含Cu化合物异质结构的制备及光催化产氢活性研究
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摘要
光催化分解水制氢将取之不尽的低密度太阳能通过光化学反应转换为化学能,是一种清洁的、可持续发展的获得氢能的方式。而开发高效、稳定的光催化材料用于光催化分解水的催化剂是发展太阳光催化制氢技术的核心。迄今为止,该领域的科研工作者开发了多种可用于光催化制氢的材料,但是由于光生电子和空穴的复合导致的较低的产氢效率严重的限制了此类材料的实际应用。因此,寻找合适的途径强化光生电子与空穴的分离、增加光生载流子的利用效率,就成为提高光催化剂产氢活性的关键所在。而异质结复合材料在载流子输运方面的独特优势,另外具有特殊形貌的异质结复合光催化剂对光生电荷的分离效果更佳。本论文以光催化领域最具代表性的光催化材料Ti02和ZnS为主要研究对象,以构建高效的Cu化合物异质结构复合光催化剂为研究目标,致力于开发高效异质结的构建方法,从提高异质结复合光催化材料界面电荷迁移的驱动力入手,构建高效的、具有特殊形貌的Cu化合物异质结构复合光催化材料用于光催化制氢。主要研究内容如下：
1、基于能带结构对异质结电荷分离的影响,采用低温乙醇诱导结合退火处理的方法,制备了具有优异电荷分离效果的q-Cu2O/TiO2异质结构复合光催化材料,我们通过改变Cu20前驱物的用量来实现了Cu20纳米的尺寸调控,从而使得Cu20的导带位置上移,增加了Cu20与P25导带间的电位梯度,增大了异质结界面电荷迁移的驱动。另一方面,量子尺寸效应对Cu20能带结构的调控,使其控制下的电子迁移与p-n结内建内场控制下的电子迁移相一致,从而实现了该异质结复合光催化材料光生载流子的有效分离,提高了其产氢活性。该部分研究结果提供了一种简单、绿色的制备方法沉积Cu20量子点在Ti02表面,而且也提供了一种有效构建p-n异质结的研究思路。
2、基于非半导体的难溶化合物的电极电势的位置与异质结电荷分离的关系,发现了一种简易构建高效异质结复合光催化材料的方法。通过调节非半导体难溶化合物的溶解性(Ksp)即简单改变CuX (X:(OH)2CO32-、S2-、OH-、 C2O42-)中阴离子的种类,可实现对CuX/Cu电极电势的调控,从而影响了异质结CuX/P25中光生电子与空穴的分离。采用这一方法,我们发现Cu2(OH)2CO3/Cu还原电势介于P25的导带底与H+/H2还原电位之间,且与P25的导带底具有相对较大的电位梯度。因此,Cu2(OH)2CO3可作为一种优异的助催化剂与P25构建异质结复合光催化材料,并表现出较好的电荷分离效果与光催化制氢性能。该异质结复合材料在模拟太阳光下产氢活性可达0.51mmolh-1,量子效率为31.2%,是纯P25的485倍。该工作不仅开发了一种优异的可用于光催化制氢的助催化剂-Cu2(OH)2CO3,而且提供了一种简易的高效异质结复合光催化剂的构建方法。
3、考虑到形貌调控在光催化制氢中的优势,我们以ZnS为代表,基于界面电荷迁移理论,采用微波水热结合阳离子交换方法构建了CuS/ZnS花状异质结复合光催化剂。该异质结的构建拓宽了ZnS的光响应范围,在可见光下,光激发ZnS产生的电子向CuS/Cu2S电位的迁移,实现了光生电子与空穴的空间有效分离,使ZnS/CuS花状异质结复合光催化剂在无助催化剂负载时可见光产氢活性达到0.33mmol h-1,420nm波长光照的量子效率达到22.8%,与CuS/ZnS片状异质结复合光催化剂相比产氢活性和量子效率均有所提高,证明了当都具备光诱导界面电荷传输效应(IFCT)时,特殊形貌异质结构因具有高比表面积和光吸收率,在光生电荷分离上有突出的优势。另外我们通过时间序,详细地研究了ZnS/CuS花状异质结的形成机理,并揭示了其微观结构与性能的关系。
Photocatalytic hydrogen production from water splitting is a clean and renewable hydrogen production method, because it can convert the inexhaustible and low density solar energy to the chemical energy. Preparing highly efficient photocatalytsts is the key for developing the photocatalytic hydrogen production technology. So far, the applications of many photocatalytic materials in the photocatalytic hydrogen production field have been greatly limited due to the low efficiencies resulted from the easy recombination of photogenerated charge carriers. Therefore, seeking a suitable approach to effectively separate the photogenerated electrons and holes and increase the utilization of photogenerated charge carriers is significant for enhancing the photocatalytic activity for hydrogen production. Heterostructured materials have unique advantages for the transportation of carriers and exhibit potential values in the photocatalytic hydrogen production field. In this dissertation, the representative TiO2and ZnS were chose as the research objects and the fabrication of highly efficient Cu-cotaining composites heterostructured was as the research aim. We addict to develop highly efficient Cu-cotaining composites heterostructured photocatalysts with special morphology via increasing the driven force of the photogenerated charge carriers transfer. Main research topics are as follows:
1. Based on the effect of the bandgap structure on the separation of photogenerated charges, we prepared q-Cu2O/TiO2heterojunction composites with excellent charges separation efficiency via ethanol induced method at low temperature followed by calcination. The Cu2O nanosize was controlled by adjusting the amount of Cu2O precursor. The qautum size effect maked the conduction band bottom of Cu2O shift up. This can efficiently increase the potential gradient between the conduction band bottom of Cu2O and that of TiO2, and thus enhance the driven force of the interfacial charges transfer. On the other hand, the energy band structure of Cu2O was tuned by the quantum size effect, which makes the electrons transfer from Cu2O to TiO2. The transfer was consistent with that in p-n junctions controlled by the built-in electrical field resulting in the enhanced photocatalytic activity for hydrogen production. This study not only provides a facial and green method to prepared Cu2O quantum dots on TiO2surfaces, but also supports an efficient approach to fabricate p-n heterojunctions with an increased interfacial charge transfer.
2. Based on the relation between the charge separation of heterojuntions and the potentials of the insoluble non-semiconductor compounds, we find an facile method to develop efficient heterostructured composites. The separation of the photogenerated electrons and holes in the CuX/P25heteroj unctions was easily controlled by tuning the CuX/Cu electrode potentials, which was closely related to the solubility (Ksp) of insoluble non-semiconductor compounds. This can be achieved by simply changing the anion species in CuX (X:(OH)2CO32-、S2-、OH-、 C2O42-). According to this method, we have found that the Cu2(OH)2CO3/Cu reduction potential is between the conduction band bottom of P25and the redox potential of H+/H2with a relatively large potential gradient. Thus, Cu2(OH)2CO3can be used as an excellent co-catalyst to build heteroj unction composites with P25, which exhibited an excellent charge separation efficiency and photocatalytic hydrogen production activity. The photocatalytic activity for hydrogen production of the heteroj unction composites was up to0.51mmol h-1under the simulant solar light irradiation, and the quantum efficiency was up to31.2%which was485times higher than that of pure P25. This work develops an excellent cocatalyst-Cu2(OH)2CO3for photocatalytic hydrogen production as well as provides an facile and efficient method for fabricating heteroj unction composite photocatalysts.
3. Considering the advantages of morphology control in photocatalytic hydrogen production, the flower-like ZnS/CuS heterostructured composites were prepared by the combination of microwave hydrothermal and cation exchange methods according to the interfacial charge transfer theory. The fabrication of the heterojunctions broadened the range of light response of ZnS. The photoexcited electrons of ZnS migrated to the redox potential of CuS/Cu2S under visible light irradiation, which can facilitate the effective separation of photogenerated electrons and holes in space. The visible photocatalytic activity towards hydrogen production for ZnS/CuS flower-like heterostructed composites without co-catalyst achieved0.33mmol h-1, and the quantum efficiency was up to22.8%under the wavelength with420nm visible light irradiation. Compared with the sheet-like photocatalyst composite, hydrogen production activity and quantum efficiency were improved. It proved that when both have photoinduced interfacial charge transfer (IFCT) effect, heterostructures photocatalyst composites with special morphology which possess high surface area and light absorption rate, have outstanding advantages in photoinduced charge separation. In addition, the formation mechanisms of the flakes and flower-like ZnS/CuS heterojunctions were also studied in detail by tuning the reaction time and temperature. Finally the relationship of the microstructure and the performance was revealed.
1、基于能带结构对异质结电荷分离的影响,采用低温乙醇诱导结合退火处理的方法,制备了具有优异电荷分离效果的q-Cu2O/TiO2异质结构复合光催化材料,我们通过改变Cu20前驱物的用量来实现了Cu20纳米的尺寸调控,从而使得Cu20的导带位置上移,增加了Cu20与P25导带间的电位梯度,增大了异质结界面电荷迁移的驱动。另一方面,量子尺寸效应对Cu20能带结构的调控,使其控制下的电子迁移与p-n结内建内场控制下的电子迁移相一致,从而实现了该异质结复合光催化材料光生载流子的有效分离,提高了其产氢活性。该部分研究结果提供了一种简单、绿色的制备方法沉积Cu20量子点在Ti02表面,而且也提供了一种有效构建p-n异质结的研究思路。
2、基于非半导体的难溶化合物的电极电势的位置与异质结电荷分离的关系,发现了一种简易构建高效异质结复合光催化材料的方法。通过调节非半导体难溶化合物的溶解性(Ksp)即简单改变CuX (X:(OH)2CO32-、S2-、OH-、 C2O42-)中阴离子的种类,可实现对CuX/Cu电极电势的调控,从而影响了异质结CuX/P25中光生电子与空穴的分离。采用这一方法,我们发现Cu2(OH)2CO3/Cu还原电势介于P25的导带底与H+/H2还原电位之间,且与P25的导带底具有相对较大的电位梯度。因此,Cu2(OH)2CO3可作为一种优异的助催化剂与P25构建异质结复合光催化材料,并表现出较好的电荷分离效果与光催化制氢性能。该异质结复合材料在模拟太阳光下产氢活性可达0.51mmolh-1,量子效率为31.2%,是纯P25的485倍。该工作不仅开发了一种优异的可用于光催化制氢的助催化剂-Cu2(OH)2CO3,而且提供了一种简易的高效异质结复合光催化剂的构建方法。
3、考虑到形貌调控在光催化制氢中的优势,我们以ZnS为代表,基于界面电荷迁移理论,采用微波水热结合阳离子交换方法构建了CuS/ZnS花状异质结复合光催化剂。该异质结的构建拓宽了ZnS的光响应范围,在可见光下,光激发ZnS产生的电子向CuS/Cu2S电位的迁移,实现了光生电子与空穴的空间有效分离,使ZnS/CuS花状异质结复合光催化剂在无助催化剂负载时可见光产氢活性达到0.33mmol h-1,420nm波长光照的量子效率达到22.8%,与CuS/ZnS片状异质结复合光催化剂相比产氢活性和量子效率均有所提高,证明了当都具备光诱导界面电荷传输效应(IFCT)时,特殊形貌异质结构因具有高比表面积和光吸收率,在光生电荷分离上有突出的优势。另外我们通过时间序,详细地研究了ZnS/CuS花状异质结的形成机理,并揭示了其微观结构与性能的关系。
Photocatalytic hydrogen production from water splitting is a clean and renewable hydrogen production method, because it can convert the inexhaustible and low density solar energy to the chemical energy. Preparing highly efficient photocatalytsts is the key for developing the photocatalytic hydrogen production technology. So far, the applications of many photocatalytic materials in the photocatalytic hydrogen production field have been greatly limited due to the low efficiencies resulted from the easy recombination of photogenerated charge carriers. Therefore, seeking a suitable approach to effectively separate the photogenerated electrons and holes and increase the utilization of photogenerated charge carriers is significant for enhancing the photocatalytic activity for hydrogen production. Heterostructured materials have unique advantages for the transportation of carriers and exhibit potential values in the photocatalytic hydrogen production field. In this dissertation, the representative TiO2and ZnS were chose as the research objects and the fabrication of highly efficient Cu-cotaining composites heterostructured was as the research aim. We addict to develop highly efficient Cu-cotaining composites heterostructured photocatalysts with special morphology via increasing the driven force of the photogenerated charge carriers transfer. Main research topics are as follows:
1. Based on the effect of the bandgap structure on the separation of photogenerated charges, we prepared q-Cu2O/TiO2heterojunction composites with excellent charges separation efficiency via ethanol induced method at low temperature followed by calcination. The Cu2O nanosize was controlled by adjusting the amount of Cu2O precursor. The qautum size effect maked the conduction band bottom of Cu2O shift up. This can efficiently increase the potential gradient between the conduction band bottom of Cu2O and that of TiO2, and thus enhance the driven force of the interfacial charges transfer. On the other hand, the energy band structure of Cu2O was tuned by the quantum size effect, which makes the electrons transfer from Cu2O to TiO2. The transfer was consistent with that in p-n junctions controlled by the built-in electrical field resulting in the enhanced photocatalytic activity for hydrogen production. This study not only provides a facial and green method to prepared Cu2O quantum dots on TiO2surfaces, but also supports an efficient approach to fabricate p-n heterojunctions with an increased interfacial charge transfer.
2. Based on the relation between the charge separation of heterojuntions and the potentials of the insoluble non-semiconductor compounds, we find an facile method to develop efficient heterostructured composites. The separation of the photogenerated electrons and holes in the CuX/P25heteroj unctions was easily controlled by tuning the CuX/Cu electrode potentials, which was closely related to the solubility (Ksp) of insoluble non-semiconductor compounds. This can be achieved by simply changing the anion species in CuX (X:(OH)2CO32-、S2-、OH-、 C2O42-). According to this method, we have found that the Cu2(OH)2CO3/Cu reduction potential is between the conduction band bottom of P25and the redox potential of H+/H2with a relatively large potential gradient. Thus, Cu2(OH)2CO3can be used as an excellent co-catalyst to build heteroj unction composites with P25, which exhibited an excellent charge separation efficiency and photocatalytic hydrogen production activity. The photocatalytic activity for hydrogen production of the heteroj unction composites was up to0.51mmol h-1under the simulant solar light irradiation, and the quantum efficiency was up to31.2%which was485times higher than that of pure P25. This work develops an excellent cocatalyst-Cu2(OH)2CO3for photocatalytic hydrogen production as well as provides an facile and efficient method for fabricating heteroj unction composite photocatalysts.
3. Considering the advantages of morphology control in photocatalytic hydrogen production, the flower-like ZnS/CuS heterostructured composites were prepared by the combination of microwave hydrothermal and cation exchange methods according to the interfacial charge transfer theory. The fabrication of the heterojunctions broadened the range of light response of ZnS. The photoexcited electrons of ZnS migrated to the redox potential of CuS/Cu2S under visible light irradiation, which can facilitate the effective separation of photogenerated electrons and holes in space. The visible photocatalytic activity towards hydrogen production for ZnS/CuS flower-like heterostructed composites without co-catalyst achieved0.33mmol h-1, and the quantum efficiency was up to22.8%under the wavelength with420nm visible light irradiation. Compared with the sheet-like photocatalyst composite, hydrogen production activity and quantum efficiency were improved. It proved that when both have photoinduced interfacial charge transfer (IFCT) effect, heterostructures photocatalyst composites with special morphology which possess high surface area and light absorption rate, have outstanding advantages in photoinduced charge separation. In addition, the formation mechanisms of the flakes and flower-like ZnS/CuS heterojunctions were also studied in detail by tuning the reaction time and temperature. Finally the relationship of the microstructure and the performance was revealed.
引文
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