ZnO和ZnO/CdSe的可控合成及其光催化性能研究
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摘要
纳米材料是21世纪科技发展的重要内容,纳米材料的制备和性能研究是纳米材料研究的重点.纳米材料因其所具有的优异性能,越来越多的引起人们的关注,在物理学、化学、生物医学和界面科学等学科均有广泛的应用。
ZnO是一种典型的直接带隙半导体材料,在常温下的禁带宽度为3.37eV,同时其激子结合能达到了60meV,所以有很高的应用价值。ZnO化学性质非常的稳定,同时具有非常特殊的导热和导电性能,因其具有极高的工作稳定性,在短波发光器件方面具有很高的应用价值。ZnO的应用非常广泛,在太阳能电池、光催化、压电材料、气敏材料和激光发射方面都有很高的利用价值。最近通过可控制备各种形貌的ZnO来提高其性能成为研究的热点。
本文的主要工作如下：
1.以硝酸锌和六次甲基四胺作为反应物,乙二胺作为表面活性剂,制备具有不同形貌的ZnO纳米材料。在该反应体系中,通过改变NaOH的加入量来改变溶液的PH值,得到具有“片状、哑铃状、双子结构和花状结构”形貌的ZnO纳米材料。通过XRD,SEM等物相表征方式证明得到了纯净的ZnO。分析了产物的构成,推测出了反应机理,并利用上述不同形貌的ZnO样品进行光催化降解亚甲基蓝实验,结果表明样品的形貌与光催化效率有直接关系,在光催化降解的对比中,具有最好光催化降解效率的是“花状”的ZnO,其次是“哑铃状”ZnO,而后是“片状”和“双子”结构的ZnO,光催化效果最差的是“无定形”的ZnO颗粒。推断出不同形貌的样品不同比表面积对光催化性能造成影响。
2.通过水溶液直接沉淀法,在室温条件下,使用乙酸锌和氢氧化钾制备了具有绒线球结构的ZnO。通过分析不同反应时间下所生成的ZnO的形貌,推测出了产物的生长机理。使用X射线衍射仪、扫描电子显微镜、透射电子显微镜和高倍透射电子显微镜对产物进行了物相分析和表征,在XRD图谱中看以看出除了ZnO的特征衍射峰外没有其他杂质峰的出现,说明说生成了纯净的ZnO。样品的SEM图显示绒线球状ZnO是由厚度为50nm的ZnO纳米片交错叠加构成的,在该结构中形成许多孔洞,可以作为载流子和小分子的通道作用。通过光催化降解亚甲基蓝实验证明了产物具有优良的光催化性能,并且光催化循环反应进行6次以后,样品的形貌和结构仍然保持完好,说明样品作为光催化剂具有良好的稳定性和耐久性。
3.ZnO的禁带宽度比较宽,在电子激发后具有较高的氧化还原电位,可以很好地降解有机污染物,但是过宽的禁带宽度只能利用紫外光,而对可见光没有响应,降低了光的使用效率。通过窄带半导体CdSe的复合,可以拓宽材料对光的响应范围,通过在可见光的照射下对比有机染料亚甲基蓝在以ZnO/CdSe复合物、P25、商业ZnO为光催化剂的降解速率得出ZnO/CdSe复合物具有更加优异的光催化性能,同时样品对光的响应由紫外光区扩展到可见光区,更加有效的利用了光能。我们水溶液法制备ZnO/CdSe复合物的方法具有能耗低、便捷、环境友好等优点,可以大范围推广使用。在反应的过程中,不加入任何有机的表面活性剂,只是通过改变反应的温度、稳定剂和ZnO的量得到负载量和微观结构不同的ZnO/CdSe复合物。本实验方法具有普适性,可以用来制备其他的半导体复合材料。
Nanomaterials with superior performance, more and more cause for concern. Nanomaterials is an important part of the21st century scientific and technological development Preparation and properties of nanomaterials is the focus of the study of nanomaterials and cross-use of the disciplines of physics, chemistry, biomedical and interface science.
ZnO is a key semiconductor for short wavelength electrooptical denices and low-voltage due to its large exciton binding energy of60meV and wide band gap(3.2eV). ZnO nanomaterials exhibit more optical properties and prominent electronic, and has been applied in solar cell, catalyst, piezoelectricity, gas sensor, laser generator and so on. At present, the research on applications and research on controllable synthesis of ZnO nanomaterials become attractive. The main contents of this thesis are listed as below:
1. ZnO with different morphology was prepared by changing pH in the reaction system consisting of Zn(NO3)2·6H2O, Hexamethylene tetramine and CH3COONH4The morphologies and structures of the prepared materials were detailedly characterized by SEM, XRD。 The photocatalytic activities of as-prepared ZnO samples were characterized by photodegradation of Methylene blue
2. In this paper, an efficient and simple route combined with a subsequent calcining process to synthesize pompon-like ZnO microstructures at room-temperature (25℃) has been developed. The samples were intensively investigated by SEM, TEM, HRTEM, XRD. The results indicate that the well-crystallized pompon-like ZnO is assembled by interlaced nanoplates with uniform thickness of about50nm. The photocatalytic trials confirm that the pompon-like ZnO exhibits excellent degradation efficiency under UV light. Moreover, the as-prepared ZnO samples show superior durability and stability after six photodegradation cycling runs. Finally, a mechanism was proposed to elucidate the photodegradation reaction of the pompon-like ZnO.
3. Semiconductor based nanoscale heterostructures are promising candidates for photocatalytic andphotovoltaic applications with the sensitization of a wide bandgap semiconductor with a narrow bandgap material being the most viable strategy to maximize the utilization of the solar spectrum. Here,we present a simple wet chemical route to obtain nanoscale heterostructures of ZnO/CdSe without usingany molecular linker. We show that the heterostructures with the lowest CdSe loading exhibit an exceptionally high activity for the degradation of methylene blue (MB) under solar irradiation conditions; In particular. the absence of any molecularlinker at the interface makes our method appealing for photovoltaic applications where faster rates of electron transfer at the heterojunctions are highly desirable.
ZnO是一种典型的直接带隙半导体材料,在常温下的禁带宽度为3.37eV,同时其激子结合能达到了60meV,所以有很高的应用价值。ZnO化学性质非常的稳定,同时具有非常特殊的导热和导电性能,因其具有极高的工作稳定性,在短波发光器件方面具有很高的应用价值。ZnO的应用非常广泛,在太阳能电池、光催化、压电材料、气敏材料和激光发射方面都有很高的利用价值。最近通过可控制备各种形貌的ZnO来提高其性能成为研究的热点。
本文的主要工作如下：
1.以硝酸锌和六次甲基四胺作为反应物,乙二胺作为表面活性剂,制备具有不同形貌的ZnO纳米材料。在该反应体系中,通过改变NaOH的加入量来改变溶液的PH值,得到具有“片状、哑铃状、双子结构和花状结构”形貌的ZnO纳米材料。通过XRD,SEM等物相表征方式证明得到了纯净的ZnO。分析了产物的构成,推测出了反应机理,并利用上述不同形貌的ZnO样品进行光催化降解亚甲基蓝实验,结果表明样品的形貌与光催化效率有直接关系,在光催化降解的对比中,具有最好光催化降解效率的是“花状”的ZnO,其次是“哑铃状”ZnO,而后是“片状”和“双子”结构的ZnO,光催化效果最差的是“无定形”的ZnO颗粒。推断出不同形貌的样品不同比表面积对光催化性能造成影响。
2.通过水溶液直接沉淀法,在室温条件下,使用乙酸锌和氢氧化钾制备了具有绒线球结构的ZnO。通过分析不同反应时间下所生成的ZnO的形貌,推测出了产物的生长机理。使用X射线衍射仪、扫描电子显微镜、透射电子显微镜和高倍透射电子显微镜对产物进行了物相分析和表征,在XRD图谱中看以看出除了ZnO的特征衍射峰外没有其他杂质峰的出现,说明说生成了纯净的ZnO。样品的SEM图显示绒线球状ZnO是由厚度为50nm的ZnO纳米片交错叠加构成的,在该结构中形成许多孔洞,可以作为载流子和小分子的通道作用。通过光催化降解亚甲基蓝实验证明了产物具有优良的光催化性能,并且光催化循环反应进行6次以后,样品的形貌和结构仍然保持完好,说明样品作为光催化剂具有良好的稳定性和耐久性。
3.ZnO的禁带宽度比较宽,在电子激发后具有较高的氧化还原电位,可以很好地降解有机污染物,但是过宽的禁带宽度只能利用紫外光,而对可见光没有响应,降低了光的使用效率。通过窄带半导体CdSe的复合,可以拓宽材料对光的响应范围,通过在可见光的照射下对比有机染料亚甲基蓝在以ZnO/CdSe复合物、P25、商业ZnO为光催化剂的降解速率得出ZnO/CdSe复合物具有更加优异的光催化性能,同时样品对光的响应由紫外光区扩展到可见光区,更加有效的利用了光能。我们水溶液法制备ZnO/CdSe复合物的方法具有能耗低、便捷、环境友好等优点,可以大范围推广使用。在反应的过程中,不加入任何有机的表面活性剂,只是通过改变反应的温度、稳定剂和ZnO的量得到负载量和微观结构不同的ZnO/CdSe复合物。本实验方法具有普适性,可以用来制备其他的半导体复合材料。
Nanomaterials with superior performance, more and more cause for concern. Nanomaterials is an important part of the21st century scientific and technological development Preparation and properties of nanomaterials is the focus of the study of nanomaterials and cross-use of the disciplines of physics, chemistry, biomedical and interface science.
ZnO is a key semiconductor for short wavelength electrooptical denices and low-voltage due to its large exciton binding energy of60meV and wide band gap(3.2eV). ZnO nanomaterials exhibit more optical properties and prominent electronic, and has been applied in solar cell, catalyst, piezoelectricity, gas sensor, laser generator and so on. At present, the research on applications and research on controllable synthesis of ZnO nanomaterials become attractive. The main contents of this thesis are listed as below:
1. ZnO with different morphology was prepared by changing pH in the reaction system consisting of Zn(NO3)2·6H2O, Hexamethylene tetramine and CH3COONH4The morphologies and structures of the prepared materials were detailedly characterized by SEM, XRD。 The photocatalytic activities of as-prepared ZnO samples were characterized by photodegradation of Methylene blue
2. In this paper, an efficient and simple route combined with a subsequent calcining process to synthesize pompon-like ZnO microstructures at room-temperature (25℃) has been developed. The samples were intensively investigated by SEM, TEM, HRTEM, XRD. The results indicate that the well-crystallized pompon-like ZnO is assembled by interlaced nanoplates with uniform thickness of about50nm. The photocatalytic trials confirm that the pompon-like ZnO exhibits excellent degradation efficiency under UV light. Moreover, the as-prepared ZnO samples show superior durability and stability after six photodegradation cycling runs. Finally, a mechanism was proposed to elucidate the photodegradation reaction of the pompon-like ZnO.
3. Semiconductor based nanoscale heterostructures are promising candidates for photocatalytic andphotovoltaic applications with the sensitization of a wide bandgap semiconductor with a narrow bandgap material being the most viable strategy to maximize the utilization of the solar spectrum. Here,we present a simple wet chemical route to obtain nanoscale heterostructures of ZnO/CdSe without usingany molecular linker. We show that the heterostructures with the lowest CdSe loading exhibit an exceptionally high activity for the degradation of methylene blue (MB) under solar irradiation conditions; In particular. the absence of any molecularlinker at the interface makes our method appealing for photovoltaic applications where faster rates of electron transfer at the heterojunctions are highly desirable.
引文
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