TiO_2基纳米复合纤维光催化材料的组分设计、制备及性能研究
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摘要
当今社会,能源危机和环境污染已成为亟待解决的全球性问题,半导体材料由于其在环境净化和新能源中的潜在应用逐渐引起了科学界的广泛关注。在半导体材料中,二氧化钛(TiO2)由于其原料易得、无毒、性能稳定等特点,与其它半导体材料相比具有明显的优势,对其进行深入研究有重要意义。随着纳米技术的发展,科学家们发现纳米级的TiO2在光催化降解污染物上比大颗粒的TiO2效率更高,将其制成纳米纤维后增加了催化剂与污染物的接触面积、缩短了光生载流子迁移到表面的时间,纳米纤维相比纳米颗粒更易复合化与回收利用。
静电纺丝已成为一种能快速制备连续、直径均匀的TiO2纳米纤维的常规方法。但TiO2纳米纤维光催化剂的催化效率距实际应用还有相当大的差距,主要原因是TiO2内部光生电子-空穴易复合导致其光催化活性还不够高,同时TiO2是一种宽带隙半导体,仅能利用太阳光中的紫外光。虽然已有工作制备了TiO2纳米纤维并对其进行了改进,提高了TiO2纳米纤维的催化能力,但开发新型高效、制备工艺简单、实用的光催化材料仍是我们努力的方向。从微观结构上讲,TiO2纳米纤维是由内部纳米颗粒按照一定方向团聚起来的,减小晶粒尺寸、增大比表面积、掺杂、与其他半导体耦合等方式均能进一步提升其光催化效率。本论文即是基于以上思路,以TiO2基纳米纤维为研究对象,通过对纤维内颗粒的原位结晶、掺杂、复合等研究来优化纳米纤维光催化剂的性能,主要研究内容与结果如下：
(1)以微流体法合成的TiO2纳米颗粒为增加相,将其纺入纳米纤维中。利用微流体技术,在一缩二乙二醇(DEG)介质中制备超细晶粒尺寸(约5.0nm)的锐钛矿相TiO2纳米晶,其比表面积高达314.5m2g-1。将其加入到聚乙烯吡咯烷酮(PVP)的乙醇溶液中制备出纺丝液并进行静电纺丝,得到Ti02纳米晶均匀分散的PVP纳米纤维复合物,可用于柔性自清洁材料、空气净化、过滤膜等方面。
(2)以钛酸四丁酯为钛源,将静电纺得到的含大量无定形Ti02颗粒的TiO2/PVP纳米复合纤维经水蒸气处理,得到锐钛矿相的TiO2/PVP纳米复合纤维,研究了水蒸气处理温度对纳米纤维内部颗粒结晶行为的影响。将PVP用有机溶剂溶解后,得到有机官能团修饰的超细结晶Ti02纳米晶(粒径约5-10nm),可作为填料加入到其它有机基体中,应用于光催化相关的领域中。
(3)制备W6+掺杂的Ti02纳米纤维,研究不同掺杂量对纳米纤维晶粒尺寸、比表面积、纤维直径的影响,将掺杂纳米纤维采用沉积的方式固定在石英管壁上,研究可见光照射下其对甲苯气体的矿化。研究结果表明：随着掺杂离子浓度的增加,纤维的粒径减小,比表面积较单组分TiO2纤维提高了1.28倍。最佳掺杂量为20wt%,此时甲苯气体的矿化度达到76.6%。
(4)采用特制的双孔纺丝喷丝头,制备肩并肩结构的TiO2/SnO2复合纳米纤维异质结,用SEM、TEM、N2等温吸附-脱附、XPS等对其进行表征,研究了异质结结构对促进电子和空穴的分离的影响。将Pt纳米晶负载在异质结构的TiO2/SnO2复合纳米纤维上,Pt优异的传导电子功能进一步提高了催化剂的活性。结果表明：表面负载有约1.0wt%Pt纳米晶的TiO2/SnO2复合纳米纤维其催化能力大于TiO2/SnO2复合纳米纤维及TiO2/Pt纳米纤维；Pt团簇在复合纤维表面分布均匀、稳定,4次循环利用后,催化剂的催化效率依然在90%以上。
(5)将Ti02纳米纤维在钨酸、双氧水的水溶液中水热处理,制备多级结构的TiO2/WO3复合纳米纤维。结果表明,经180℃水热处理12小时,引入晶种层的TiO2纳米纤维表面垂直生长了W03纳米棒,这种复合结构催化剂拓宽了Ti02的光谱响应范围,在可见光照射下该结构的催化剂对亚甲基蓝以及罗丹明的降解效率均优于单组分Ti02纳米纤维。
(6)采用改进的Hummers法制备出氧化石墨烯(GO),将其分散在有机溶剂氮氮二甲基甲酰胺(DMF)中,与钛酸四丁酯与PVP的乙醇溶液混合后,采用静电纺丝方法制备TiO2/GO复合纳米纤维,研究GO的添加量对复合纳米纤维光催化性能的影响。结果表明,添加GO后拓宽了Ti02对可见光的光谱响应范围,减少了纤维内部电子-空穴的复合。且随着GO含量的增加,Ti02晶粒尺寸逐渐减小。在可见光照射下,添加4.0wt%GO的复合光催化剂催化活性最高。
本文为改善Ti02基纳米纤维性能进行了多种尝试和深入研究,得到了几种新型高效的光催化材料,为静电纺丝法制备其它纳米复合纤维材料及拓展其应用范围提供了参考。
In nowadays, the energy crisis and environmental pollution have become a global issue to be addressed urgently. Semiconductor materials gradually caused widespread concern due to their potential applications in environmental purification and solving the energy problem. Among numerous semiconductors, titanium dioxide (TiO2) has obvious advantages over other semiconductors due to its low cost, non-toxic, and stable performance. With the development of nanotechnology, scientists have found that the nanoscaled TiO2photocatalyst has a higher efficiency for degradation of pollutants than that of TiO2in the form of larger particles. TiO2nanofibers behave finer grain size, increased specific surface area as well as the contact area between the catalyst and the pollutants, and the superior recycling ability comparing with TiO2nanoparticles.
In recent years, with the development of the electrospinning technique, a variety of inorganic oxides including TiO2have been prepared into nanofibrous structure. Electrospinning has become a conventional method for rapid preparation of continuous TiO2nanofibers with a uniform diameter. However, it is still a challenge to enhance the photocatalytic efficiency of these semiconductors to meet the practical application requirements because of the drawback of poor quantum yield caused by the fast recombination of photogenerated charge carriers (hole-electron pairs). TiO2is a wide band gap semiconductor only photoactivated under UV light irradiation. Although there is a lot of work to prepare modified TiO2to improve their catalytic activity, the development of new, efficient and practical photocatalytic materials with a simple preparation method is still the direction of our efforts. TiO2nanofibers were formed by the internal nanoparticles reunioning in a certain direction. Reducing size of the nanoparticles within the nanofibers, increasing the specific surface area and coupling with other semiconductor could further increase the UV/visible light catalytic ability of the nanofibers. Based on the above ideas, we optimize the performance of the nanofiber photocatalyst by the crystallization, doping and compositing of the nanoparticles within the nanofibers. Main contents and results are listed as follows:
(1) Prepared optimized and modified TiO2nanoparticles, and then added them in the spinning solution for preparing TiO2nanofibers. By the microfluidic technology, the TiO2nanocrystals were prepared with the crystallite size of5.0nm and a surface area of314.5m2g-1. The TiO2nanocrystals were monodispersed in the PVP nanofibers with the potential application in self-cleaning materials, air purification, and filtration membranes.
(2) The amorous TiO2nanoparticles/PVP composite nanofibers were treated by water vapor, and then the amorous TiO2in situ crystallized into anatase TiO2within the composite nanofibers. The effect of temperature on the crystallization was also studied. Dissolving the PVP by organic solution, the ultrafine TiO2nanoparticles (5-10nm) with their surfaces modified by organic function group could be added to other organic materials for application in catalysis.
(3) W-doped TiO2nanofibers were prepared. They behave finer crystallite size, stronger visible light absorbance, and larger surface area comparing with pure TiO2nanofibers. The nanofiber structured morphology on the quartz tube promotes the reaction rates for the gas-phase photo-oxidation of toluene. The concentrations of the produced CO2keep steady during the photodegradation process, indicating the practicality and operability for the whole experiment. This research is conducive to the development of novel photocatalytic materials to efficiently mineralize toxic gas pollutants including toluene for practical application.
(4) Heterostructured TiO2/SnO2nanofibers deposited with ultrafine Pt nanocrystals (Pt-TiO2/SnO2) were prepared by combining electrospinning and polyol reduced method. The samples have been characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), UV-vis diffuse reflection spectroscopy (DRS), photoluminescence spectra (PL) and nitrogen adsorption-desorption isotherm analysis. The results indicated that heterojunctions formed between TiO2fibers and SnO2fibers in the side-by-side structure with Pt nanocrystals uniformly deposited on them. The photocatalytic activity of Pt-TiO2/SnO2for the degradation of methylene blue was much higher than that of bare TiO2and SnO2nanofibers, which could be ascribed to the formation of heterojunctions in the TiO2/SnO2nanofibers and the rapid transportation of electrons to the surface by Pt nanocrystals.
(5) Hierarchically nanostructured TiO2/WO3photocatalyst was synthesized via the subsequent hydrothermal treatment of electrospun TiO2nanofibers in the presence of tungstic acid. The WO3nanorods with a diameter of about40nm and an average length of about150nm grew perpendicularly on the TiO2nanofibers. The TiO2/WO3heterostructures have larger surface area for adsorption of the pollutants, and WO3nanorods possess a single crystal structure, which facilitates the migration of the photogenerated electrons. Photocatalytic tests display that the TiO2/WO3heterostructures exhibit a remarkably higher degradation rate of organic pollutants than that of the bare TiO2nanofibers under visible light irradiation. The enhanced photocatalytic activity is attributed to the extended absorption in the visible light region and the effective charge separation derived from the coupling effect of TiO2and WO3nanocomposite.
(6) Graphene is a good conductor of electrons and cheaper compared to the noble metals. C in graphene and Ti in titanium dioxide are easy to form C-Ti bond to broaden the spectral response range of TiO2. GO was prepared by modified Hummers method and dispersed in an organic solvent of dimethylformamide (DMF), and was added at different concentrations to the TiO2nanofibers using electrospinning method. The results show that adding GO broadened the spectral response range of TiO2to visible light region. With increasing the content of graphene, TiO2grain size bacame finer. The composite nanofibers with4.0wt%GO show the highest catalytic activity under visible light irradiation.
Our study provides a feasible path to deal with the puzzles of the recombination of photogenerated electron-holes and the low visible photoactivity. Several new and efficient photocatalysts were developed in our work. Improving the performance of the nanofibers by optimization design of internal nanoparticles provides a reference for the use of electrospinning method to prepare other oxide nanofibers and expand its range of applications.
静电纺丝已成为一种能快速制备连续、直径均匀的TiO2纳米纤维的常规方法。但TiO2纳米纤维光催化剂的催化效率距实际应用还有相当大的差距,主要原因是TiO2内部光生电子-空穴易复合导致其光催化活性还不够高,同时TiO2是一种宽带隙半导体,仅能利用太阳光中的紫外光。虽然已有工作制备了TiO2纳米纤维并对其进行了改进,提高了TiO2纳米纤维的催化能力,但开发新型高效、制备工艺简单、实用的光催化材料仍是我们努力的方向。从微观结构上讲,TiO2纳米纤维是由内部纳米颗粒按照一定方向团聚起来的,减小晶粒尺寸、增大比表面积、掺杂、与其他半导体耦合等方式均能进一步提升其光催化效率。本论文即是基于以上思路,以TiO2基纳米纤维为研究对象,通过对纤维内颗粒的原位结晶、掺杂、复合等研究来优化纳米纤维光催化剂的性能,主要研究内容与结果如下：
(1)以微流体法合成的TiO2纳米颗粒为增加相,将其纺入纳米纤维中。利用微流体技术,在一缩二乙二醇(DEG)介质中制备超细晶粒尺寸(约5.0nm)的锐钛矿相TiO2纳米晶,其比表面积高达314.5m2g-1。将其加入到聚乙烯吡咯烷酮(PVP)的乙醇溶液中制备出纺丝液并进行静电纺丝,得到Ti02纳米晶均匀分散的PVP纳米纤维复合物,可用于柔性自清洁材料、空气净化、过滤膜等方面。
(2)以钛酸四丁酯为钛源,将静电纺得到的含大量无定形Ti02颗粒的TiO2/PVP纳米复合纤维经水蒸气处理,得到锐钛矿相的TiO2/PVP纳米复合纤维,研究了水蒸气处理温度对纳米纤维内部颗粒结晶行为的影响。将PVP用有机溶剂溶解后,得到有机官能团修饰的超细结晶Ti02纳米晶(粒径约5-10nm),可作为填料加入到其它有机基体中,应用于光催化相关的领域中。
(3)制备W6+掺杂的Ti02纳米纤维,研究不同掺杂量对纳米纤维晶粒尺寸、比表面积、纤维直径的影响,将掺杂纳米纤维采用沉积的方式固定在石英管壁上,研究可见光照射下其对甲苯气体的矿化。研究结果表明：随着掺杂离子浓度的增加,纤维的粒径减小,比表面积较单组分TiO2纤维提高了1.28倍。最佳掺杂量为20wt%,此时甲苯气体的矿化度达到76.6%。
(4)采用特制的双孔纺丝喷丝头,制备肩并肩结构的TiO2/SnO2复合纳米纤维异质结,用SEM、TEM、N2等温吸附-脱附、XPS等对其进行表征,研究了异质结结构对促进电子和空穴的分离的影响。将Pt纳米晶负载在异质结构的TiO2/SnO2复合纳米纤维上,Pt优异的传导电子功能进一步提高了催化剂的活性。结果表明：表面负载有约1.0wt%Pt纳米晶的TiO2/SnO2复合纳米纤维其催化能力大于TiO2/SnO2复合纳米纤维及TiO2/Pt纳米纤维；Pt团簇在复合纤维表面分布均匀、稳定,4次循环利用后,催化剂的催化效率依然在90%以上。
(5)将Ti02纳米纤维在钨酸、双氧水的水溶液中水热处理,制备多级结构的TiO2/WO3复合纳米纤维。结果表明,经180℃水热处理12小时,引入晶种层的TiO2纳米纤维表面垂直生长了W03纳米棒,这种复合结构催化剂拓宽了Ti02的光谱响应范围,在可见光照射下该结构的催化剂对亚甲基蓝以及罗丹明的降解效率均优于单组分Ti02纳米纤维。
(6)采用改进的Hummers法制备出氧化石墨烯(GO),将其分散在有机溶剂氮氮二甲基甲酰胺(DMF)中,与钛酸四丁酯与PVP的乙醇溶液混合后,采用静电纺丝方法制备TiO2/GO复合纳米纤维,研究GO的添加量对复合纳米纤维光催化性能的影响。结果表明,添加GO后拓宽了Ti02对可见光的光谱响应范围,减少了纤维内部电子-空穴的复合。且随着GO含量的增加,Ti02晶粒尺寸逐渐减小。在可见光照射下,添加4.0wt%GO的复合光催化剂催化活性最高。
本文为改善Ti02基纳米纤维性能进行了多种尝试和深入研究,得到了几种新型高效的光催化材料,为静电纺丝法制备其它纳米复合纤维材料及拓展其应用范围提供了参考。
In nowadays, the energy crisis and environmental pollution have become a global issue to be addressed urgently. Semiconductor materials gradually caused widespread concern due to their potential applications in environmental purification and solving the energy problem. Among numerous semiconductors, titanium dioxide (TiO2) has obvious advantages over other semiconductors due to its low cost, non-toxic, and stable performance. With the development of nanotechnology, scientists have found that the nanoscaled TiO2photocatalyst has a higher efficiency for degradation of pollutants than that of TiO2in the form of larger particles. TiO2nanofibers behave finer grain size, increased specific surface area as well as the contact area between the catalyst and the pollutants, and the superior recycling ability comparing with TiO2nanoparticles.
In recent years, with the development of the electrospinning technique, a variety of inorganic oxides including TiO2have been prepared into nanofibrous structure. Electrospinning has become a conventional method for rapid preparation of continuous TiO2nanofibers with a uniform diameter. However, it is still a challenge to enhance the photocatalytic efficiency of these semiconductors to meet the practical application requirements because of the drawback of poor quantum yield caused by the fast recombination of photogenerated charge carriers (hole-electron pairs). TiO2is a wide band gap semiconductor only photoactivated under UV light irradiation. Although there is a lot of work to prepare modified TiO2to improve their catalytic activity, the development of new, efficient and practical photocatalytic materials with a simple preparation method is still the direction of our efforts. TiO2nanofibers were formed by the internal nanoparticles reunioning in a certain direction. Reducing size of the nanoparticles within the nanofibers, increasing the specific surface area and coupling with other semiconductor could further increase the UV/visible light catalytic ability of the nanofibers. Based on the above ideas, we optimize the performance of the nanofiber photocatalyst by the crystallization, doping and compositing of the nanoparticles within the nanofibers. Main contents and results are listed as follows:
(1) Prepared optimized and modified TiO2nanoparticles, and then added them in the spinning solution for preparing TiO2nanofibers. By the microfluidic technology, the TiO2nanocrystals were prepared with the crystallite size of5.0nm and a surface area of314.5m2g-1. The TiO2nanocrystals were monodispersed in the PVP nanofibers with the potential application in self-cleaning materials, air purification, and filtration membranes.
(2) The amorous TiO2nanoparticles/PVP composite nanofibers were treated by water vapor, and then the amorous TiO2in situ crystallized into anatase TiO2within the composite nanofibers. The effect of temperature on the crystallization was also studied. Dissolving the PVP by organic solution, the ultrafine TiO2nanoparticles (5-10nm) with their surfaces modified by organic function group could be added to other organic materials for application in catalysis.
(3) W-doped TiO2nanofibers were prepared. They behave finer crystallite size, stronger visible light absorbance, and larger surface area comparing with pure TiO2nanofibers. The nanofiber structured morphology on the quartz tube promotes the reaction rates for the gas-phase photo-oxidation of toluene. The concentrations of the produced CO2keep steady during the photodegradation process, indicating the practicality and operability for the whole experiment. This research is conducive to the development of novel photocatalytic materials to efficiently mineralize toxic gas pollutants including toluene for practical application.
(4) Heterostructured TiO2/SnO2nanofibers deposited with ultrafine Pt nanocrystals (Pt-TiO2/SnO2) were prepared by combining electrospinning and polyol reduced method. The samples have been characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), UV-vis diffuse reflection spectroscopy (DRS), photoluminescence spectra (PL) and nitrogen adsorption-desorption isotherm analysis. The results indicated that heterojunctions formed between TiO2fibers and SnO2fibers in the side-by-side structure with Pt nanocrystals uniformly deposited on them. The photocatalytic activity of Pt-TiO2/SnO2for the degradation of methylene blue was much higher than that of bare TiO2and SnO2nanofibers, which could be ascribed to the formation of heterojunctions in the TiO2/SnO2nanofibers and the rapid transportation of electrons to the surface by Pt nanocrystals.
(5) Hierarchically nanostructured TiO2/WO3photocatalyst was synthesized via the subsequent hydrothermal treatment of electrospun TiO2nanofibers in the presence of tungstic acid. The WO3nanorods with a diameter of about40nm and an average length of about150nm grew perpendicularly on the TiO2nanofibers. The TiO2/WO3heterostructures have larger surface area for adsorption of the pollutants, and WO3nanorods possess a single crystal structure, which facilitates the migration of the photogenerated electrons. Photocatalytic tests display that the TiO2/WO3heterostructures exhibit a remarkably higher degradation rate of organic pollutants than that of the bare TiO2nanofibers under visible light irradiation. The enhanced photocatalytic activity is attributed to the extended absorption in the visible light region and the effective charge separation derived from the coupling effect of TiO2and WO3nanocomposite.
(6) Graphene is a good conductor of electrons and cheaper compared to the noble metals. C in graphene and Ti in titanium dioxide are easy to form C-Ti bond to broaden the spectral response range of TiO2. GO was prepared by modified Hummers method and dispersed in an organic solvent of dimethylformamide (DMF), and was added at different concentrations to the TiO2nanofibers using electrospinning method. The results show that adding GO broadened the spectral response range of TiO2to visible light region. With increasing the content of graphene, TiO2grain size bacame finer. The composite nanofibers with4.0wt%GO show the highest catalytic activity under visible light irradiation.
Our study provides a feasible path to deal with the puzzles of the recombination of photogenerated electron-holes and the low visible photoactivity. Several new and efficient photocatalysts were developed in our work. Improving the performance of the nanofibers by optimization design of internal nanoparticles provides a reference for the use of electrospinning method to prepare other oxide nanofibers and expand its range of applications.
引文
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