BiOX（X=Cl、I）/TiO_2纳米复合阵列的可控构筑及其有机污染物降解性能研究
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摘要
半导体光催化技术具有解决环境污染和能源短缺问题的潜在能力，是当今材料、环境和能源等领域的研究前沿和热点。高性能光催化材料的研发一直是制约该技术应用的难点与瓶颈，如何增强其光催化性能和拓展其可见光响应范围成为亟待解决的两大关键科学问题。本文以铋系层状化合物BiOX（X=Cl、Br、I）和有序TiO2纳米管阵列（TiO2nanotube arrays，TNTAs）应用于光催化技术为目的，进行新型高性能光催化材料的可控制备与有机污染物降解性能研究：采用有效方法将BiOX（X=Cl、I）纳米结构导入有序TiO2纳米管阵列，发展了新型BiOX（X=Cl、I）/TiO2纳米复合阵列薄膜光催化材料；针对BiOCl/TiO2体系仅对紫外光响应的应用瓶颈，将Ag纳米颗粒进一步导入BiOCl/TiO2体系，调控构筑了可见光响应的新型Ag-BiOCl/TiO2纳米复合阵列薄膜光催化材料；此外，通过引入可生物降解的表面活性剂PVA，发展了一种简易且环境友好的微纳分级结构BiOCl光催化材料的合成方法。全文主要研究结果如下：
1、采用电化学阳极氧化法，通过增大电解液中H2O含量至10vol.%，制备出适于负载改性、超大比表面、管与管相互分离的有序TiO2纳米管阵列薄膜基体；进而采用化学浴循环浸渍沉积法，通过调节浸渍温度、单次浸渍时间和浸渍循环次数等参数调控制备了具有独特片–管结构的BiOCl/TiO2纳米复合阵列薄膜光催化材料；通过对模拟有机污染物甲基橙（MO）的光催化降解实验来评价目标材料的有机污染物降解性能，利用瞬时光电流响应测试进一步分析目标材料的光电性能，结果表明：浸渍温度为60℃、单次浸渍时间为5min条件下，循环浸渍2次所获得的BiOCl/TNTAs-2样品的紫外光催化活性和效率最高，明显优于TNTAs基体，并且其性质稳定、可重复利用，相同测试条件下的光电流密度最大，其原因主要是：①BiOCl/TiO2异质结构促进了光生电子-空穴对的有效分离；②BiOCl/TNTAs-2样品中不仅BiOCl负载适量，负载分布均匀弥散，而且其负载后的微观结构（纳米管中空结构和基本连通的纳米管间隙）不仅有效提高了催化剂表面对入射光的吸收和利用，并且有利于后续待降解有机物溶液的浸入与扩散；③BiOCl纳米片的适量负载显著增大了TNTAs基体的比表面积，从而有效增大了待降解有机物分子与催化剂表面的接触面积。
2、沿用化学浴循环浸渍沉积法将窄带隙BiOI纳米片负载于TiO2纳米管内外表面，调控制备了新型片–管结构、可见光响应的BiOI/TiO2纳米复合阵列薄膜光催化材料。通过调节循环浸渍次数来调控BiOI负载效果，其中经过5个浸渍循环所获得的5-BiOI/TNTAs样品在可见光范围内表现出最高的光学吸收特性，对模拟有机污染物MO的光电催化降解活性和效率最高，并且性质稳定、可重复利用，相同测试条件下的光电流密度最大，其主要原因是：①负载的窄带隙BiOI纳米片对可见光的有效吸收提高了可见光条件下的载流子产率；②BiOI/TiO2异质结构对光生电子-空穴对的分离作用有效降低了光生载流子的复合几率；③5-BiOI/TNTAs样品中BiOI负载适量，负载分布均匀弥散，其负载后的微观结构（纳米管中空结构和基本连通的纳米管间隙）不仅可以提高催化剂表面对入射光的吸收与利用，而且也有利于待降解有机物溶液的浸入与扩散；④适量BiOI纳米片的弥散负载有效增大了TNTAs基体的比表面积，从而增大了待降解有机物分子与催化剂表面的接触面积；⑤外加电场作用可以有效促进光生载流子分离与迁移。
3、采用原位光还原法和化学浴循环浸渍沉积法将Ag纳米颗粒和BiOCl纳米片先后负载于有序TiO2纳米管内外表面，调控制备了可见光响应的新型Ag-BiOCl/TiO2纳米复合阵列（Ag-BiOCl/TNTAs）薄膜光催化材料：Ag-BiOCl/TNTAs具有由fcc结构Ag0、锐钛矿TiO2和四方相BiOCl组成的Ag/TiO2、Ag/BiOCl和BiOCl/TiO2多种复合结构，Ag颗粒粒径主要集中在10~15nm，BiOCl纳米片尺寸约20~30nm；与TNTAs、BiOCl/TNTAs-2和Ag/TNTAs相比，Ag-BiOCl/TNTAs在可见光范围内表现出最高的光学吸收特性，在紫外和模拟日光条件下对模拟有机污染物MO的光催化降解活性最高，其主要原因是：①Ag纳米颗粒的SPR效应及其对光生电子的俘获作用显著提高了TNTAs基体对可见光的吸收及光催化活性；②BiOCl纳米片进一步导入后使目标Ag-BiOCl/TNTAs中新增Ag/BiOCl复合结构，从而增大了Ag/半导体（TiO2与BiOCl）接触面积，可以更高效地发挥Ag的SPR效应及其对光生电子的俘获作用；③BiOCl纳米片进一步导入后新增的BiOCl/TiO2异质结构对光生载流子的分离作用以及使目标Ag-BiOCl/TNTAs比表面积的进一步增大均有利于光催化活性的进一步提高。
4、通过在NaCl水溶液滴入Bi(NO3)3-HNO3溶液过程中引入一种可生物降解的表面活性剂PVA，发展了一种简易且环境友好的三维微纳分级结构BiOCl光催化材料的合成方法：与常规BiOCl纳米片相比，所合成的花状分级结构BiOCl具有多孔特性、更大的比表面积以及更强的光吸收能力，因而对模拟有机污染物MO表现出更高的紫外光催化降解活性与效率，并且性质稳定，可重复利用；PVA引入量会显著影响目标分级结构BiOCl材料的微结构和光催化活性，根据光催化性能测试结果确定了优选的PVA引入量。
Semiconductor photocatalysis promises great potential in solving environmentalpollution and energy shortage problems, and has become the research forefront andhotspot in the fields of materials, environment and energy. However, shortage of highperformance photocatalyst has been the bottleneck in booming the photocatalysisapplications. Hence, how to enhance the photocatalytic performance and expand thevisible-light response range of the catalyst have been the two key scientific issues.This research work is mainly focused on the controllable synthesis and organicpollutant degradation performance of novel high performance photocatalysts byhybridizing layered bismuth-based compounds of BiOX(X=Cl, Br, I) andhighly-ordered TiO2nanotube arrays (TNTAs) for photocatalysis application. Novelhigh performance film catalyst of BiOX(X=Cl, I)/TiO2nanocomposite arrays aredeveloped by introducing nanostructured BiOX(X=Cl, I) into highly-ordered TNTAs.Considering the application bottleneck of BiOCl/TiO2system which only responses toUV light, Ag nanoparticles are introduced into the BiOCl/TiO2system to obtainAg-BiOCl/TiO2nanocomposite arrays with highly enhanced visible-lightphotocatalytic performance. In addition, a facile and environment friendly approach tosynthesize unique hierarchical BiOCl photocatalyst is developed with the assistance ofa biodegradable surfactant Polyvinyl Alcohol (PVA). Main research results in thiswork can be summarized as following:
1. Novel flake-tube structured film catalyst of BiOCl/TiO2nanocomposite arrays(BiOCl/TNTAs) is successfully prepared by uniformly loading BiOCl nanoflakes ontoboth outer and inner walls of well-separated TiO2nanotubes (NTs) via anodization inthe10vol.%H2O electrolyte followed by sequential chemical bath deposition(S-CBD) method. The loading effect can be fine-tuned by adjusting depositiontemperature, deposition time and cycle times. The organic pollutant degradationperformance of as-prepared BiOCl/TNTAs samples is evaluated by the photocatalytic(PC) degradation test toward the methyl orange (MO) solutions under UV lightirradiation. In addition, the UV light PC performance of BiOCl/TNTAs samples isfurther confirmed by the transient photocurrent response test. The results from thecurrent study reveal that the BiOCl/TNTAs-2sample prepared with depositiontemperature of60℃, single deposition time of5min and2deposition cycles exhibits the best PC activity, favorable stability and the highest photocurrent density among allthe BiOCl/TNTAs samples, revealing that loading proper amount of BiOCl nanoflakescan effectively improve the PC performance and photoelectric properties of TNTAs,and over loading may lead to the decline of PC activity and photoelectric performance.Synergistic effect of the following factors may contribute to the remarkably enhancedPC activity and photoelectric property for the BiOCl/TNTAs-2sample including:①the formation of BiOCl/TiO2heterojunction for promoting the separation ofphoto-induced electron-hole pairs;②3D connected intertube spacing system andopen tube-mouth structure may benefit the light absorption and utilization, as well asthe convenient immersion and diffusion of the solution to be degraded;③largerspecific surface area resulted from the dispersion of tiny nanosized BiOCl nanoflakesonto the surface of TiO2NTs for increasing the contact area between the organicmolecules and catalyst.
2. Flake-tube structured film catalyst of BiOI/TiO2nanocomposite arrays(BiOI/TNTAs) is successfully prepared by loading large amounts of narrow band gapBiOI nanoflakes onto both outer and inner walls of well-separated TiO2NTs usinganodization followed by S-CBD method. The loading effect can be fine-tuned byadjusting deposition cycle times. The results from the current study reveal that undervisible-light irradiation (λ>420nm), the5-BiOI/TNTAs sample with five depositioncycles exhibits the best photoelectrocatalytic (PEC) activity and efficiency, favorablestability in the MO degradation test, and shows the highest photocurrent densityamong all the BiOI/TNTAs heterostructured samples. The combined effects of severalfactors may contribute to the remarkable visible-light PEC performance for the5-BiOI/TNTAs sample including:①strong visible-light absorption by BiOI forraising the carriers yield;②the formation of BiOI/TiO2heterojunction for promotingthe separation of photo-induced electron-hole pairs;③3D connected intertubespacing system and open tube-mouth structure benefit the light absorption andutilization, as well as the convenient immersion of the organic solution;④largerspecific surface area resulted from the dispersion of tiny BiOI nanoflakes on thesurface of TiO2NTs for increasing the contact area between the organic molecules andcatalyst;⑤the applied external electrostatic field for promoting the separation andtransfer of carriers.
3. Novel film photocatalyst of Ag-BiOCl/TiO2nanocomposite arrays(Ag-BiOCl/TNTAs) is successfully prepared by loading Ag nanoparticles and BiOCl nanoflakes successively onto the surface of TiO2NTs via in situ light reductionfollowed by S-CBD method. Ag-BiOCl/TNTAs film catalyst contains Ag/TiO2,Ag/BiOCl and BiOCl/TiO2composite structures comprised of fcc structure Ag,anatase phaseTiO2and tetragonal phase BiOCl. Ag nanoparticle size is about10~15nm, and the BiOCl nanflake size is about20~30nm. Compared with TNTAs,BiOCl/TNTAs-2and Ag/TNTAs samples, Ag-BiOCl/TNTA sample shows the highestoptical absorption properties in the visible light region, and exhibits the highest PCactivity under both UV and simulated sunlight irradiation towards the degradation ofMO solution. Main causes are proposed as follows:①SPR effect and electroncapturing function of Ag nanoparticles enhance the visible light absorption and PCactivity of Ag/TNTAs;②The contact area of Ag/semiconductor increases due to theformation of Ag/BiOCl junction in the Ag-BiOCl/TNTAs by further introducingBiOCl nanoflakes into Ag/TNTAs, thus full playing the SPR effect and electroncapturing function of Ag nanoparticles;③larger specific surface area and theformation of BiOCl/TiO2junction may further enhance the PC activity of theAg-BiOCl/TNTAs by further introducing BiOCl nanoflakes into Ag/TNTAs.
4. A facile and environment friendly approach to synthesize unique hierarchicalBiOCl photocatalyst is developed with the assistance of a biodegradable surfactantPolyvinyl Alcohol (PVA). Compared with common BiOCl nanosheets synthesized inthe absence of PVA, the resulting hierarchical BiOCl photocatalyst demonstratessignificantly enhanced PC activity towards the degradation of MO solution due to itslarge specific surface area, porosity, and suitable band gap for improving the lightabsorption and utilization, dye molecules adsorption, and the transportation ofreactants and products. The amount of PVA has obvious influence on themicrostructures and PC performance of the target hierarchical BiOCl catalytst. Theoptimized amount of PVA added into the reaction system is determined according tothe results of the PC performance test.
1、采用电化学阳极氧化法，通过增大电解液中H2O含量至10vol.%，制备出适于负载改性、超大比表面、管与管相互分离的有序TiO2纳米管阵列薄膜基体；进而采用化学浴循环浸渍沉积法，通过调节浸渍温度、单次浸渍时间和浸渍循环次数等参数调控制备了具有独特片–管结构的BiOCl/TiO2纳米复合阵列薄膜光催化材料；通过对模拟有机污染物甲基橙（MO）的光催化降解实验来评价目标材料的有机污染物降解性能，利用瞬时光电流响应测试进一步分析目标材料的光电性能，结果表明：浸渍温度为60℃、单次浸渍时间为5min条件下，循环浸渍2次所获得的BiOCl/TNTAs-2样品的紫外光催化活性和效率最高，明显优于TNTAs基体，并且其性质稳定、可重复利用，相同测试条件下的光电流密度最大，其原因主要是：①BiOCl/TiO2异质结构促进了光生电子-空穴对的有效分离；②BiOCl/TNTAs-2样品中不仅BiOCl负载适量，负载分布均匀弥散，而且其负载后的微观结构（纳米管中空结构和基本连通的纳米管间隙）不仅有效提高了催化剂表面对入射光的吸收和利用，并且有利于后续待降解有机物溶液的浸入与扩散；③BiOCl纳米片的适量负载显著增大了TNTAs基体的比表面积，从而有效增大了待降解有机物分子与催化剂表面的接触面积。
2、沿用化学浴循环浸渍沉积法将窄带隙BiOI纳米片负载于TiO2纳米管内外表面，调控制备了新型片–管结构、可见光响应的BiOI/TiO2纳米复合阵列薄膜光催化材料。通过调节循环浸渍次数来调控BiOI负载效果，其中经过5个浸渍循环所获得的5-BiOI/TNTAs样品在可见光范围内表现出最高的光学吸收特性，对模拟有机污染物MO的光电催化降解活性和效率最高，并且性质稳定、可重复利用，相同测试条件下的光电流密度最大，其主要原因是：①负载的窄带隙BiOI纳米片对可见光的有效吸收提高了可见光条件下的载流子产率；②BiOI/TiO2异质结构对光生电子-空穴对的分离作用有效降低了光生载流子的复合几率；③5-BiOI/TNTAs样品中BiOI负载适量，负载分布均匀弥散，其负载后的微观结构（纳米管中空结构和基本连通的纳米管间隙）不仅可以提高催化剂表面对入射光的吸收与利用，而且也有利于待降解有机物溶液的浸入与扩散；④适量BiOI纳米片的弥散负载有效增大了TNTAs基体的比表面积，从而增大了待降解有机物分子与催化剂表面的接触面积；⑤外加电场作用可以有效促进光生载流子分离与迁移。
3、采用原位光还原法和化学浴循环浸渍沉积法将Ag纳米颗粒和BiOCl纳米片先后负载于有序TiO2纳米管内外表面，调控制备了可见光响应的新型Ag-BiOCl/TiO2纳米复合阵列（Ag-BiOCl/TNTAs）薄膜光催化材料：Ag-BiOCl/TNTAs具有由fcc结构Ag0、锐钛矿TiO2和四方相BiOCl组成的Ag/TiO2、Ag/BiOCl和BiOCl/TiO2多种复合结构，Ag颗粒粒径主要集中在10~15nm，BiOCl纳米片尺寸约20~30nm；与TNTAs、BiOCl/TNTAs-2和Ag/TNTAs相比，Ag-BiOCl/TNTAs在可见光范围内表现出最高的光学吸收特性，在紫外和模拟日光条件下对模拟有机污染物MO的光催化降解活性最高，其主要原因是：①Ag纳米颗粒的SPR效应及其对光生电子的俘获作用显著提高了TNTAs基体对可见光的吸收及光催化活性；②BiOCl纳米片进一步导入后使目标Ag-BiOCl/TNTAs中新增Ag/BiOCl复合结构，从而增大了Ag/半导体（TiO2与BiOCl）接触面积，可以更高效地发挥Ag的SPR效应及其对光生电子的俘获作用；③BiOCl纳米片进一步导入后新增的BiOCl/TiO2异质结构对光生载流子的分离作用以及使目标Ag-BiOCl/TNTAs比表面积的进一步增大均有利于光催化活性的进一步提高。
4、通过在NaCl水溶液滴入Bi(NO3)3-HNO3溶液过程中引入一种可生物降解的表面活性剂PVA，发展了一种简易且环境友好的三维微纳分级结构BiOCl光催化材料的合成方法：与常规BiOCl纳米片相比，所合成的花状分级结构BiOCl具有多孔特性、更大的比表面积以及更强的光吸收能力，因而对模拟有机污染物MO表现出更高的紫外光催化降解活性与效率，并且性质稳定，可重复利用；PVA引入量会显著影响目标分级结构BiOCl材料的微结构和光催化活性，根据光催化性能测试结果确定了优选的PVA引入量。
Semiconductor photocatalysis promises great potential in solving environmentalpollution and energy shortage problems, and has become the research forefront andhotspot in the fields of materials, environment and energy. However, shortage of highperformance photocatalyst has been the bottleneck in booming the photocatalysisapplications. Hence, how to enhance the photocatalytic performance and expand thevisible-light response range of the catalyst have been the two key scientific issues.This research work is mainly focused on the controllable synthesis and organicpollutant degradation performance of novel high performance photocatalysts byhybridizing layered bismuth-based compounds of BiOX(X=Cl, Br, I) andhighly-ordered TiO2nanotube arrays (TNTAs) for photocatalysis application. Novelhigh performance film catalyst of BiOX(X=Cl, I)/TiO2nanocomposite arrays aredeveloped by introducing nanostructured BiOX(X=Cl, I) into highly-ordered TNTAs.Considering the application bottleneck of BiOCl/TiO2system which only responses toUV light, Ag nanoparticles are introduced into the BiOCl/TiO2system to obtainAg-BiOCl/TiO2nanocomposite arrays with highly enhanced visible-lightphotocatalytic performance. In addition, a facile and environment friendly approach tosynthesize unique hierarchical BiOCl photocatalyst is developed with the assistance ofa biodegradable surfactant Polyvinyl Alcohol (PVA). Main research results in thiswork can be summarized as following:
1. Novel flake-tube structured film catalyst of BiOCl/TiO2nanocomposite arrays(BiOCl/TNTAs) is successfully prepared by uniformly loading BiOCl nanoflakes ontoboth outer and inner walls of well-separated TiO2nanotubes (NTs) via anodization inthe10vol.%H2O electrolyte followed by sequential chemical bath deposition(S-CBD) method. The loading effect can be fine-tuned by adjusting depositiontemperature, deposition time and cycle times. The organic pollutant degradationperformance of as-prepared BiOCl/TNTAs samples is evaluated by the photocatalytic(PC) degradation test toward the methyl orange (MO) solutions under UV lightirradiation. In addition, the UV light PC performance of BiOCl/TNTAs samples isfurther confirmed by the transient photocurrent response test. The results from thecurrent study reveal that the BiOCl/TNTAs-2sample prepared with depositiontemperature of60℃, single deposition time of5min and2deposition cycles exhibits the best PC activity, favorable stability and the highest photocurrent density among allthe BiOCl/TNTAs samples, revealing that loading proper amount of BiOCl nanoflakescan effectively improve the PC performance and photoelectric properties of TNTAs,and over loading may lead to the decline of PC activity and photoelectric performance.Synergistic effect of the following factors may contribute to the remarkably enhancedPC activity and photoelectric property for the BiOCl/TNTAs-2sample including:①the formation of BiOCl/TiO2heterojunction for promoting the separation ofphoto-induced electron-hole pairs;②3D connected intertube spacing system andopen tube-mouth structure may benefit the light absorption and utilization, as well asthe convenient immersion and diffusion of the solution to be degraded;③largerspecific surface area resulted from the dispersion of tiny nanosized BiOCl nanoflakesonto the surface of TiO2NTs for increasing the contact area between the organicmolecules and catalyst.
2. Flake-tube structured film catalyst of BiOI/TiO2nanocomposite arrays(BiOI/TNTAs) is successfully prepared by loading large amounts of narrow band gapBiOI nanoflakes onto both outer and inner walls of well-separated TiO2NTs usinganodization followed by S-CBD method. The loading effect can be fine-tuned byadjusting deposition cycle times. The results from the current study reveal that undervisible-light irradiation (λ>420nm), the5-BiOI/TNTAs sample with five depositioncycles exhibits the best photoelectrocatalytic (PEC) activity and efficiency, favorablestability in the MO degradation test, and shows the highest photocurrent densityamong all the BiOI/TNTAs heterostructured samples. The combined effects of severalfactors may contribute to the remarkable visible-light PEC performance for the5-BiOI/TNTAs sample including:①strong visible-light absorption by BiOI forraising the carriers yield;②the formation of BiOI/TiO2heterojunction for promotingthe separation of photo-induced electron-hole pairs;③3D connected intertubespacing system and open tube-mouth structure benefit the light absorption andutilization, as well as the convenient immersion of the organic solution;④largerspecific surface area resulted from the dispersion of tiny BiOI nanoflakes on thesurface of TiO2NTs for increasing the contact area between the organic molecules andcatalyst;⑤the applied external electrostatic field for promoting the separation andtransfer of carriers.
3. Novel film photocatalyst of Ag-BiOCl/TiO2nanocomposite arrays(Ag-BiOCl/TNTAs) is successfully prepared by loading Ag nanoparticles and BiOCl nanoflakes successively onto the surface of TiO2NTs via in situ light reductionfollowed by S-CBD method. Ag-BiOCl/TNTAs film catalyst contains Ag/TiO2,Ag/BiOCl and BiOCl/TiO2composite structures comprised of fcc structure Ag,anatase phaseTiO2and tetragonal phase BiOCl. Ag nanoparticle size is about10~15nm, and the BiOCl nanflake size is about20~30nm. Compared with TNTAs,BiOCl/TNTAs-2and Ag/TNTAs samples, Ag-BiOCl/TNTA sample shows the highestoptical absorption properties in the visible light region, and exhibits the highest PCactivity under both UV and simulated sunlight irradiation towards the degradation ofMO solution. Main causes are proposed as follows:①SPR effect and electroncapturing function of Ag nanoparticles enhance the visible light absorption and PCactivity of Ag/TNTAs;②The contact area of Ag/semiconductor increases due to theformation of Ag/BiOCl junction in the Ag-BiOCl/TNTAs by further introducingBiOCl nanoflakes into Ag/TNTAs, thus full playing the SPR effect and electroncapturing function of Ag nanoparticles;③larger specific surface area and theformation of BiOCl/TiO2junction may further enhance the PC activity of theAg-BiOCl/TNTAs by further introducing BiOCl nanoflakes into Ag/TNTAs.
4. A facile and environment friendly approach to synthesize unique hierarchicalBiOCl photocatalyst is developed with the assistance of a biodegradable surfactantPolyvinyl Alcohol (PVA). Compared with common BiOCl nanosheets synthesized inthe absence of PVA, the resulting hierarchical BiOCl photocatalyst demonstratessignificantly enhanced PC activity towards the degradation of MO solution due to itslarge specific surface area, porosity, and suitable band gap for improving the lightabsorption and utilization, dye molecules adsorption, and the transportation ofreactants and products. The amount of PVA has obvious influence on themicrostructures and PC performance of the target hierarchical BiOCl catalytst. Theoptimized amount of PVA added into the reaction system is determined according tothe results of the PC performance test.
引文
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