铋系异质结光催化剂的原位制备及其环境净化性能研究
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摘要
拓宽半导体光催化材料的光响应范围和提高光催化反应效率是目前光催化研究的重点。铋系复合氧化物因其独特的电子结构和优良的可见光吸收性能,近年来受到人们的广泛关注。结合我国铋矿资源优势,设计制备廉价、高效、可用于环境净化领域的铋系光催化剂具有很好的发展前景。本文使用软化学原位合成技术,设计制备一系列分布均匀、能级匹配的铋系异质结型复合半导体光催化剂。并分别将其用于有机污染物的分解、病原微生物的灭杀、重金属离子的减毒以及室内挥发性有机物的去除等环境净化领域。通过不同的实验参数控制材料的复合比例、表面微结构、光吸收性能等,研究了复合光催化剂结构对光催化环境净化性能的影响。本文的主要研究工作如下：
采用简单易行的低温溶液法,将Ti的聚合阳离子引入到Bi3Nb07颗粒的表面,原位合成了BiOCl/Bi5Nb3O15/TiO2复合光催化剂。分别通过XRD、XPS、 HR-TEM、紫外-可见漫反射、N2-吸附脱附等多种测试手段对复合光催化剂样品进行了分析。BiOCl/Bi5Nb3O15/TiO2复合样品具有高比表面积和双介孔结构。光催化实验结果表明,该复合光催化剂对罗丹明B和气态丙酮都具有很好的光催化降解活性。原位形成的多相异质结界面有效结合匹配,从而促进光生电荷的分离,增强光催化活性。该光催化剂对罗丹明B的降解先以脱乙基作用为主导,后对发色基团进行攻击破坏,活性自由基O2·-在光催化降解罗丹明B中起主要作用。
采用水热法,探讨了不同铋源化合物和反应体系pH值对合成Bi2O2CO3的形貌结构、表面官能团、光吸收性及光催化活性的影响。以BiCl3为铋源所合成的样品具有更小的粒径尺寸,吸收边带出现了明显的蓝移现象。在紫外光照射下,以BiCl3为铋源所合成的样品对甲基橙具有最高的光催化活性。在pH约为8时所制备的Bi2O2CO3样品由微米/纳米片自组装形成具有分级结构的球状,有利于对光量子的捕集,表现出很好的光催化活性。
采用水热法原位合成了Bi2O2CO3/Bi3NbO7复合光催化剂,并研究了所制备样品在可见光下对大肠杆菌的光催化灭菌活性。通过多种测试表征手段对合成样品的物相、表面微结构、光吸收性能等进行分析,并对其光催化灭菌机理进行了初探。不同比例的Bi2O2CO3/Bi3NbO7复合物的光吸收波长阙值λg范围从428nm到445nm之间。光催化灭菌结果表明,BiCO/BiNbO-2样品在可见光下对大肠杆菌具有较好的灭活能力。原位制备所形成的Bi2O2CO3/Bi3NbO7异质结结构可以有效延长光生电子空穴的寿命。复合光催化剂具有大的比表面积和多孔径结构,这有利于增加反应活性位点,从而进一步提高光催化反应效率。
采用水热原位制备技术合成了Bi2S3/Bi202C03复合光催化剂,并考察了所制备的复合光催化剂在模拟太阳光下对溶液中Cr(Ⅵ)的去除效率。通过XRD、 SEM、TEM、UV-vis Diffuse Reflectance等多种测试表征手段对合成样品的物相组成、形貌结构、表面官能团、光吸收性能等进行了分析。复合物中Bi2S3和Bi2O2CO3分别以棒状纤维和片层结构存在,且两种半导体界面紧密结合。Bi2O2CO3复合样品在紫外光区域和可见光区域都具有明显的光吸收性能。光催化实验结果表明,在模拟太阳光照射下,Bi2O2CO3复合光催化剂比N掺杂Bi2O2CO3具有更好的Cr(Ⅵ)吸附性能和光催化还原效果。复合物中Bi2S3和Bi2O2CO3间较高的界面结合度、匹配的能级位置有利于光生电子的转移率,提高光生载流子的寿命,从而增加光催化反应效率。
To broaden the light response range of semiconductor photocatalysts and improve the efficiency of photocatalytic reaction is the focus of the photocatalytic study. Due to its unique layered structure and excellent light absorption properties, the bismuth-based composite oxides have attracted more and more attention in recent years. Based on the rich domestic bismuth mineral resource, to develop low-cost, efficient and applying in environmental purification bismuth-based photocatalysts has good prospects. In this work, a series of bismuth-based composite photocatalysts with tightly interface, evenly distributed and matching energy level, was designed and prepared by soft chemical in-situ synthesis technology. And the prepared bismuth-based composite photocatalysts was used in the field of environmental purification, such as decomposition of organic pollutants, the sterilization of pathogenic contaminants, reduction of heavy metal ions and removal of indoor VOCs, respectively. Different experimental parameters were studied for controlling the proportion of composite materials, surface microstructure, and optical absorption performance. The influence of composite photocatalysts structure on the photocatalytic performance was also studied. The main research work is as follows:
By a facile solution method at low temperature, introducing the Ti polymeric cationic to the surface of BisNbO7particles, the BiOCl/Bi5Nb3O15/TiO2composite photocatalyst was in-situ synthesized. The as-prepared composites were characterized by XRD, XPS, HR-TEM, UV-vis DRS and N2adsorption-desorption. The BiOCl/Bi5Nb3O15/TiO2composite samples have high specific surface area and dual-mesoporous structure. The multiphase interfaces formed in-situ are matching effective, which could favor for the separation of the light generated electron-hole, and thus increase the photocatalytic efficiency. The photocatalytic degradation results show that the composite photocatalysts have good photocatalytic activity for the degradation of rhodamine B and gaseous acetone. The photocatalyst degradation of rhodamine B was initial deethylation and then attacking and destruction the chromophore. The active radical O2-play an important role in the photocatalytic degradation of Rhodamine B.
By hydrothermal method, the different synthesis conditions, bismuth source compounds and the effect of pH values, on the characteristic of the as-prepared Bi2O2CO3samples, such as morphology, surface functional groups, light absorption and photocatalytic activity was studied. The as-prepared samples using BiCl3as bismuth source having a smaller particle size. The absorption edge has a clear blue shift. The as-prepared samples using BiCl3as bismuth source have the highest photocatalytic activity for the degradation of methyl orange under UV irradiation. Under different pH conditions, the Bi2O2CO3sample synthesized at pH8have a hierarchical structure with self-assembled sphere-like morphology, which is favor for trapping light quantum. The sample Bi2O2CO3sample synthesized at pH8shows the best photocatalytic efficiency.
The Bi2O2CO3/Bi3NbO7composite photocatalyst was synthesized by in-situ hydrothermal method and the photocatalytic bactericidal activity against E. coli was also discussed. The phase structure, surface microstructure and optical absorption performance was analyzed by a variety of characterizations. Light absorption edges of different proportion Bi2O2CO3/Bi3NbO7composites were from428-455nm. The result shows that the BiCO/BiNbO-2composite has good photocatalytic bactericidal activity. The in-situ formed Bi2O2CC3/Bi3NbO7heterojunction structure can effectively extend the life of the light generated electron-hole. And the composite photocatalyst have a large specific surface area and multi-porous structure, which is conducive to increase the reactive sites, thus enhancing the efficiency of the photocatalytic reaction.
The Bi2S3/Bi2O2CO3composite photocatalyst was synthesized by in-situ hydrothermal technology and photocatalytic reduction of Cr (VI) in aqueous solutions under simulated sunlight irradiation was also studied. The phase composition, morphology, surface functional groups and light absorption property was analyzed by XRD, SEM, TEM, FT-IR and UV-vis Diffuse Reflectance. Bi2S3and Bi2O2CO3existed in the composites as rod-like fibers and plate-like structure, respectively, and the interface of two components closely integrated. The Bi2S3/Bi2O2CO3composite photocatalyst shows better adsorption performance and photocatalytic reduction activity for the Cr (VI) than the N-doped Bi2O2CO3. The tightly interfaces and matching energy level are benefit for the transferring of photo-induced electrons and improving the life of the light generated carriers, thus increasing the efficiency of the photocatalytic reaction.
采用简单易行的低温溶液法,将Ti的聚合阳离子引入到Bi3Nb07颗粒的表面,原位合成了BiOCl/Bi5Nb3O15/TiO2复合光催化剂。分别通过XRD、XPS、 HR-TEM、紫外-可见漫反射、N2-吸附脱附等多种测试手段对复合光催化剂样品进行了分析。BiOCl/Bi5Nb3O15/TiO2复合样品具有高比表面积和双介孔结构。光催化实验结果表明,该复合光催化剂对罗丹明B和气态丙酮都具有很好的光催化降解活性。原位形成的多相异质结界面有效结合匹配,从而促进光生电荷的分离,增强光催化活性。该光催化剂对罗丹明B的降解先以脱乙基作用为主导,后对发色基团进行攻击破坏,活性自由基O2·-在光催化降解罗丹明B中起主要作用。
采用水热法,探讨了不同铋源化合物和反应体系pH值对合成Bi2O2CO3的形貌结构、表面官能团、光吸收性及光催化活性的影响。以BiCl3为铋源所合成的样品具有更小的粒径尺寸,吸收边带出现了明显的蓝移现象。在紫外光照射下,以BiCl3为铋源所合成的样品对甲基橙具有最高的光催化活性。在pH约为8时所制备的Bi2O2CO3样品由微米/纳米片自组装形成具有分级结构的球状,有利于对光量子的捕集,表现出很好的光催化活性。
采用水热法原位合成了Bi2O2CO3/Bi3NbO7复合光催化剂,并研究了所制备样品在可见光下对大肠杆菌的光催化灭菌活性。通过多种测试表征手段对合成样品的物相、表面微结构、光吸收性能等进行分析,并对其光催化灭菌机理进行了初探。不同比例的Bi2O2CO3/Bi3NbO7复合物的光吸收波长阙值λg范围从428nm到445nm之间。光催化灭菌结果表明,BiCO/BiNbO-2样品在可见光下对大肠杆菌具有较好的灭活能力。原位制备所形成的Bi2O2CO3/Bi3NbO7异质结结构可以有效延长光生电子空穴的寿命。复合光催化剂具有大的比表面积和多孔径结构,这有利于增加反应活性位点,从而进一步提高光催化反应效率。
采用水热原位制备技术合成了Bi2S3/Bi202C03复合光催化剂,并考察了所制备的复合光催化剂在模拟太阳光下对溶液中Cr(Ⅵ)的去除效率。通过XRD、 SEM、TEM、UV-vis Diffuse Reflectance等多种测试表征手段对合成样品的物相组成、形貌结构、表面官能团、光吸收性能等进行了分析。复合物中Bi2S3和Bi2O2CO3分别以棒状纤维和片层结构存在,且两种半导体界面紧密结合。Bi2O2CO3复合样品在紫外光区域和可见光区域都具有明显的光吸收性能。光催化实验结果表明,在模拟太阳光照射下,Bi2O2CO3复合光催化剂比N掺杂Bi2O2CO3具有更好的Cr(Ⅵ)吸附性能和光催化还原效果。复合物中Bi2S3和Bi2O2CO3间较高的界面结合度、匹配的能级位置有利于光生电子的转移率,提高光生载流子的寿命,从而增加光催化反应效率。
To broaden the light response range of semiconductor photocatalysts and improve the efficiency of photocatalytic reaction is the focus of the photocatalytic study. Due to its unique layered structure and excellent light absorption properties, the bismuth-based composite oxides have attracted more and more attention in recent years. Based on the rich domestic bismuth mineral resource, to develop low-cost, efficient and applying in environmental purification bismuth-based photocatalysts has good prospects. In this work, a series of bismuth-based composite photocatalysts with tightly interface, evenly distributed and matching energy level, was designed and prepared by soft chemical in-situ synthesis technology. And the prepared bismuth-based composite photocatalysts was used in the field of environmental purification, such as decomposition of organic pollutants, the sterilization of pathogenic contaminants, reduction of heavy metal ions and removal of indoor VOCs, respectively. Different experimental parameters were studied for controlling the proportion of composite materials, surface microstructure, and optical absorption performance. The influence of composite photocatalysts structure on the photocatalytic performance was also studied. The main research work is as follows:
By a facile solution method at low temperature, introducing the Ti polymeric cationic to the surface of BisNbO7particles, the BiOCl/Bi5Nb3O15/TiO2composite photocatalyst was in-situ synthesized. The as-prepared composites were characterized by XRD, XPS, HR-TEM, UV-vis DRS and N2adsorption-desorption. The BiOCl/Bi5Nb3O15/TiO2composite samples have high specific surface area and dual-mesoporous structure. The multiphase interfaces formed in-situ are matching effective, which could favor for the separation of the light generated electron-hole, and thus increase the photocatalytic efficiency. The photocatalytic degradation results show that the composite photocatalysts have good photocatalytic activity for the degradation of rhodamine B and gaseous acetone. The photocatalyst degradation of rhodamine B was initial deethylation and then attacking and destruction the chromophore. The active radical O2-play an important role in the photocatalytic degradation of Rhodamine B.
By hydrothermal method, the different synthesis conditions, bismuth source compounds and the effect of pH values, on the characteristic of the as-prepared Bi2O2CO3samples, such as morphology, surface functional groups, light absorption and photocatalytic activity was studied. The as-prepared samples using BiCl3as bismuth source having a smaller particle size. The absorption edge has a clear blue shift. The as-prepared samples using BiCl3as bismuth source have the highest photocatalytic activity for the degradation of methyl orange under UV irradiation. Under different pH conditions, the Bi2O2CO3sample synthesized at pH8have a hierarchical structure with self-assembled sphere-like morphology, which is favor for trapping light quantum. The sample Bi2O2CO3sample synthesized at pH8shows the best photocatalytic efficiency.
The Bi2O2CO3/Bi3NbO7composite photocatalyst was synthesized by in-situ hydrothermal method and the photocatalytic bactericidal activity against E. coli was also discussed. The phase structure, surface microstructure and optical absorption performance was analyzed by a variety of characterizations. Light absorption edges of different proportion Bi2O2CO3/Bi3NbO7composites were from428-455nm. The result shows that the BiCO/BiNbO-2composite has good photocatalytic bactericidal activity. The in-situ formed Bi2O2CC3/Bi3NbO7heterojunction structure can effectively extend the life of the light generated electron-hole. And the composite photocatalyst have a large specific surface area and multi-porous structure, which is conducive to increase the reactive sites, thus enhancing the efficiency of the photocatalytic reaction.
The Bi2S3/Bi2O2CO3composite photocatalyst was synthesized by in-situ hydrothermal technology and photocatalytic reduction of Cr (VI) in aqueous solutions under simulated sunlight irradiation was also studied. The phase composition, morphology, surface functional groups and light absorption property was analyzed by XRD, SEM, TEM, FT-IR and UV-vis Diffuse Reflectance. Bi2S3and Bi2O2CO3existed in the composites as rod-like fibers and plate-like structure, respectively, and the interface of two components closely integrated. The Bi2S3/Bi2O2CO3composite photocatalyst shows better adsorption performance and photocatalytic reduction activity for the Cr (VI) than the N-doped Bi2O2CO3. The tightly interfaces and matching energy level are benefit for the transferring of photo-induced electrons and improving the life of the light generated carriers, thus increasing the efficiency of the photocatalytic reaction.
引文
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