TiO_2纳米管复合膜的光生阴极保护研究
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摘要
TiO_2具有良好的光电特性、光催化性及化学稳定性等,在光催化剂、气敏传感器、太阳能电池、光生阴极保护等高科技领域有着广阔的应用前景,成为一种最具潜力的半导体材料。将光照下的纳米氧化钛膜层产生的光生阴极保护作用应用于金属防腐蚀已经引起科学家的极大兴趣。但TiO_2覆盖膜作为金属防腐蚀涂层存在膜层缺陷和不均一性的技术问题,而且由于TiO_2带隙较宽(E_g=3.0-3.2eV),只吸收λ＜387nm的紫外光,而且光激发产生电子—空穴对易于复合,导致光量子效率低,太阳光谱中占绝对大分量的可见光未能有效利用,导致在可见光和暗态下不能起到有效的光生阴极保护作用。
本论文侧重发展多种先进的TiO_2纳米复合膜材料和表面改性技术,采用溶胶凝胶法和浸渍提拉技术在316不锈钢及铜表面构筑纳米TiO_2薄膜及SnO_2-TiO_2、N-TiO_2复合膜,引入紫外光对薄膜进行改性。同时发展电化学阳极氧化法,在钛基体表面制备一层具有特殊纳米结构的TiO_2纳米管阵列和金属离子掺杂的TiO_2纳米管膜。利用SEM、XRD、XPS、UV-Vis等表征方法系统研究纳米薄膜的形貌、晶型、组成等。采用腐蚀电化学和光电化学相结合技术,测试膜层的光电化学性质,研究TiO_2复合颗粒膜及掺杂半导体纳米管阵列薄膜对金属基体的光生阴极保护作用。以期通过掺杂改性技术和利用具有奇特性质的纳米管阵列作为光阳极有效延长光生电子-空穴对的寿命,强化可见光范围内和暗态下持续有效的光生阴极保护的作用,并探明膜层光生阴极保护的作用机理。主要进展及研究成果如下:
1.对传统TiO_2溶胶制备方法进行了改进,简化实验操作程序,在室温下制备了颗粒尺寸可控的超微粒子TiO_2、TiO_2-SnO_2、N-TiO_2溶胶,各种光电化学技术研究在金属表面超薄纳米TiO_2复合掺杂颗粒膜在不同腐蚀性溶液体系中的耐腐蚀行为,同时考察溶液浓度、膜厚、掺杂等条件的影响,制备了有最佳耐蚀性的纳米膜,有效提高金属或合金的耐腐蚀性能,并探明纳米膜的抗腐蚀机理。
2.采用腐蚀电化学和光电化学方法研究纳米TiO_2膜及其复合膜的光电性能及影响因素。发现复合膜能够减缓光生电子空穴对电荷的复合,在紫外光照射下产生较强的光生电流;采用湿法实现了有效的N掺杂,N掺杂形成了新能级,通过N_(2P)与O_(2P)态的混合而导致TiO_2禁带宽度变窄,获得了良好的可见光响应。实现在紫外、可见光和暗态下高效的光生阴极保护,同时也使纳米膜和复合膜具有更强的阻挡层作用,发挥纳米复合膜的双重保护协同作用的功能。
3.在含有F~-的电解液体系中,采用电化学阳极氧化法成功地在钛基体表面制备了排列整齐、高度有序的TiO_2纳米管及Fe掺杂型纳米管阵列。采用光电化学联用系统研究纳米管阵列的光电响应特性,结果表明:以TiO_2纳米管阵列膜作为光生阳极时,在紫外光区(λ＜387m)有显著增强的光生电流响应。
4.采用在氟化电解液中直接加入含有Fe~(2+)掺杂物的方法,成功实现了纳米TiO_2的Fe掺杂,铁元素以Fe的氧化物或者Fe(Ⅲ)离子的形式接入半导体TiO_2的晶格中,窄化TiO_2带隙,使光谱响应扩展到波长大于400nm的可见光区,首次采用Fe掺杂的TiO_2纳米管阵列膜作为光生阳极研究光生阴极保护作用。测试发现:在紫外光和可见光照射下,TiO_2纳米管及Fe掺杂纳米管阵列膜层对316不锈钢有很好的光生阴极保护作用,暗态下,光生电极电位仍可维持较长的一段时间,能够继续发挥阴极保护作用。
Titania (TiO_2) is one of the most important semiconductor oxides because of its excellent photo-electrochemistry, photo-catalysis and good chemical stability. It can be used in many hi-tech applications including photocatalysis, gas sensors, solar cells, cathodic protection and etc. It is of great interest to develop TiO_2 coatings or composites of nano TiO_2 with other dopants on metals for the photogenerated cathodic protection of metals under ultraviolet (UV) or visible light illumination. However, the application of TiO_2 nano coatings serving as anticorrosion measure has been limited by some technical bottleneck, including non uniform and defects for the coating. Especially, due to the wide band gap of TiO_2 (E_g=3.0-3.2eV), it is only excited by ultraviolet light (λ< 390 nm) so that the efficiency of light utilization to solar irradiation is very low, and the recombination rate of photogenerated e~--h~+ pairs in TiO_2 is high and the quantum efficiency is low. The technical problems result in the unefficient photocathodic protection performance of metals under both visible light illumination and dark conditions.
The main goal and motivation of this thesis are to develop various uniform and functional nano TiO_2 composite coatings, and to increase the quantum efficiency of TiO_2 to both UV and visible light excitation. An attempt is made to extend the life of the photo-generated electron-hole pairs and to enhance efficient cathodic protection performances in UV-visible illumination and dark conditions. The mechanism of the photo-generated cathodic protection is also discussed in the thesis. The main results and conclusions are summaried as following:
1. The sol-gel method and dip-coating technique have been developed to fabricate theultra fine particles coating of TiO_2, TiO_2-SnO_2 and N-TiO_2 at the room temperature.
The size and thickness of TiO_2 are crack-free, ultra purity and controllable, and the preparation method is simple and easy to be reproduced.
2. It is shown that the as-prepared nano TiO_2, films on metal own better anticorrosion performances, and the nano TiO_2 films can suppress the recombination of photo-generated electron-hole pairs. The efficient photo-cathodic protection of the N doped TiO_2 nanoparticle films is achieved under UV-visible wavelength spectra regions for the first time. It is indicated that the ultra fine nanoparticle coatings have a good quality of dual functions in anticorrosion of metals, that is, the corrosion protection as the barrier layers and photocathodic protection as a photoanode.
3. Highly density and well aligned uniform titanium oxide nanotubes have been fabricated by electrochemical anodic oxidation of a pure titanium substrate in fluorinated electrolyte solutions. The morphologies, composition, structure and photoelectrochemical performances have been studied by using SEM, XRD, UV-Vis, electrochemical methods etc., and the photochemical properties of doped TiO_2 nanotube arrays and their possible applications of anticorrosion for metals have been investigated systemically. It is noted that the TiO_2 nanotubes show a stronger absorption in the ultraviolet (UV) light range, the open-circuit potentials of 316 SS coupled with the TiO_2 nanotubes layers shift negatively under UV light irradiation (λ<380nm).
4. The photocathodic protection of the Fe-doped TiO_2-based nanotube layers has been evaluated through the electrochemical measurements under visible light irradiation and dark conditions. The effects of the electrolyte system, anodized time, heat treated temperature on its photoelectrochemical activity and photogenerated cathodic protection performances are emphatically investigated. It is found that the Fe-doped TiO_2 nanotubes show a stronger absorption in the 410-650nm range. The open-circuit potentials of 316 SS coupled with the Fe-doped TiO_2 nanotubes layers shift negatively under visible light irradiation (λ>400nm), and maintain negatively for a period even in dark condition. It is indicated that the Fe-doped TiO_2 nanotube layers are able to function effectively a photogenerated cathodic protection for metals under regular sunlight conditions and remain a durative cathodic protection even in the dark condition.
本论文侧重发展多种先进的TiO_2纳米复合膜材料和表面改性技术,采用溶胶凝胶法和浸渍提拉技术在316不锈钢及铜表面构筑纳米TiO_2薄膜及SnO_2-TiO_2、N-TiO_2复合膜,引入紫外光对薄膜进行改性。同时发展电化学阳极氧化法,在钛基体表面制备一层具有特殊纳米结构的TiO_2纳米管阵列和金属离子掺杂的TiO_2纳米管膜。利用SEM、XRD、XPS、UV-Vis等表征方法系统研究纳米薄膜的形貌、晶型、组成等。采用腐蚀电化学和光电化学相结合技术,测试膜层的光电化学性质,研究TiO_2复合颗粒膜及掺杂半导体纳米管阵列薄膜对金属基体的光生阴极保护作用。以期通过掺杂改性技术和利用具有奇特性质的纳米管阵列作为光阳极有效延长光生电子-空穴对的寿命,强化可见光范围内和暗态下持续有效的光生阴极保护的作用,并探明膜层光生阴极保护的作用机理。主要进展及研究成果如下:
1.对传统TiO_2溶胶制备方法进行了改进,简化实验操作程序,在室温下制备了颗粒尺寸可控的超微粒子TiO_2、TiO_2-SnO_2、N-TiO_2溶胶,各种光电化学技术研究在金属表面超薄纳米TiO_2复合掺杂颗粒膜在不同腐蚀性溶液体系中的耐腐蚀行为,同时考察溶液浓度、膜厚、掺杂等条件的影响,制备了有最佳耐蚀性的纳米膜,有效提高金属或合金的耐腐蚀性能,并探明纳米膜的抗腐蚀机理。
2.采用腐蚀电化学和光电化学方法研究纳米TiO_2膜及其复合膜的光电性能及影响因素。发现复合膜能够减缓光生电子空穴对电荷的复合,在紫外光照射下产生较强的光生电流;采用湿法实现了有效的N掺杂,N掺杂形成了新能级,通过N_(2P)与O_(2P)态的混合而导致TiO_2禁带宽度变窄,获得了良好的可见光响应。实现在紫外、可见光和暗态下高效的光生阴极保护,同时也使纳米膜和复合膜具有更强的阻挡层作用,发挥纳米复合膜的双重保护协同作用的功能。
3.在含有F~-的电解液体系中,采用电化学阳极氧化法成功地在钛基体表面制备了排列整齐、高度有序的TiO_2纳米管及Fe掺杂型纳米管阵列。采用光电化学联用系统研究纳米管阵列的光电响应特性,结果表明:以TiO_2纳米管阵列膜作为光生阳极时,在紫外光区(λ＜387m)有显著增强的光生电流响应。
4.采用在氟化电解液中直接加入含有Fe~(2+)掺杂物的方法,成功实现了纳米TiO_2的Fe掺杂,铁元素以Fe的氧化物或者Fe(Ⅲ)离子的形式接入半导体TiO_2的晶格中,窄化TiO_2带隙,使光谱响应扩展到波长大于400nm的可见光区,首次采用Fe掺杂的TiO_2纳米管阵列膜作为光生阳极研究光生阴极保护作用。测试发现:在紫外光和可见光照射下,TiO_2纳米管及Fe掺杂纳米管阵列膜层对316不锈钢有很好的光生阴极保护作用,暗态下,光生电极电位仍可维持较长的一段时间,能够继续发挥阴极保护作用。
Titania (TiO_2) is one of the most important semiconductor oxides because of its excellent photo-electrochemistry, photo-catalysis and good chemical stability. It can be used in many hi-tech applications including photocatalysis, gas sensors, solar cells, cathodic protection and etc. It is of great interest to develop TiO_2 coatings or composites of nano TiO_2 with other dopants on metals for the photogenerated cathodic protection of metals under ultraviolet (UV) or visible light illumination. However, the application of TiO_2 nano coatings serving as anticorrosion measure has been limited by some technical bottleneck, including non uniform and defects for the coating. Especially, due to the wide band gap of TiO_2 (E_g=3.0-3.2eV), it is only excited by ultraviolet light (λ< 390 nm) so that the efficiency of light utilization to solar irradiation is very low, and the recombination rate of photogenerated e~--h~+ pairs in TiO_2 is high and the quantum efficiency is low. The technical problems result in the unefficient photocathodic protection performance of metals under both visible light illumination and dark conditions.
The main goal and motivation of this thesis are to develop various uniform and functional nano TiO_2 composite coatings, and to increase the quantum efficiency of TiO_2 to both UV and visible light excitation. An attempt is made to extend the life of the photo-generated electron-hole pairs and to enhance efficient cathodic protection performances in UV-visible illumination and dark conditions. The mechanism of the photo-generated cathodic protection is also discussed in the thesis. The main results and conclusions are summaried as following:
1. The sol-gel method and dip-coating technique have been developed to fabricate theultra fine particles coating of TiO_2, TiO_2-SnO_2 and N-TiO_2 at the room temperature.
The size and thickness of TiO_2 are crack-free, ultra purity and controllable, and the preparation method is simple and easy to be reproduced.
2. It is shown that the as-prepared nano TiO_2, films on metal own better anticorrosion performances, and the nano TiO_2 films can suppress the recombination of photo-generated electron-hole pairs. The efficient photo-cathodic protection of the N doped TiO_2 nanoparticle films is achieved under UV-visible wavelength spectra regions for the first time. It is indicated that the ultra fine nanoparticle coatings have a good quality of dual functions in anticorrosion of metals, that is, the corrosion protection as the barrier layers and photocathodic protection as a photoanode.
3. Highly density and well aligned uniform titanium oxide nanotubes have been fabricated by electrochemical anodic oxidation of a pure titanium substrate in fluorinated electrolyte solutions. The morphologies, composition, structure and photoelectrochemical performances have been studied by using SEM, XRD, UV-Vis, electrochemical methods etc., and the photochemical properties of doped TiO_2 nanotube arrays and their possible applications of anticorrosion for metals have been investigated systemically. It is noted that the TiO_2 nanotubes show a stronger absorption in the ultraviolet (UV) light range, the open-circuit potentials of 316 SS coupled with the TiO_2 nanotubes layers shift negatively under UV light irradiation (λ<380nm).
4. The photocathodic protection of the Fe-doped TiO_2-based nanotube layers has been evaluated through the electrochemical measurements under visible light irradiation and dark conditions. The effects of the electrolyte system, anodized time, heat treated temperature on its photoelectrochemical activity and photogenerated cathodic protection performances are emphatically investigated. It is found that the Fe-doped TiO_2 nanotubes show a stronger absorption in the 410-650nm range. The open-circuit potentials of 316 SS coupled with the Fe-doped TiO_2 nanotubes layers shift negatively under visible light irradiation (λ>400nm), and maintain negatively for a period even in dark condition. It is indicated that the Fe-doped TiO_2 nanotube layers are able to function effectively a photogenerated cathodic protection for metals under regular sunlight conditions and remain a durative cathodic protection even in the dark condition.
引文
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