钛酸盐纳米管薄膜的合成、一维自组装特性及应用性能研究
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摘要
作为新型功能材料的钛酸盐纳米管，具有良好的电化学、光化学性能，因此，在催化、储氢、化学传感器、离子交换、分子吸附等领域应用广泛。现阶段，人们对钛酸盐纳米管的研究还多停留在粉体方面,相比之下，集纳米管和薄膜优点于一身的钛酸盐纳米管薄膜材料比粉体材料在应用领域上的前景更为广阔。目前，采用水热法合成钛酸盐纳米管的研究已经取得了多方面的进展，但仍有许多问题尚未明确，对其形成机理、化学组成、性能及应用等还有待进一步研究。
本课题采用水热法在钛基底上合成出管径小、稳定性强、与基底结合力良好的多层钛酸盐纳米管薄膜。为了确定合成纳米管薄膜的最佳反应条件，我们对反应条件进行了详细地考察，并提出了钛酸盐纳米管的形成机理。此外，我们选取不同的钛源，控制溶液碱度和冷却温度等反应条件，尝试将一维纳米结构的制备与自组装结合起来，成功地合成出鸟巢状钛酸盐纳米带自组装聚集体、绒球状钛酸盐纳米带自组装聚集体以及海胆状钛酸盐纳米管自组装聚集体，并通过引入碳酸钠模板，合成出碳酸钠-钛酸盐香蒲状纳米管自组装聚集体复合材料。通过考察钛酸盐自组装聚集体的结构以及一维自组装特性，我们提出了“生长-自组装”的两步生长机理。与此同时，我们对钛酸盐纳米管多层膜、纳米管自组装聚集体的应用性能进行深入研究，并利用金属掺杂等方法对其性能进行改善，为开发利用新型的钛基底表面钛酸盐纳米管薄膜材料奠定基础。我们分别以镍和银为掺杂元素对其进行掺杂改性。首先，采用离子交换法合成镍掺杂钛酸盐纳米管薄膜，结果表明：镍的掺杂导致了钛酸盐纳米管中出现了杂质能级，降低了其禁带宽度，提高光生电子-空穴对的分离效率，在可见光的吸收范围得到拓展，提高了对可见光的利用率。我们又通过光催化还原反应将Ag/AgNO3纳米粒子负载到钛酸盐纳米管薄膜上，合成了Ag/AgNO3修饰钛酸盐纳米管薄膜。Ag/AgNO3等离子共振效应增强了钛酸盐纳米管薄膜对可见光的吸收，提高了光催化活性。此外，Ag/AgNO3修饰钛酸盐纳米管薄膜还展现出奇特的光致变色特性和优良的抗菌性能。
As a new functional material, the titanate nanotube is widely applied in ionexchange, catalysis, adsorption, chemical sensors, hydrogen storage and other fieldsdue to its good electrochemical, photochemical properties. In recent years, thepreparation of titanate nanotubes and the development of its application have becomeanother hot spot after carbon nanotube material. At this stage, most of researches ofthe synthesis of the titanate nanotube are still focused on powder type. By comparison,the titanate nanotubes film which sets the merits of nanotubes and thin films in a bodyis often more desirable for applications. Hitherto the research of preparing titanatenanotubes by the hydrothermal technique has made much progress. While theformation mechanism, crystalline compositions, performance and application are still incontroversy.
The aim of our study is to find a kind of simple and easy method to prepare multilayertitanate nanotubes film which has a small diameter, high stability and the good bindingforce with Ti substrate. We artificially regulated the morphology and the structure oftitanate nanotubes by controlling the reaction conditions. We tried to prepare thewell-regulated one-dimensional nanostructures aggregates by combining the synthesisof the one-dimensional nanostructures and self-assembly synthesis of aggregates. Inthe graduation thesis, we discussed the formation mechanism of the titanate nanotubemultilayer film and self-assembled aggregates in detail. We studied the thermalstability, the photocatalytic properties and the hydrogen storage property of thetitanate nanotube multilayer, and improved its performance though the metal dopingmethods. It would lay the foundation for the development and the utilization of thenew titanate nanotubes film material on Ti substrate. The main research contents are as follows:
1. Multilayered titanate nanotubes thin films grew on titanium metal surface via ahydrothermal surface treatment process. The outer diameter of the nanotube was6-8nm, the inner diameter was4-6nm. Its length was a few micrometers. The tube wallwas multiple, and its layers were not symmetrical. The thickness of the film withcontinuous multilayer structure was about8μm. By a lot of study on reaction conditions,we determined the optimum preparation conditions of titanate nanotube films: Thereaction temperature was140℃, the reaction time was12h, NaOH concentration was10M. Finally, we got a stable multilayer titanate nanotube film on Ti substrate by thewashing processing procedure of slowly reducing pH value. A general formationmechanism for the oriented titanate nanotube thin film was proposed. The overallformation of titanate nanotubes can be summarized as a sequence of four steps: Thefirst, titanium dissolution and alkali titanate hydrogel formation; The second, alkalititanate hydrogel dissolution and layered Na_2Ti_3O7formation; The third, layeredNa_2Ti_3O7growth; The forth, nanotube formation via layered Na_2Ti_3O7splitting andthe multilayer scrolling process.
2. Bird's nest-like titanate nanoribbon self-assembly aggregates, fluff Sphere-liketitanate nanoribbon self-assembly aggregates and urchin-like titanate nanotubeself-assembly aggregates were prepared without template technique from Ti flake (orP25) under hydrothermal conditions by adjusting NaOH concentration and coolingtemperature. Cattail-like Na_2CO3-titanate nanotubes self-assembly complexaggregates were prepared with template technique using sodium carbonate. A possibletwo-stage growth mechanism involving the initial formation of primary1Dnanostructure that subsequently self-assembly was proposed. This method willprovide a promising approach that the function materials are assembled into thehighly ordered structure in the ideal way.
3. The thermal stability, the photocatalytic activity and the hydrogen storage abilityof titanate nanotubes thin films and self-assembly titanate nanotube aggregates werestudied in depth. The multilayer titanate nanotube film was stable on Ti substrate bythe washing procedure of slowly reducing pH value. The layer-delaminating ofmultilayered titanate nanotubes thin films have been come ture using ultrasonictreatment method. The thermal stability of Na-type titanate nanotubes films (TNTW)was higher than that of H-type titanate nanotubes films (TNTA). TNTW could still keep the nanotube structure when the heat treatment temperature was up to500℃, whileTNTA began to lose the nanotube structure when the heat treatment temperature wasmore than400℃. The photocatalytic activity of TNTW and TNTA was weak,however, their calcined products showed better photocatalytic activity. The visiblelight absorption wavelength of the calcined products of TNTW and TNTA shifted tolong wavelength. Their absorption ability for long wavelength was stronger than P25and was conducive to visible light photocatalytic reaction. At same pressure, thehydrogen adsorption capacity of urchin-like titanate nanotube self-assemblyaggregates and TNTA was higher than cattail-like nanotube self-assembly aggregatesand TNTW. According to the different properties of titanate nanotubes film andnanotubes self-assembled aggregates, it is expected to develop these functionalmaterials for different applications.
4. Ni-doped titanate nanotubes films were synthesized on Ti substrate byhydrothermal treatment，followed by a facile ion-exchange process in NiCl2solution.The nickel doping greatly broadened the absorption wavelength range of the titanatenanotubes film and brought an obvious red shift effect for the threshold wavelength.The utilization ratio of the visible light for the titanate nanotubes film was greatlyimproved. Therefore, Ni-doped titanate nanotubes film is expected to be a new kind ofcomposite material which is used in visible light catalysis.
5. Ag/AgNO3modified titanate nanotubes film was prepared by hydrothermaltreatment method and followed by photo reduction method. The film exhibited highphotocatalytic actibity, which was due to the surface Plasmon resonance effect andfast separation of photogenerated electron-hole pairs. Ag/AgNO3acted as the activecenter and generated·O2-, HO2· and·OH. These strong oxidative free radicals not onlydegraded the organic matter, but also eliminated bacterium. The film exhibitedphotochromic property from grayish white to bluish black or brownish black afterUV-rays irradiation. Ag/AgNO3modified titanate nanotubes films would be apromising material in various of application areas in virtue of its excellentphotocatalytic activity, photochromic property and antibacterial activity.
本课题采用水热法在钛基底上合成出管径小、稳定性强、与基底结合力良好的多层钛酸盐纳米管薄膜。为了确定合成纳米管薄膜的最佳反应条件，我们对反应条件进行了详细地考察，并提出了钛酸盐纳米管的形成机理。此外，我们选取不同的钛源，控制溶液碱度和冷却温度等反应条件，尝试将一维纳米结构的制备与自组装结合起来，成功地合成出鸟巢状钛酸盐纳米带自组装聚集体、绒球状钛酸盐纳米带自组装聚集体以及海胆状钛酸盐纳米管自组装聚集体，并通过引入碳酸钠模板，合成出碳酸钠-钛酸盐香蒲状纳米管自组装聚集体复合材料。通过考察钛酸盐自组装聚集体的结构以及一维自组装特性，我们提出了“生长-自组装”的两步生长机理。与此同时，我们对钛酸盐纳米管多层膜、纳米管自组装聚集体的应用性能进行深入研究，并利用金属掺杂等方法对其性能进行改善，为开发利用新型的钛基底表面钛酸盐纳米管薄膜材料奠定基础。我们分别以镍和银为掺杂元素对其进行掺杂改性。首先，采用离子交换法合成镍掺杂钛酸盐纳米管薄膜，结果表明：镍的掺杂导致了钛酸盐纳米管中出现了杂质能级，降低了其禁带宽度，提高光生电子-空穴对的分离效率，在可见光的吸收范围得到拓展，提高了对可见光的利用率。我们又通过光催化还原反应将Ag/AgNO3纳米粒子负载到钛酸盐纳米管薄膜上，合成了Ag/AgNO3修饰钛酸盐纳米管薄膜。Ag/AgNO3等离子共振效应增强了钛酸盐纳米管薄膜对可见光的吸收，提高了光催化活性。此外，Ag/AgNO3修饰钛酸盐纳米管薄膜还展现出奇特的光致变色特性和优良的抗菌性能。
As a new functional material, the titanate nanotube is widely applied in ionexchange, catalysis, adsorption, chemical sensors, hydrogen storage and other fieldsdue to its good electrochemical, photochemical properties. In recent years, thepreparation of titanate nanotubes and the development of its application have becomeanother hot spot after carbon nanotube material. At this stage, most of researches ofthe synthesis of the titanate nanotube are still focused on powder type. By comparison,the titanate nanotubes film which sets the merits of nanotubes and thin films in a bodyis often more desirable for applications. Hitherto the research of preparing titanatenanotubes by the hydrothermal technique has made much progress. While theformation mechanism, crystalline compositions, performance and application are still incontroversy.
The aim of our study is to find a kind of simple and easy method to prepare multilayertitanate nanotubes film which has a small diameter, high stability and the good bindingforce with Ti substrate. We artificially regulated the morphology and the structure oftitanate nanotubes by controlling the reaction conditions. We tried to prepare thewell-regulated one-dimensional nanostructures aggregates by combining the synthesisof the one-dimensional nanostructures and self-assembly synthesis of aggregates. Inthe graduation thesis, we discussed the formation mechanism of the titanate nanotubemultilayer film and self-assembled aggregates in detail. We studied the thermalstability, the photocatalytic properties and the hydrogen storage property of thetitanate nanotube multilayer, and improved its performance though the metal dopingmethods. It would lay the foundation for the development and the utilization of thenew titanate nanotubes film material on Ti substrate. The main research contents are as follows:
1. Multilayered titanate nanotubes thin films grew on titanium metal surface via ahydrothermal surface treatment process. The outer diameter of the nanotube was6-8nm, the inner diameter was4-6nm. Its length was a few micrometers. The tube wallwas multiple, and its layers were not symmetrical. The thickness of the film withcontinuous multilayer structure was about8μm. By a lot of study on reaction conditions,we determined the optimum preparation conditions of titanate nanotube films: Thereaction temperature was140℃, the reaction time was12h, NaOH concentration was10M. Finally, we got a stable multilayer titanate nanotube film on Ti substrate by thewashing processing procedure of slowly reducing pH value. A general formationmechanism for the oriented titanate nanotube thin film was proposed. The overallformation of titanate nanotubes can be summarized as a sequence of four steps: Thefirst, titanium dissolution and alkali titanate hydrogel formation; The second, alkalititanate hydrogel dissolution and layered Na_2Ti_3O7formation; The third, layeredNa_2Ti_3O7growth; The forth, nanotube formation via layered Na_2Ti_3O7splitting andthe multilayer scrolling process.
2. Bird's nest-like titanate nanoribbon self-assembly aggregates, fluff Sphere-liketitanate nanoribbon self-assembly aggregates and urchin-like titanate nanotubeself-assembly aggregates were prepared without template technique from Ti flake (orP25) under hydrothermal conditions by adjusting NaOH concentration and coolingtemperature. Cattail-like Na_2CO3-titanate nanotubes self-assembly complexaggregates were prepared with template technique using sodium carbonate. A possibletwo-stage growth mechanism involving the initial formation of primary1Dnanostructure that subsequently self-assembly was proposed. This method willprovide a promising approach that the function materials are assembled into thehighly ordered structure in the ideal way.
3. The thermal stability, the photocatalytic activity and the hydrogen storage abilityof titanate nanotubes thin films and self-assembly titanate nanotube aggregates werestudied in depth. The multilayer titanate nanotube film was stable on Ti substrate bythe washing procedure of slowly reducing pH value. The layer-delaminating ofmultilayered titanate nanotubes thin films have been come ture using ultrasonictreatment method. The thermal stability of Na-type titanate nanotubes films (TNTW)was higher than that of H-type titanate nanotubes films (TNTA). TNTW could still keep the nanotube structure when the heat treatment temperature was up to500℃, whileTNTA began to lose the nanotube structure when the heat treatment temperature wasmore than400℃. The photocatalytic activity of TNTW and TNTA was weak,however, their calcined products showed better photocatalytic activity. The visiblelight absorption wavelength of the calcined products of TNTW and TNTA shifted tolong wavelength. Their absorption ability for long wavelength was stronger than P25and was conducive to visible light photocatalytic reaction. At same pressure, thehydrogen adsorption capacity of urchin-like titanate nanotube self-assemblyaggregates and TNTA was higher than cattail-like nanotube self-assembly aggregatesand TNTW. According to the different properties of titanate nanotubes film andnanotubes self-assembled aggregates, it is expected to develop these functionalmaterials for different applications.
4. Ni-doped titanate nanotubes films were synthesized on Ti substrate byhydrothermal treatment，followed by a facile ion-exchange process in NiCl2solution.The nickel doping greatly broadened the absorption wavelength range of the titanatenanotubes film and brought an obvious red shift effect for the threshold wavelength.The utilization ratio of the visible light for the titanate nanotubes film was greatlyimproved. Therefore, Ni-doped titanate nanotubes film is expected to be a new kind ofcomposite material which is used in visible light catalysis.
5. Ag/AgNO3modified titanate nanotubes film was prepared by hydrothermaltreatment method and followed by photo reduction method. The film exhibited highphotocatalytic actibity, which was due to the surface Plasmon resonance effect andfast separation of photogenerated electron-hole pairs. Ag/AgNO3acted as the activecenter and generated·O2-, HO2· and·OH. These strong oxidative free radicals not onlydegraded the organic matter, but also eliminated bacterium. The film exhibitedphotochromic property from grayish white to bluish black or brownish black afterUV-rays irradiation. Ag/AgNO3modified titanate nanotubes films would be apromising material in various of application areas in virtue of its excellentphotocatalytic activity, photochromic property and antibacterial activity.
引文
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