领域得到了广泛的应用,目前研究较多的单晶Ti02材料主要为锐钛矿型且形貌为八面体或十面体结构,研究的晶面主要为(101)面、(001)面和(010)面；同时该类单晶TiO2材料均为紫外光催化剂,不具备可见光光催化活性。针对目前单晶TiO2材料存在的不足,我们以(001)面暴露的单晶TiO2为出发点,从制备方法入手,通过优化制备方法和条件,控制催化剂的结构和形貌,制备新型单晶TiO2光催化材料。研究催化剂的形貌、晶面和孔结构对光催化性能的本质影响；对单晶TiO2光催化材料进行修饰实现可见光化,研究催化剂组分和修饰方法对光催化性能的本质影响；制备高效实用的Ti02光催化材料,解决实际应用中的一些相关问题。
本论文的具体内容和主要创新点分为以下四个方面：
(001)晶面暴露的有序介孔单晶TiO2
采用叔丁醇醇解溶剂热法以TiOSO4为钛源,在模板剂SBA-15或KIT-6的辅助下制备了(001)面暴露的二维或三维有序介孔单晶Ti02材料。以液相醇光催化选择性氧化为探针反应研究了其光催化活性。研究结果表明单晶TiO2材料比多晶TiO2材料显示了更高的光催化活性,这主要归结于单晶TiO2材料具有较高的结晶度有利于光生电子的传递,降低其与空穴的复合；(001)面有利于活化反应物分子促进光催化氧化,同时(001)面的暴露使单晶TiO2材料表面具有较多的氧空位有利于捕获光生电子抑制其与空穴的复合。同时具有有序介孔结构的TiO2材料其活性高于无序介孔结构的材料尤其是三维有序结构TiO2材料,这主要是由于有序孔结构可以对光实现多次反射提高光的利用率,同时有序孔结构利于反应物分子的吸附与扩散。
二、(001)晶面暴露的层状单晶TiO2
通过苯甲醇醇解溶剂热法以TiF4为钛源,首次制备了(001)面暴露的层状结构单晶TiO2,其(001)面暴露率高达90%。通过优化合成条件揭示了层状结构的形成机理,其形成过程由苯甲醇分子键合在(001)面暴露的TiO2纳米片上,苯甲醇分子之间的π-π键驱使Ti02纳米片进行自组装而形成层状结构,F离子作为晶面稳定剂吸附在Ti02纳米片使其暴露(001)面。同时该体系还可以制备由Ti02纳米晶定向生长形成的光子晶体薄膜,该薄膜有明显的色彩和表面等离子体共振吸收边。该层状结构单晶Ti02在醇光催化选择性氧化中体现了较好的催化性能,这主要归根于较大的比表面积、较高的(001)面暴露率和独特的层状结构。
三、CdS量子点修饰(001)晶面暴露的介孔单晶Ti02
通过离子交换法制备了CdS量子点修饰的(001)面暴露的介孔单晶Ti02可见光催化剂,并以苯甲醇可见光光催化选择性氧化为探针反应详细研究了CdS的修饰量与修饰方法对光催化活性的影响。研究表明CdS高度分散且富集于Ti02表面,其修饰有利于可见光吸收：其活性高于未修饰的Ti02,这主要归结于CdS修饰增强了敏化提高了光的吸收能力。同时离子交换法制备催化剂的活性高于直接沉淀法或物理混合法制备的催化剂,这主要归结于该催化剂表面的CdS粒子尺寸更小更分散,与催化剂的结合力更强,形成更多异质结有利于光生电子的传递,降低其与空穴的复合。同时通过添加不同的捕获剂,详细研究了苯甲醇光催化选择性氧化的主要活性物种并提出了相应的机理。
四、Ti3+修饰(001)晶面暴露的片状单晶Ti02
采用超临界醇解溶剂热法以TiF4和钛酸四正丁酯为钛源,制备了Ti3+原位掺杂的(001)面暴露的单晶TiO2纳米片可见光催化剂,该催化剂在污染物降解同步光解水产氢过程中显示了较高的催化活性。这主要归结于Ti3+原位掺杂使其形成中间能级,降低了催化剂的能带提高了光吸收能力；(001)面暴露增加了催化剂表面的氧空位,有利于捕获光生电子抑制其与空穴的复合；催化剂具有较高的结晶度有利于传递光生电子；催化剂的高比表面积提高了反应物分子的吸附与扩散。同时研究表明染料降解可促进光解水产氢,这是因为光催化降解染料消耗光生空穴抑制了其与电子的复合。
Single crystal TiO2materials have been widely studied and applied in the field of photocatalysis. To date, most studies are focused on the anatase TiO2single crystals in octahedron and decanedron with dominant (001),(101), or (010) facets. Nearly all these TiO2single crystals are used as photocatalysts under UV light irradiation rather than the visible light irradiation due to the large band gap of anatase (3.2eV). To overcome the disadvantages of the single crystal TiO2photocatalysts, this work focuses on the preparation of new single crystal TiO2materials with controllable morphology and pore structure by optimizing the preparation methods and conditions, which are used in photocatalytic reactions concerning dyes degradation, H2production by splitting water, and selective oxidation of alcohols to the corresponding aldehydes. Our research mainly concentrates on the effects of the crystal plane, pore structure, and morphology on the photocatalytic activity. Meanwhile, modification of the single crystal TiO2with CdS quantum dots and Ti3+has also been carried out to achieve highly active visible photocatalysts.
The detailed work and the main innovation are divided into the four parts addressed as follows.
1. Ordered mesoporous TiO2single crystal with exposed (001) facets as a UV photocatalyst
Single-crystal TiO2with2D or3D ordered mesoporous structures and exposed (001) facets were synthesized by SBA-15or KIT-6templated alcoholysis of TiOSO4in the solvent of tert-butyl alcohol under solvothermal conditions. During liquid phase photocatalytic selective oxidation of alcohol to aldehyde under UV-light irradiation, the single-crystal TiO2exhibited much higher activity than the poly-crystal TiO2, since the high crystallization degree favored the transfer of photoelectrons, which might reduce their recombination rate with holes. Besides, the exposed(001) facets facets favored the photocatalytic oxidation owing to the high surface energy and the increased oxygen vacancies which reduced the photocharges recombination rate by capturing photoelectrons. Meanwhile, the TiO2with ordered mesoporous structures showed higher activity than that with disordered mesopores, and the3D ordered mesoporous channels were more favalable for photocatalytic oxidation than the2D ordered mesoporous channels, which could be attributed to both the enhanced light harvesting owing to the multiple light reflections in pore channels, and the facilitated diffusion and adsorption of reactant molecules.
2. Single crystal TiO2with layered structure and exposed (001) facets
Single crystal TiO2with layered structure and exposed (001) facets was firstly synthesized by alcoholysis of TiF4in the solvent of benzyl alcohol under solvothermal conditions. The percentage of the (001) facets of the layered single crystal TiO2was about90%. The formation mechanism of the layered single crystal TiO2materials was detailed studied by optimizing the solvothermal conditions. The layered structure was constructed by the self-assembly of the π-π bonding among the benzene rings, and the fluorinion as the stabilizing agent of crystal plane could decrease the surface energy of the (001) high energy facets and stabilize the (001) facets in order to make the layered TiO2with exposed (001) facets. Meanwhile, this synthetic system can be used to prepare the TiO2photonic film, which is assembled by the oriented growth of TiO2nanocrystals. The photonic film with strong plasmonic bands is colored to the naked eye. The layered TiO2photocatalyst displays high photocatalytic activity during the photocatalytic selective oxidation of alcohols to the corresponding aldehydes, due to the high surface area, the high percentage of the (001) facets, and the layered structure enhanced the light harvesting owing to the multiple light reflections between the two adjacent nanosheets.
3. TiO2mesocrystal with exposed (001) facets and doped with CdS quantum dots as a visible photocatalyst
CdS quantum dots decorated TiO2mesocrystals visible photocatalyst with exposed{001} facets have been firstly prepared by a simple ion-exchange treatment. The Ti O2mesocrystals homogeneously decorated with surface enrichment of CdS quantum dots exhibited significant improvement in photocatalytic selective oxidation of benzyl alcohol and its derivatives under visible light irradiation than pure T1O2mesocages, ascribing to the enhanced light-harvesting capability, the enhanced photosensitizing effect of surface enriched CdS quantum dots and the formation heterojunctions between CdS and TiO2. Meanwhile, the sample prepared by ion-exchange displayed higher photocatalytic activity than those samples prepared by direct-deposited or physically mixed methods, due to the uniform dispersion of CdS quantum dots, the increasing number of heterojunctions, the lower recombination rate of photocharges, and the strong interaction between CdS and TiO2. The mechanism of photocatalytic selective oxidation of alcohols was also investigated by the addition of different scavengers.
4. In situ Ti3+-doped TiO2visible photocatalyst in nanosheets with dominant (001) facets
In situ Ti3+-doped TiO2crystal in mesoporous nanosheets with dominant (001) facets was prepared by supercritical treatment of the precursor obtained from sol-gel hydrolysis of mixed Ti(n-OC4HcH9)4and TiF4. This photocatalyst exhibited high activity in synchronical pollutant degradation and produce H2by water splitting under visible light irradiation owing to synergistic promoting effects. On one hand, the narrowed energy band gap resulted from Ti3+-doping and the high surface area enhanced light harvest and reactant adsorption. On the other hand, the high crystallization degree accelerated electron transfer and thus, inhibited photoelectron-hole recombination. Furthermore, the exposed (001) facets with high surface energy favored the activation of reactant molecules. The photocatalytic degradation of organic pollutants promoted the H2production by consuming photogenerated holes, which inhibited their recombination with photoelectrons used for reducing H+during water splitting.
本论文的具体内容和主要创新点分为以下四个方面：
(001)晶面暴露的有序介孔单晶TiO2
采用叔丁醇醇解溶剂热法以TiOSO4为钛源,在模板剂SBA-15或KIT-6的辅助下制备了(001)面暴露的二维或三维有序介孔单晶Ti02材料。以液相醇光催化选择性氧化为探针反应研究了其光催化活性。研究结果表明单晶TiO2材料比多晶TiO2材料显示了更高的光催化活性,这主要归结于单晶TiO2材料具有较高的结晶度有利于光生电子的传递,降低其与空穴的复合；(001)面有利于活化反应物分子促进光催化氧化,同时(001)面的暴露使单晶TiO2材料表面具有较多的氧空位有利于捕获光生电子抑制其与空穴的复合。同时具有有序介孔结构的TiO2材料其活性高于无序介孔结构的材料尤其是三维有序结构TiO2材料,这主要是由于有序孔结构可以对光实现多次反射提高光的利用率,同时有序孔结构利于反应物分子的吸附与扩散。
二、(001)晶面暴露的层状单晶TiO2
通过苯甲醇醇解溶剂热法以TiF4为钛源,首次制备了(001)面暴露的层状结构单晶TiO2,其(001)面暴露率高达90%。通过优化合成条件揭示了层状结构的形成机理,其形成过程由苯甲醇分子键合在(001)面暴露的TiO2纳米片上,苯甲醇分子之间的π-π键驱使Ti02纳米片进行自组装而形成层状结构,F离子作为晶面稳定剂吸附在Ti02纳米片使其暴露(001)面。同时该体系还可以制备由Ti02纳米晶定向生长形成的光子晶体薄膜,该薄膜有明显的色彩和表面等离子体共振吸收边。该层状结构单晶Ti02在醇光催化选择性氧化中体现了较好的催化性能,这主要归根于较大的比表面积、较高的(001)面暴露率和独特的层状结构。
三、CdS量子点修饰(001)晶面暴露的介孔单晶Ti02
通过离子交换法制备了CdS量子点修饰的(001)面暴露的介孔单晶Ti02可见光催化剂,并以苯甲醇可见光光催化选择性氧化为探针反应详细研究了CdS的修饰量与修饰方法对光催化活性的影响。研究表明CdS高度分散且富集于Ti02表面,其修饰有利于可见光吸收：其活性高于未修饰的Ti02,这主要归结于CdS修饰增强了敏化提高了光的吸收能力。同时离子交换法制备催化剂的活性高于直接沉淀法或物理混合法制备的催化剂,这主要归结于该催化剂表面的CdS粒子尺寸更小更分散,与催化剂的结合力更强,形成更多异质结有利于光生电子的传递,降低其与空穴的复合。同时通过添加不同的捕获剂,详细研究了苯甲醇光催化选择性氧化的主要活性物种并提出了相应的机理。
四、Ti3+修饰(001)晶面暴露的片状单晶Ti02
采用超临界醇解溶剂热法以TiF4和钛酸四正丁酯为钛源,制备了Ti3+原位掺杂的(001)面暴露的单晶TiO2纳米片可见光催化剂,该催化剂在污染物降解同步光解水产氢过程中显示了较高的催化活性。这主要归结于Ti3+原位掺杂使其形成中间能级,降低了催化剂的能带提高了光吸收能力；(001)面暴露增加了催化剂表面的氧空位,有利于捕获光生电子抑制其与空穴的复合；催化剂具有较高的结晶度有利于传递光生电子；催化剂的高比表面积提高了反应物分子的吸附与扩散。同时研究表明染料降解可促进光解水产氢,这是因为光催化降解染料消耗光生空穴抑制了其与电子的复合。
Single crystal TiO2materials have been widely studied and applied in the field of photocatalysis. To date, most studies are focused on the anatase TiO2single crystals in octahedron and decanedron with dominant (001),(101), or (010) facets. Nearly all these TiO2single crystals are used as photocatalysts under UV light irradiation rather than the visible light irradiation due to the large band gap of anatase (3.2eV). To overcome the disadvantages of the single crystal TiO2photocatalysts, this work focuses on the preparation of new single crystal TiO2materials with controllable morphology and pore structure by optimizing the preparation methods and conditions, which are used in photocatalytic reactions concerning dyes degradation, H2production by splitting water, and selective oxidation of alcohols to the corresponding aldehydes. Our research mainly concentrates on the effects of the crystal plane, pore structure, and morphology on the photocatalytic activity. Meanwhile, modification of the single crystal TiO2with CdS quantum dots and Ti3+has also been carried out to achieve highly active visible photocatalysts.
The detailed work and the main innovation are divided into the four parts addressed as follows.
1. Ordered mesoporous TiO2single crystal with exposed (001) facets as a UV photocatalyst
Single-crystal TiO2with2D or3D ordered mesoporous structures and exposed (001) facets were synthesized by SBA-15or KIT-6templated alcoholysis of TiOSO4in the solvent of tert-butyl alcohol under solvothermal conditions. During liquid phase photocatalytic selective oxidation of alcohol to aldehyde under UV-light irradiation, the single-crystal TiO2exhibited much higher activity than the poly-crystal TiO2, since the high crystallization degree favored the transfer of photoelectrons, which might reduce their recombination rate with holes. Besides, the exposed(001) facets facets favored the photocatalytic oxidation owing to the high surface energy and the increased oxygen vacancies which reduced the photocharges recombination rate by capturing photoelectrons. Meanwhile, the TiO2with ordered mesoporous structures showed higher activity than that with disordered mesopores, and the3D ordered mesoporous channels were more favalable for photocatalytic oxidation than the2D ordered mesoporous channels, which could be attributed to both the enhanced light harvesting owing to the multiple light reflections in pore channels, and the facilitated diffusion and adsorption of reactant molecules.
2. Single crystal TiO2with layered structure and exposed (001) facets
Single crystal TiO2with layered structure and exposed (001) facets was firstly synthesized by alcoholysis of TiF4in the solvent of benzyl alcohol under solvothermal conditions. The percentage of the (001) facets of the layered single crystal TiO2was about90%. The formation mechanism of the layered single crystal TiO2materials was detailed studied by optimizing the solvothermal conditions. The layered structure was constructed by the self-assembly of the π-π bonding among the benzene rings, and the fluorinion as the stabilizing agent of crystal plane could decrease the surface energy of the (001) high energy facets and stabilize the (001) facets in order to make the layered TiO2with exposed (001) facets. Meanwhile, this synthetic system can be used to prepare the TiO2photonic film, which is assembled by the oriented growth of TiO2nanocrystals. The photonic film with strong plasmonic bands is colored to the naked eye. The layered TiO2photocatalyst displays high photocatalytic activity during the photocatalytic selective oxidation of alcohols to the corresponding aldehydes, due to the high surface area, the high percentage of the (001) facets, and the layered structure enhanced the light harvesting owing to the multiple light reflections between the two adjacent nanosheets.
3. TiO2mesocrystal with exposed (001) facets and doped with CdS quantum dots as a visible photocatalyst
CdS quantum dots decorated TiO2mesocrystals visible photocatalyst with exposed{001} facets have been firstly prepared by a simple ion-exchange treatment. The Ti O2mesocrystals homogeneously decorated with surface enrichment of CdS quantum dots exhibited significant improvement in photocatalytic selective oxidation of benzyl alcohol and its derivatives under visible light irradiation than pure T1O2mesocages, ascribing to the enhanced light-harvesting capability, the enhanced photosensitizing effect of surface enriched CdS quantum dots and the formation heterojunctions between CdS and TiO2. Meanwhile, the sample prepared by ion-exchange displayed higher photocatalytic activity than those samples prepared by direct-deposited or physically mixed methods, due to the uniform dispersion of CdS quantum dots, the increasing number of heterojunctions, the lower recombination rate of photocharges, and the strong interaction between CdS and TiO2. The mechanism of photocatalytic selective oxidation of alcohols was also investigated by the addition of different scavengers.
4. In situ Ti3+-doped TiO2visible photocatalyst in nanosheets with dominant (001) facets
In situ Ti3+-doped TiO2crystal in mesoporous nanosheets with dominant (001) facets was prepared by supercritical treatment of the precursor obtained from sol-gel hydrolysis of mixed Ti(n-OC4HcH9)4and TiF4. This photocatalyst exhibited high activity in synchronical pollutant degradation and produce H2by water splitting under visible light irradiation owing to synergistic promoting effects. On one hand, the narrowed energy band gap resulted from Ti3+-doping and the high surface area enhanced light harvest and reactant adsorption. On the other hand, the high crystallization degree accelerated electron transfer and thus, inhibited photoelectron-hole recombination. Furthermore, the exposed (001) facets with high surface energy favored the activation of reactant molecules. The photocatalytic degradation of organic pollutants promoted the H2production by consuming photogenerated holes, which inhibited their recombination with photoelectrons used for reducing H+during water splitting.
引文
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