铋基复合半导体的液相可控制备及光催化性质研究
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摘要
本论文围绕新型铋基复合材料的制备、表征及其光催化性能等方面展开研究,内容主要包括以下三个部分:
(1)通过混合溶剂热路线,在AOT参与下,于160 oC反应18 h成功合成了中空橄榄状的BiVO_4。用所得橄榄状BiVO_4为前驱体,通过热液刻蚀路线,获得了核壳结构的BiVO_4@Bi_2O_3微米球。利用X-射线衍射(XRD)、场发射扫描电子显微镜(FE-SEM)、透射电镜(TEM)、BET比表面积、紫外-可见漫反射谱等分析技术对样品进行了详尽表征。系统地研究了表面活性剂、溶剂比例对产物形貌的影响。用不同时段的中间产物的X-射线衍射分析结合扫描电子显微镜像观察研究了中空橄榄状BiVO_4微米球的形成过程。光催化实验的结果显示,核壳结构的BiVO_4@Bi_2O_3复合光催化剂比单一的橄榄状BiVO_4具有更高的光催化活性。基于理论计算,分析了BiVO_4@Bi_2O_3的光催化活性增强机理。
(2)以橄榄状BiVO_4为前驱体,硫代乙酰胺为硫源,在水热条件下,通过化学转化路线,合成了Bi_2S_3/BiVO_4复合光催化剂。利用X-射线衍射(XRD)、场发射扫描电子显微镜(FE-SEM)、紫外-可见漫反射谱、荧光谱、EDX谱等分析技术对样品进行了表征。光催化实验的结果显示,Bi_2S_3/BiVO_4复合光催化剂比单一BiVO_4具有更高的光催化活性。当参与反应的BiVO_4和硫代乙酰胺的摩尔比为1:0.4时,产物的光催化活性最强。结合理论计算,分析了Bi_2S_3/BiVO_4复合光催化剂的光催化活性增强机理。(3)利用羧基化的碳纳米管为载体,通过水热法制备了
Bi_2WO_6/CNTs复合光催化剂,利用X-射线衍射和场发射扫描电镜对产物进行表征。通过扫描电镜观察,发现反应物的浓度对最终产物的形貌有明显的影响。光催化实验的结果表明Bi_2WO_6/CNTs复合材料在可见光(λ> 400 nm)照射下对罗丹明B有良好的光催化降解作用。
This paper was committed to study preparation, characterization and photocatalytic properties of bismuth-based composite materials. The main research work is listed as the following parts:
(1) Hollow olive-shaped BiVO_4 microspheres was successfully synthesized in the presence of AOT under mixed solvothermal conditions at 160 oC for 18 h on a large scale. Furthermore, core-shell BiVO_4@Bi_2O_3 was obtained by thermal solution etching route, employing olive-shaped BiVO_4 as precursors. The as-obtained products were characterized by X-ray diffraction (XRD), Field-emission scanning electron microscope (FE-SEM), Transmission electron microscope (TEM), BET specific surface area, and UV-vis diffuse reflectance spectroscopy in detail. The influences of surfactant and the ratios of mixed solvents on the resultant products were systematically surveyed. The formation process of hollow olive-shaped BiVO_4 was investigated through the X-ray diffraction analyses and scanning electron microscope observations of the intermediate products at the different reaction stages. The photocatalytic properties of the as-obtained hollow olive-shaped BiVO_4 and core-shell BiVO_4@Bi_2O_3 were compared. The results indicated that core-shell BiVO_4@Bi_2O_3 exhibited much higher photocatalytic activities than pure olive-shaped BiVO_4. The mechanism of enhanced photocatalytic activity of core-shell BiVO_4@Bi_2O_3 was proposed on the basis of theoretical calculation.
(2) Bi_2S_3/BiVO_4 composite photocatalysts were successfully synthesized through a chemical conversion route under hydrothermal conditions, employing olive-shaped BiVO_4 as precursors and Thioacetamide (TTA) as sulfur resource. The as-obtained products were characterized by X-ray diffraction (XRD), Field-emission scanning electron microscope (SEM), UV-vis diffuse reflectance spectroscopy, Photoluminescence spectra and EDX spectra in detail. The photocatalytic properties of the as-obtained BiVO_4 and Bi_2S_3/BiVO_4 composite photocatalysts were compared. The results indicated that Bi_2S_3/BiVO_4 composite photocatalysts exhibited much higher photocatalytic activities than pure BiVO_4. It was found that Bi_2S_3/BiVO_4 composite semiconductor prepared with molar ratio of BiVO_4: TAA=1:0.4 shows the best photocatalytic acticity. Combined with theoretical calculation of band-edge positions of the two semiconductors, the mechanism of enhanced photocatalytic activity of Bi_2S_3/BiVO_4 was proposed.
(3) Bi_2WO_6/CNTs composite photocatalysts were synthesized under hydrothermal conditions, using carboxylated carbon nanotubes as supports. The as-obtained products were characterized by X-ray diffraction (XRD) and Field-emission scanning electron microscope (FE-SEM) in detail. The influence of the concentration of reactants on the morphology of resultant products was studied by field-emission scanning electron microscope. The photocatalytic results shows Bi_2WO_6/CNTs nanocomposite materials have good photocatalytic performance on the degradation of Rhodamine B under visible-light irradiation (λ>400nm).
(1)通过混合溶剂热路线,在AOT参与下,于160 oC反应18 h成功合成了中空橄榄状的BiVO_4。用所得橄榄状BiVO_4为前驱体,通过热液刻蚀路线,获得了核壳结构的BiVO_4@Bi_2O_3微米球。利用X-射线衍射(XRD)、场发射扫描电子显微镜(FE-SEM)、透射电镜(TEM)、BET比表面积、紫外-可见漫反射谱等分析技术对样品进行了详尽表征。系统地研究了表面活性剂、溶剂比例对产物形貌的影响。用不同时段的中间产物的X-射线衍射分析结合扫描电子显微镜像观察研究了中空橄榄状BiVO_4微米球的形成过程。光催化实验的结果显示,核壳结构的BiVO_4@Bi_2O_3复合光催化剂比单一的橄榄状BiVO_4具有更高的光催化活性。基于理论计算,分析了BiVO_4@Bi_2O_3的光催化活性增强机理。
(2)以橄榄状BiVO_4为前驱体,硫代乙酰胺为硫源,在水热条件下,通过化学转化路线,合成了Bi_2S_3/BiVO_4复合光催化剂。利用X-射线衍射(XRD)、场发射扫描电子显微镜(FE-SEM)、紫外-可见漫反射谱、荧光谱、EDX谱等分析技术对样品进行了表征。光催化实验的结果显示,Bi_2S_3/BiVO_4复合光催化剂比单一BiVO_4具有更高的光催化活性。当参与反应的BiVO_4和硫代乙酰胺的摩尔比为1:0.4时,产物的光催化活性最强。结合理论计算,分析了Bi_2S_3/BiVO_4复合光催化剂的光催化活性增强机理。(3)利用羧基化的碳纳米管为载体,通过水热法制备了
Bi_2WO_6/CNTs复合光催化剂,利用X-射线衍射和场发射扫描电镜对产物进行表征。通过扫描电镜观察,发现反应物的浓度对最终产物的形貌有明显的影响。光催化实验的结果表明Bi_2WO_6/CNTs复合材料在可见光(λ> 400 nm)照射下对罗丹明B有良好的光催化降解作用。
This paper was committed to study preparation, characterization and photocatalytic properties of bismuth-based composite materials. The main research work is listed as the following parts:
(1) Hollow olive-shaped BiVO_4 microspheres was successfully synthesized in the presence of AOT under mixed solvothermal conditions at 160 oC for 18 h on a large scale. Furthermore, core-shell BiVO_4@Bi_2O_3 was obtained by thermal solution etching route, employing olive-shaped BiVO_4 as precursors. The as-obtained products were characterized by X-ray diffraction (XRD), Field-emission scanning electron microscope (FE-SEM), Transmission electron microscope (TEM), BET specific surface area, and UV-vis diffuse reflectance spectroscopy in detail. The influences of surfactant and the ratios of mixed solvents on the resultant products were systematically surveyed. The formation process of hollow olive-shaped BiVO_4 was investigated through the X-ray diffraction analyses and scanning electron microscope observations of the intermediate products at the different reaction stages. The photocatalytic properties of the as-obtained hollow olive-shaped BiVO_4 and core-shell BiVO_4@Bi_2O_3 were compared. The results indicated that core-shell BiVO_4@Bi_2O_3 exhibited much higher photocatalytic activities than pure olive-shaped BiVO_4. The mechanism of enhanced photocatalytic activity of core-shell BiVO_4@Bi_2O_3 was proposed on the basis of theoretical calculation.
(2) Bi_2S_3/BiVO_4 composite photocatalysts were successfully synthesized through a chemical conversion route under hydrothermal conditions, employing olive-shaped BiVO_4 as precursors and Thioacetamide (TTA) as sulfur resource. The as-obtained products were characterized by X-ray diffraction (XRD), Field-emission scanning electron microscope (SEM), UV-vis diffuse reflectance spectroscopy, Photoluminescence spectra and EDX spectra in detail. The photocatalytic properties of the as-obtained BiVO_4 and Bi_2S_3/BiVO_4 composite photocatalysts were compared. The results indicated that Bi_2S_3/BiVO_4 composite photocatalysts exhibited much higher photocatalytic activities than pure BiVO_4. It was found that Bi_2S_3/BiVO_4 composite semiconductor prepared with molar ratio of BiVO_4: TAA=1:0.4 shows the best photocatalytic acticity. Combined with theoretical calculation of band-edge positions of the two semiconductors, the mechanism of enhanced photocatalytic activity of Bi_2S_3/BiVO_4 was proposed.
(3) Bi_2WO_6/CNTs composite photocatalysts were synthesized under hydrothermal conditions, using carboxylated carbon nanotubes as supports. The as-obtained products were characterized by X-ray diffraction (XRD) and Field-emission scanning electron microscope (FE-SEM) in detail. The influence of the concentration of reactants on the morphology of resultant products was studied by field-emission scanning electron microscope. The photocatalytic results shows Bi_2WO_6/CNTs nanocomposite materials have good photocatalytic performance on the degradation of Rhodamine B under visible-light irradiation (λ>400nm).
引文
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