分级结构半导体材料的绿色化学合成及其高效降解有机污染物性能
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摘要
本论文采用绿色化学合成技术,简捷地制备出了一系列具有独特分级结构的半导体微纳米材料,考察了微纳米结构的晶体生长形成机制,评价了分级结构半导体材料结构增强的降解模拟水污染物的性能。主要研究内容归纳如下：
1、采用超声化学技术,以醋酸铜和硫脲的水溶液为前驱体溶液,通过一步超声辐照反应,成功地制得了分级结构的半导体CuS中空微球。中空微球由厚度约为20nm CuS纳米片交叠自组装而成,纳米片在超声辅助生长过程中产生大量的堆叠位错。在过氧化氢作用下,这种分级中空结构的CuS微晶显示了氧化高浓度水污染物的降解性能,具有潜在的实际应用价值。
2、采用微波化学技术,以醋酸镉和硫脲的水溶液为前驱体溶液,通过调控乙二胺的量,成功地控制合成了三种不同物相和形貌相的CdS微纳米晶。随着矿化剂的体积增大,CdS微晶历经六方相单晶纳米球、六方相分级结构的“虫草”状纳米棒、再到立方相分级结构的“菜花”状微球的演变。可见光催化降解有机染料的实验表明,纯立方相“菜花”状CdS微晶显示最好的可见光催化性能,这归功于其最小的能级带宽、最弱的荧光和较大的比表面积等结构特性。
3、采用超声化学技术,将硝酸铋、硫脲和CTAB的前驱体反应液经一步超声辐照,得到一种超薄的圆片状BiOBr前驱体；前驱体经退火热处理成功地制得了具有分级和多孔结构的半导体BiOBr中空半球壳。半球壳类似于“蛋壳”状,壳壁为典型的类无机富勒烯层状结构,由大量的纳米粒子和孔隙组成。以有机染料RhB为分子探针,可见光光催化降解实验表明,这种独特的分级结构BiOBr中空“蛋壳”显示了高效的可见光催化降解有机污染物的性能。
4、采用微波化学技术,将硝酸铋、硫脲和CTAB的前驱体反应液经一步微波加热反应,成功地制得了三元高阶硫氯属化合物Bi19S27Br3自支撑超结构。超结构是由单晶的纳米纤维十字编织成微米“筛”,而纳米纤维是由更细的纳米丝融合而成。材料的固体紫外-可见-近红外吸收光谱表明在可见光和近红外光有较强的吸收。以模拟污染物RhB为分子探针,可见光催化实验表明其具有较好的可见光降解水污染物性能,为下一步开发近红外光响应的光催化剂提供有益参考。
In this dissertation, we have explored the controllable synthesis of hierarchically-structured semiconductor micro/nano materials via a facile and green chemical technique, in order to developing their promising application in aspects of environmental pollution treatment. The plausible crystal formation mechanisms of those novel hierarchical micro/nanostructures have been analyzed. Meanwhile, the corresponding structure-dependent degradation of organic pollutions on as-obtained hierarchically structured micro/nano materials has been also investigated. The details are summarized briefly as follows:
1. The hierarchically structured hollow microspheres composed of copper sulfide (CuS) nanoplatelets have been successfully fabricated via a one-pot and green sonochemical process for the first time, using copper acetate and thiourea aqueous solution as precursors without surfactant or template. Large-scaled hollow architectures with outer diameters in the range of1-1.2μm are assembled by pure hexagonal single crystalline CuS nanoplatelets, being of about20nm in thickness with stacking faults in the crystal lattice. Moreover, the possible growth mechanism for CuS hollow spheres is proposed on the basis of the temporal evolution controlled experiments. More importantly, this hierarchically structured CuS semiconductor material show highly efficient Fenton-like degradation activity of highly concentrated dye containing solution with the help of hydrogen peroxide, suggesting a promising application in wastewater purification.
2. Three kinds of CdS nanostructures, that is, hexagonal nanospheres, hierarchical caterpillarfungus-like hexagonal nanorods and hierarchical cubic microspheres, were controllably synthesized by a facile and one-pot microwave-assisted aqueous chemical method using ethanediamine as a phase and morphology controlling reagent. The characterization results show that hexagonal nanospheres is monodispersed with average diameters of about100nm; hexagonal caterpillarfungus-like nanorods has lengths in the range of600-800nm and diameters of40-60nm, assembled by nanoparticles about20nm in diameter; and hierarchical cubic microspheres is pure cubic microspheres with diameters in the range of0.8-1.3mm, aggregated by tiny nanograins with size of5.8nm. The visible light photodegradation of methylene blue and rhodamine B in the presence of CdS photocatalysts illustrate that all of them display high photocatalytic activities. Significantly, the hierarchical cubic microspheres exhibit the highest photocatalytic efficient in degradation of organic dyes, which is closely related to the phase and morphology structure of cubic CdS material.
3. Novel hollow BiOBr eggshells with inorganic fullerene-like structure have been successfully fabricated on a large scale via a facile ultrasound-assisted anion exchange reaction and subsequent heating treatment process. The products demonstrate that the hollow eggshells possess a pure tetragonal phase BiOBr, with the average thickness of about12nm, opening diameters of500-800nm and depths of400-600nm. The walls of eggshells, owning inorganic fullerene-like layered structure, are constructed by nanograins with size of about10nm. The average pore diameter of intercrystal mesopore is2.8nm. A possible formation mechanism for BiOBr hollow eggshells is proposed. According to the photodegradation of Rhodamine B under visible light irradiation, the hollow BiOBr eggshells exhibit excellent photocatalytic performance compared to P25catalyst.
4. Novel hierarchical self-supported Bi19S27Br3superstructures have been synthesized on a large scale by a facile and green microwave-assisted aqueous chemical process for the first time. The products have been characterized and the results reveal that the self-supported fabric-like Bi19S27Br3superstructures possess a hexagonal phase with diameters of4-5μm, constructed by cross-bedded nanofibers with average diameters of about80nm. Further, the nanofibers are aggregated by ultrafine nanosilks containing stacking faults. According to the photodegradation of RhodamineB under visible lighting, the self-supported Bi19S27Br3superstructures display high efficient catalytic performance. This work may reignite the intensive study of the higher-order sulfohalogenides for their application in solar and near-infrared light driven photodegradation of organic pollution.
1、采用超声化学技术,以醋酸铜和硫脲的水溶液为前驱体溶液,通过一步超声辐照反应,成功地制得了分级结构的半导体CuS中空微球。中空微球由厚度约为20nm CuS纳米片交叠自组装而成,纳米片在超声辅助生长过程中产生大量的堆叠位错。在过氧化氢作用下,这种分级中空结构的CuS微晶显示了氧化高浓度水污染物的降解性能,具有潜在的实际应用价值。
2、采用微波化学技术,以醋酸镉和硫脲的水溶液为前驱体溶液,通过调控乙二胺的量,成功地控制合成了三种不同物相和形貌相的CdS微纳米晶。随着矿化剂的体积增大,CdS微晶历经六方相单晶纳米球、六方相分级结构的“虫草”状纳米棒、再到立方相分级结构的“菜花”状微球的演变。可见光催化降解有机染料的实验表明,纯立方相“菜花”状CdS微晶显示最好的可见光催化性能,这归功于其最小的能级带宽、最弱的荧光和较大的比表面积等结构特性。
3、采用超声化学技术,将硝酸铋、硫脲和CTAB的前驱体反应液经一步超声辐照,得到一种超薄的圆片状BiOBr前驱体；前驱体经退火热处理成功地制得了具有分级和多孔结构的半导体BiOBr中空半球壳。半球壳类似于“蛋壳”状,壳壁为典型的类无机富勒烯层状结构,由大量的纳米粒子和孔隙组成。以有机染料RhB为分子探针,可见光光催化降解实验表明,这种独特的分级结构BiOBr中空“蛋壳”显示了高效的可见光催化降解有机污染物的性能。
4、采用微波化学技术,将硝酸铋、硫脲和CTAB的前驱体反应液经一步微波加热反应,成功地制得了三元高阶硫氯属化合物Bi19S27Br3自支撑超结构。超结构是由单晶的纳米纤维十字编织成微米“筛”,而纳米纤维是由更细的纳米丝融合而成。材料的固体紫外-可见-近红外吸收光谱表明在可见光和近红外光有较强的吸收。以模拟污染物RhB为分子探针,可见光催化实验表明其具有较好的可见光降解水污染物性能,为下一步开发近红外光响应的光催化剂提供有益参考。
In this dissertation, we have explored the controllable synthesis of hierarchically-structured semiconductor micro/nano materials via a facile and green chemical technique, in order to developing their promising application in aspects of environmental pollution treatment. The plausible crystal formation mechanisms of those novel hierarchical micro/nanostructures have been analyzed. Meanwhile, the corresponding structure-dependent degradation of organic pollutions on as-obtained hierarchically structured micro/nano materials has been also investigated. The details are summarized briefly as follows:
1. The hierarchically structured hollow microspheres composed of copper sulfide (CuS) nanoplatelets have been successfully fabricated via a one-pot and green sonochemical process for the first time, using copper acetate and thiourea aqueous solution as precursors without surfactant or template. Large-scaled hollow architectures with outer diameters in the range of1-1.2μm are assembled by pure hexagonal single crystalline CuS nanoplatelets, being of about20nm in thickness with stacking faults in the crystal lattice. Moreover, the possible growth mechanism for CuS hollow spheres is proposed on the basis of the temporal evolution controlled experiments. More importantly, this hierarchically structured CuS semiconductor material show highly efficient Fenton-like degradation activity of highly concentrated dye containing solution with the help of hydrogen peroxide, suggesting a promising application in wastewater purification.
2. Three kinds of CdS nanostructures, that is, hexagonal nanospheres, hierarchical caterpillarfungus-like hexagonal nanorods and hierarchical cubic microspheres, were controllably synthesized by a facile and one-pot microwave-assisted aqueous chemical method using ethanediamine as a phase and morphology controlling reagent. The characterization results show that hexagonal nanospheres is monodispersed with average diameters of about100nm; hexagonal caterpillarfungus-like nanorods has lengths in the range of600-800nm and diameters of40-60nm, assembled by nanoparticles about20nm in diameter; and hierarchical cubic microspheres is pure cubic microspheres with diameters in the range of0.8-1.3mm, aggregated by tiny nanograins with size of5.8nm. The visible light photodegradation of methylene blue and rhodamine B in the presence of CdS photocatalysts illustrate that all of them display high photocatalytic activities. Significantly, the hierarchical cubic microspheres exhibit the highest photocatalytic efficient in degradation of organic dyes, which is closely related to the phase and morphology structure of cubic CdS material.
3. Novel hollow BiOBr eggshells with inorganic fullerene-like structure have been successfully fabricated on a large scale via a facile ultrasound-assisted anion exchange reaction and subsequent heating treatment process. The products demonstrate that the hollow eggshells possess a pure tetragonal phase BiOBr, with the average thickness of about12nm, opening diameters of500-800nm and depths of400-600nm. The walls of eggshells, owning inorganic fullerene-like layered structure, are constructed by nanograins with size of about10nm. The average pore diameter of intercrystal mesopore is2.8nm. A possible formation mechanism for BiOBr hollow eggshells is proposed. According to the photodegradation of Rhodamine B under visible light irradiation, the hollow BiOBr eggshells exhibit excellent photocatalytic performance compared to P25catalyst.
4. Novel hierarchical self-supported Bi19S27Br3superstructures have been synthesized on a large scale by a facile and green microwave-assisted aqueous chemical process for the first time. The products have been characterized and the results reveal that the self-supported fabric-like Bi19S27Br3superstructures possess a hexagonal phase with diameters of4-5μm, constructed by cross-bedded nanofibers with average diameters of about80nm. Further, the nanofibers are aggregated by ultrafine nanosilks containing stacking faults. According to the photodegradation of RhodamineB under visible lighting, the self-supported Bi19S27Br3superstructures display high efficient catalytic performance. This work may reignite the intensive study of the higher-order sulfohalogenides for their application in solar and near-infrared light driven photodegradation of organic pollution.
引文
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