基于石墨烯或类石墨氮化碳复合光催化剂的制备、表征及其光催化性能的研究
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摘要
环境污染与能源危机是当今人类所面临的两个重大问题。光催化技术作为一门新兴的催化技术，为人类解决环境污染与能源危机提供了可能。光催化剂在光降解有机污染物、光解水制氢等方面表现出了广阔的应用前景。然而，单一组份光催化剂的太阳能利用率低下，光生电子-空穴复合率高，量子效率低以及催化剂回收困难等问题限制了其应用。因此，通过对光催化剂进行改性，拓展其光吸收范围以实现对太阳能的充分利用，抑制光生载流子复合，提高其催化活性，已成为材料、化学与环境等学科的研究热点。层状结构材料如石墨烯以及类石墨氮化碳等具有优异的物理、化学性质而受到科研工作者的广泛关注。以石墨烯与类石墨氮化碳作为载体材料，构筑纳米复合光催化材料，不仅可保留各自的优异性能，而且还可能产生协同效应。金属氧化物与石墨烯构筑的复合光催化剂能够提高材料的导电性能与吸附性能，从而提高光催化活性。此外，类石墨氮化碳上负载氧化物之后，能够有效地抑制其光生电子-空穴复合。本论文主要是基于石墨烯或类石墨氮化碳复合光催化剂的制备、表征及光催化性能的研究，主要内容如下：
(1)采用水热法以及水-乙醇混合溶剂热法，分别了制备了石墨烯负载SnO2纳米棒以及负载SnO2纳米片复合材料。通过XRD、电镜、XPS以及TGA等多种表征手段对复合物体系的组成﹑形貌以及光催化性质进行了表征分析。相比于P25与单独SnO2，复合材料对RhB的降解具有更高的催化活性。通过分析电化学阻抗谱与紫外-可见光谱，探讨了材料催化性能增强的原因。石墨烯与SnO2之间的协同效应，使该复合物导电性能以及对染料RhB的吸附性能大大提高。
(2)采用热缩聚方法，以三聚氰胺与SnO2纳米颗粒为反应原料，成功地制备了SnO2/g-C3N4复合物。该复合物在可见光下对RhB具有良好的催化活性，其表观动力学常数为1.37h-1，是单独g-C3N4的4.54倍。光催化机理实验表明，该复合物对RhB的降解主要是通过空穴的氧化作用实现的，并且在体系中排除了光敏化现象。与此类似的，采用分两步制备了氮化碳负载SnO2纳米颗粒复合物，该复合物能够有效的保持了热处理后g-C3N4的大比表面积。同时，所合成的材料可以较容易的回收与重复使用。
(3)通过对热缩聚法制备的g-C3N4进行热处理，其比表面积大大增加。以热处理后的g-C3N4与硝酸铟为原料，机械混合后煅烧得到了氮化碳负载In2O3纳米颗粒复合物。分别利用XRD、DRS、SEM、TEM以及BET等手段对材料的组成、光学性质、形貌以及比表面积进行了表征与分析。该复合物在可见光下不仅对有色染料RhB，同时对于无色的4-硝基酚也具有很高的催化降解活性。光催化机理实验表明，该复合物对RhB的降解主要是通过空穴与超氧自由基的氧化作用实现的。
(4)基于氮化碳与半导体材料的物理化学特性和相对能带位置，设计并制备了BaTiO3/g-C3N4复合物。BaTiO3导带电位负于RhB的激发态电位，该复合物可以避免在降解RhB过程中出现光敏化现象。同时相比于SnO2，BaTiO3的导带位置足够负，能够与溶解氧发生反应生成其它氧化物种，进而更加有效地利用这部分电子，使其参与光催化反应。
总之，异质结光催化材料有效地解决了光催化剂的可见光吸收和光催化过程中的光生电子空穴分离的问题，开辟了一条探索新型高效可见光光催化材料的新途径。
Environment pollution and energy crisis are two of the most serious problems facinghumanity today. As a hot research issue, photocatalytic technology provides a possible routeto solve the environmental pollution and energy crisis. The fast development in thephotocatalytic technology field has suggested the great potential of photocatalysts for theremoval of organic pollutants and water splitting. However, the limited utilization of sunlightand high recombination rate of the photogenerated electron-hole pairs of the many reportedphotocatalysts have restricted the applications of photocatalysis. So far, various approacheshave been introduced to improve the photocatalytic activity for photocatalysts, such as doping,loading metals as a co-catalyst and coupling with other semiconductors.
Two-dimensional materials with layed structure, such as graphene and graphitic-likecarbon nitride have draw much attentions due to their excellent physical and chemicalproperties. Nanocomposite photocatalysts based on metal oxides and graphene or g-C3N4possess the properties of individual components or even with a synergistic effect. The highphotocatalytic activity of the catalysts could be a result of the adsorption of contaminantmolecules form the supporter. Nanocomposite photocatalysts also can accelerate theinterfacial electron-transfer process and suppresses the recombination of electrons and holes,thus improving the photocatalytic activity. In this dissertation, we focus on the synthesis,characterization and photocatalytic activity of graphene-or graphitic carbon nitride-basedphotocatalysts. The main points of this thesis are summaried as follows:
(1) SnO2nanorods-GR and SnO2nanosheets-GR composites were prepared viahydrothermal and solvothermal process respectively. The samples were characterized bypowder X-ray diffraction, scanning electron microscopy, transmission electron microscopy,UV-vis diffuse reflection spectroscopy, X-ray photoelectron spectroscopy andthermogravimetric analysis. By incorporation of graphene, SnO2-GR show enhancedphotocatalytic activity towards the decomposition of Rhodamine B. The mechanism of theirhigh photocatalytic activity is mainly ascribed to the synergy effect between SnO2andgraphene, resulting in the superior adsorption and the improved electric conductivity.
(2) Composite photocatalysts based on g-C3N4and SnO2nanoparticles were prepared byheating the mixture of SnO2nanoparticles and melamine in a muffle furnace. Theas-synthesized samples were characterized by X-ray diffraction, scanning electron microscopy,transmission electron microscopy, ultraviolet-visible light absorbance spectra, FT-IR and TG analysis. The significantly enhanced photocatalytic activity of the composite photocatalystswas attributed to the enhancement of electron-hole separation at the interface. It was foundthat holes (h+) was the main reactive species in the photocatalytic degradation of RhB.Furthermore, the dye-sensitised photocatalysis would not happen in this system, althoughRhB was active to visible light.
(3) A novel photocatalyst In2O3/g-C3N4(HT) was prepared through a simple method. Thecomposite catalysts displayed higher photocatalytic performance towards the decompositionof RhB and4-NP, which can be attributed to superior adsorption from g-C3N4and the synergyeffect between In2O3and g-C3N4. The highest photocatalytic activity of In2O3/g-C3N4(HT)composite was obtained with19.0wt%In2O3content. It was found that holes (h+) andsuperoxide (O2-) were the main reactive species in the photocatalytic degradation of RhB. Inaddition, The In2O3/g-C3N4(HT) composite catalysts are stable during the reaction and can beused repeatedly.
(4) BaTiO3/g-C3N4was prepared based on bandgap engineering between carbon nitrideand BaTiO3semiconductor. The dye-sensitised photocatalysis did not happen inBaTiO3/g-C3N4, due to the lowest unoccupied molecular orbital (LUMO) potential of RhBwas more positive than the CB of BaTiO3. Under visible light irradiation, g-C3N4was excitedto form the photo-generated electron-hole pairs. The most excited electrons in the CB ofg-C3N4were quickly transferred to the CB of BaTiO3.The excited electrons further react withthe absorbed O2to form O2-and H2O2. Thus, more electrons react with the absorbed O2, andthe higher photocatalytic activity was achieved.
In summary, construction of heterostructured semiconductor photocatalysts is a promisingway to enhance the separation rate of electons-holes and improve the photocatalyticperformance.
(1)采用水热法以及水-乙醇混合溶剂热法，分别了制备了石墨烯负载SnO2纳米棒以及负载SnO2纳米片复合材料。通过XRD、电镜、XPS以及TGA等多种表征手段对复合物体系的组成﹑形貌以及光催化性质进行了表征分析。相比于P25与单独SnO2，复合材料对RhB的降解具有更高的催化活性。通过分析电化学阻抗谱与紫外-可见光谱，探讨了材料催化性能增强的原因。石墨烯与SnO2之间的协同效应，使该复合物导电性能以及对染料RhB的吸附性能大大提高。
(2)采用热缩聚方法，以三聚氰胺与SnO2纳米颗粒为反应原料，成功地制备了SnO2/g-C3N4复合物。该复合物在可见光下对RhB具有良好的催化活性，其表观动力学常数为1.37h-1，是单独g-C3N4的4.54倍。光催化机理实验表明，该复合物对RhB的降解主要是通过空穴的氧化作用实现的，并且在体系中排除了光敏化现象。与此类似的，采用分两步制备了氮化碳负载SnO2纳米颗粒复合物，该复合物能够有效的保持了热处理后g-C3N4的大比表面积。同时，所合成的材料可以较容易的回收与重复使用。
(3)通过对热缩聚法制备的g-C3N4进行热处理，其比表面积大大增加。以热处理后的g-C3N4与硝酸铟为原料，机械混合后煅烧得到了氮化碳负载In2O3纳米颗粒复合物。分别利用XRD、DRS、SEM、TEM以及BET等手段对材料的组成、光学性质、形貌以及比表面积进行了表征与分析。该复合物在可见光下不仅对有色染料RhB，同时对于无色的4-硝基酚也具有很高的催化降解活性。光催化机理实验表明，该复合物对RhB的降解主要是通过空穴与超氧自由基的氧化作用实现的。
(4)基于氮化碳与半导体材料的物理化学特性和相对能带位置，设计并制备了BaTiO3/g-C3N4复合物。BaTiO3导带电位负于RhB的激发态电位，该复合物可以避免在降解RhB过程中出现光敏化现象。同时相比于SnO2，BaTiO3的导带位置足够负，能够与溶解氧发生反应生成其它氧化物种，进而更加有效地利用这部分电子，使其参与光催化反应。
总之，异质结光催化材料有效地解决了光催化剂的可见光吸收和光催化过程中的光生电子空穴分离的问题，开辟了一条探索新型高效可见光光催化材料的新途径。
Environment pollution and energy crisis are two of the most serious problems facinghumanity today. As a hot research issue, photocatalytic technology provides a possible routeto solve the environmental pollution and energy crisis. The fast development in thephotocatalytic technology field has suggested the great potential of photocatalysts for theremoval of organic pollutants and water splitting. However, the limited utilization of sunlightand high recombination rate of the photogenerated electron-hole pairs of the many reportedphotocatalysts have restricted the applications of photocatalysis. So far, various approacheshave been introduced to improve the photocatalytic activity for photocatalysts, such as doping,loading metals as a co-catalyst and coupling with other semiconductors.
Two-dimensional materials with layed structure, such as graphene and graphitic-likecarbon nitride have draw much attentions due to their excellent physical and chemicalproperties. Nanocomposite photocatalysts based on metal oxides and graphene or g-C3N4possess the properties of individual components or even with a synergistic effect. The highphotocatalytic activity of the catalysts could be a result of the adsorption of contaminantmolecules form the supporter. Nanocomposite photocatalysts also can accelerate theinterfacial electron-transfer process and suppresses the recombination of electrons and holes,thus improving the photocatalytic activity. In this dissertation, we focus on the synthesis,characterization and photocatalytic activity of graphene-or graphitic carbon nitride-basedphotocatalysts. The main points of this thesis are summaried as follows:
(1) SnO2nanorods-GR and SnO2nanosheets-GR composites were prepared viahydrothermal and solvothermal process respectively. The samples were characterized bypowder X-ray diffraction, scanning electron microscopy, transmission electron microscopy,UV-vis diffuse reflection spectroscopy, X-ray photoelectron spectroscopy andthermogravimetric analysis. By incorporation of graphene, SnO2-GR show enhancedphotocatalytic activity towards the decomposition of Rhodamine B. The mechanism of theirhigh photocatalytic activity is mainly ascribed to the synergy effect between SnO2andgraphene, resulting in the superior adsorption and the improved electric conductivity.
(2) Composite photocatalysts based on g-C3N4and SnO2nanoparticles were prepared byheating the mixture of SnO2nanoparticles and melamine in a muffle furnace. Theas-synthesized samples were characterized by X-ray diffraction, scanning electron microscopy,transmission electron microscopy, ultraviolet-visible light absorbance spectra, FT-IR and TG analysis. The significantly enhanced photocatalytic activity of the composite photocatalystswas attributed to the enhancement of electron-hole separation at the interface. It was foundthat holes (h+) was the main reactive species in the photocatalytic degradation of RhB.Furthermore, the dye-sensitised photocatalysis would not happen in this system, althoughRhB was active to visible light.
(3) A novel photocatalyst In2O3/g-C3N4(HT) was prepared through a simple method. Thecomposite catalysts displayed higher photocatalytic performance towards the decompositionof RhB and4-NP, which can be attributed to superior adsorption from g-C3N4and the synergyeffect between In2O3and g-C3N4. The highest photocatalytic activity of In2O3/g-C3N4(HT)composite was obtained with19.0wt%In2O3content. It was found that holes (h+) andsuperoxide (O2-) were the main reactive species in the photocatalytic degradation of RhB. Inaddition, The In2O3/g-C3N4(HT) composite catalysts are stable during the reaction and can beused repeatedly.
(4) BaTiO3/g-C3N4was prepared based on bandgap engineering between carbon nitrideand BaTiO3semiconductor. The dye-sensitised photocatalysis did not happen inBaTiO3/g-C3N4, due to the lowest unoccupied molecular orbital (LUMO) potential of RhBwas more positive than the CB of BaTiO3. Under visible light irradiation, g-C3N4was excitedto form the photo-generated electron-hole pairs. The most excited electrons in the CB ofg-C3N4were quickly transferred to the CB of BaTiO3.The excited electrons further react withthe absorbed O2to form O2-and H2O2. Thus, more electrons react with the absorbed O2, andthe higher photocatalytic activity was achieved.
In summary, construction of heterostructured semiconductor photocatalysts is a promisingway to enhance the separation rate of electons-holes and improve the photocatalyticperformance.
引文
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