不同形貌的纳米ZnO材料的控制合成及其光催化性能研究
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摘要
随着化学工业的迅速发展,环境污染问题,尤其是有机物的污染日趋严重,对有机污染物的治理已刻不容缓。光催化降解是一种非常有效的治理有机污染物的方法,与传统的吸附、过滤、沉降等处理方法相比,光催化降解过程不需要复杂的后处理工序,大大降低了实际应用过程中的操作成本。在此背景下,本论文拟研发高性能的纳米ZnO光催化材料用于有机污染物的催化降解。主要开展以下几个方面的研究:(1)对ZnO的制备方法进行系统优化,(2)对不同形貌纳米ZnO的形成机制进行详细探讨,(3)以罗丹明B降解为模型反应,评价不同形貌ZnO的光催化性能,分析影响催化活性的因素,(4)在多种表征基础上,对催化剂的结构与催化性能进行关联。
在最初的工作中,采用简单的一步溶剂热合成法,成功制备出了一种具有特殊绒球状三维纳米结构的ZnO材料,这种材料由一些纳米片组装而成,具有独特的孔道结构和较大的比表面积;借助实验结果,我们推测了这种三维纳米ZnO结构的生长机理。光催化测试结果表明:与具有花状,螺旋盘状,哑铃状和棒状形貌的纳米ZnO材料相比,绒球状纳米ZnO材料具有更高的光生电子-光生空穴分离效率,因而具有更高的光催化活性。为了进一步提高材料的光催化效率,采用一步合成法成功制备出了Ag掺杂的绒球状纳米ZnO材料,结果表明Ag的掺杂非但没有破坏ZnO原有的绒球状结构,而且还大大提高了其光催化性能。借助表征手段,对Ag在ZnO材料上的作用机制进行了深入探讨。
为了进一步探索纳米材料的制备方法,在制备过程中引入了一些新的考察因素。
首先,采用简单的超声辅助水热合成方法,通过调变柠檬酸的用量,成功制备出了一系列花状纳米ZnO材料,并系统考察了超声作用对花状纳米ZnO材料的形貌、光致发光和光催化性能的影响。超声作用对花状纳米ZnO材料形貌的影响程度与反应体系中柠檬酸的用量密切相关。光致发光和光催化性能测试结果表明,超声作用有效抑制了花状纳米ZnO材料中氧空位的相对含量,进而抑制了其绿色发光性能和光催化活性。在大量实验结果的基础上,提出了这种花状纳米ZnO材料所具有的独特的两步双模板生长机理,并对带缺陷ZnO材料的光致发光和光催化作用机制进行了深入探讨。
其次,基于大量的实验摸索,直接利用简单的超声作用成功制备出了纳米ZnO材料,并实现了Ag的一步掺杂。通过考察超声频率和Ag~+的加入对ZnO形貌的影响,深入探讨了超声作用下Ag~+参与的纳米ZnO材料独特的生长机理。光催化测试结果表明:Ag的掺杂能大幅提高ZnO的光催化活性。
最后,为了提高所合成的纳米ZnO材料的比表面积,引入P123作为模板剂来制备纳米ZnO材料,通过调节Zn~(2+)和P123的用量成功制备出了一系列具有较大比表面积的纳米ZnO材料。结果表明,无论是Zn~(2+)的用量还是P123的用量,对最终纳米ZnO材料的形貌和光催化性能都有显著影响。
综合以上研究内容,在论文的结尾部分对“纳米ZnO光催化材料的研究方法”进行了系统总结和深入探讨,并对纳米光催化材料的发展前景进行了展望。
With the rapid development of chemical industry, the pollution on environment, especially that originating from organic pollutants, becomes more and more serious, so, it is urgent to eliminate organic pollutants. Photocatalytic degradation is a kind of effective techniques for the removal of organic pollutants. Compared with traditional methods such as adsorption, filter and sedimentation, photocatalytic degradation can directly eliminate the secondary pollution without further treatment, largely decreasing the process cost. Under this background, we aim to develop high-performance nano ZnO photocatalytic materials used for the organic pollutants elimination. This dissertation mainly focuss on the following aspects: (1) the systematic optimization of preparation methods of ZnO materials, (2) the careful investigation on the formation mechanisms for the ZnO with different morphology, (3) the evaluation of photocatalytic performance by using the degradation of Rhodamine B as model reaction, (4) the exploration of structure-performance relationship on the basis of multiple characterizations.
Firstly, a series of nanosheets-constructed ZnO spheres with novel three-dimensional (3D) fluffy structure were successfully synthesized by a facile one-step solvothermal method. Such special hollow 3D structure makes the ZnO exhibit larger specific surface area. The photocatalytic activity measurement shows that such fluffy ZnO spheres do possess much higher photocatalytic activity than other commonly reported nanostructured ZnO, such as nanoflowers, nanospiraldisks, nanodumbbells and nanorods. Through one-pot synthesis Ag is readily doped on the fluffy spheres, which strongly interacts with them, further improving the photocatalytic performance of ZnO. Based on the properties and characterization results, a special growth mechanism for such fluffy ZnO spheres is proposed, and the photocatalytic reaction mechanism is also discussed.
Secondly, to further optimize the preparation methods, the ultrasonic technique was introduced to the preparation process. For comparison, a series of flower-like ZnO materials were successfully synthesized with or without ultrasonic-assistance through changing the dosage of citric acid during hydrothermal synthesis. It is found that both the ultrasonic treatment and the dosage of citric acid have influences on the flower-like structure. The photoluminescence spectra and the photocatalytic activity evaluation show that the employment of ultrasonic treatment during preparation decreases the relative content of oxygen vacancy, thus suppressing green emission and lowering the photocatalytic activity of such flower-like ZnO. However, the ultrasonic treatment can be used for the direct preparation of nano ZnO or Ag/ZnO meterials, whose morphology and photocatalytic activity are obviously influenced by the dosage of Ag~+ and the ultrasonic frequency. The special growth mechanism of such nano ZnO materials with or without Ag~+ involvement under ultrasonic treatment was
investigated in detail. Thirdly, to increase the specific surface area of ZnO materials, P123 was adopted as the template during preparation, as a result, a series of nano ZnO materials with special morphology and larger specific surface area were successfully synthesized. The effects of the concentration of Zn~(2+) and P123 on the morphology and photocatalytic activity of the ZnO materials were also studied.
Finally, a summary about“the Research Methods of Nano ZnO Materials”was made, and the development perspective of nano materials was outlooked.
在最初的工作中,采用简单的一步溶剂热合成法,成功制备出了一种具有特殊绒球状三维纳米结构的ZnO材料,这种材料由一些纳米片组装而成,具有独特的孔道结构和较大的比表面积;借助实验结果,我们推测了这种三维纳米ZnO结构的生长机理。光催化测试结果表明:与具有花状,螺旋盘状,哑铃状和棒状形貌的纳米ZnO材料相比,绒球状纳米ZnO材料具有更高的光生电子-光生空穴分离效率,因而具有更高的光催化活性。为了进一步提高材料的光催化效率,采用一步合成法成功制备出了Ag掺杂的绒球状纳米ZnO材料,结果表明Ag的掺杂非但没有破坏ZnO原有的绒球状结构,而且还大大提高了其光催化性能。借助表征手段,对Ag在ZnO材料上的作用机制进行了深入探讨。
为了进一步探索纳米材料的制备方法,在制备过程中引入了一些新的考察因素。
首先,采用简单的超声辅助水热合成方法,通过调变柠檬酸的用量,成功制备出了一系列花状纳米ZnO材料,并系统考察了超声作用对花状纳米ZnO材料的形貌、光致发光和光催化性能的影响。超声作用对花状纳米ZnO材料形貌的影响程度与反应体系中柠檬酸的用量密切相关。光致发光和光催化性能测试结果表明,超声作用有效抑制了花状纳米ZnO材料中氧空位的相对含量,进而抑制了其绿色发光性能和光催化活性。在大量实验结果的基础上,提出了这种花状纳米ZnO材料所具有的独特的两步双模板生长机理,并对带缺陷ZnO材料的光致发光和光催化作用机制进行了深入探讨。
其次,基于大量的实验摸索,直接利用简单的超声作用成功制备出了纳米ZnO材料,并实现了Ag的一步掺杂。通过考察超声频率和Ag~+的加入对ZnO形貌的影响,深入探讨了超声作用下Ag~+参与的纳米ZnO材料独特的生长机理。光催化测试结果表明:Ag的掺杂能大幅提高ZnO的光催化活性。
最后,为了提高所合成的纳米ZnO材料的比表面积,引入P123作为模板剂来制备纳米ZnO材料,通过调节Zn~(2+)和P123的用量成功制备出了一系列具有较大比表面积的纳米ZnO材料。结果表明,无论是Zn~(2+)的用量还是P123的用量,对最终纳米ZnO材料的形貌和光催化性能都有显著影响。
综合以上研究内容,在论文的结尾部分对“纳米ZnO光催化材料的研究方法”进行了系统总结和深入探讨,并对纳米光催化材料的发展前景进行了展望。
With the rapid development of chemical industry, the pollution on environment, especially that originating from organic pollutants, becomes more and more serious, so, it is urgent to eliminate organic pollutants. Photocatalytic degradation is a kind of effective techniques for the removal of organic pollutants. Compared with traditional methods such as adsorption, filter and sedimentation, photocatalytic degradation can directly eliminate the secondary pollution without further treatment, largely decreasing the process cost. Under this background, we aim to develop high-performance nano ZnO photocatalytic materials used for the organic pollutants elimination. This dissertation mainly focuss on the following aspects: (1) the systematic optimization of preparation methods of ZnO materials, (2) the careful investigation on the formation mechanisms for the ZnO with different morphology, (3) the evaluation of photocatalytic performance by using the degradation of Rhodamine B as model reaction, (4) the exploration of structure-performance relationship on the basis of multiple characterizations.
Firstly, a series of nanosheets-constructed ZnO spheres with novel three-dimensional (3D) fluffy structure were successfully synthesized by a facile one-step solvothermal method. Such special hollow 3D structure makes the ZnO exhibit larger specific surface area. The photocatalytic activity measurement shows that such fluffy ZnO spheres do possess much higher photocatalytic activity than other commonly reported nanostructured ZnO, such as nanoflowers, nanospiraldisks, nanodumbbells and nanorods. Through one-pot synthesis Ag is readily doped on the fluffy spheres, which strongly interacts with them, further improving the photocatalytic performance of ZnO. Based on the properties and characterization results, a special growth mechanism for such fluffy ZnO spheres is proposed, and the photocatalytic reaction mechanism is also discussed.
Secondly, to further optimize the preparation methods, the ultrasonic technique was introduced to the preparation process. For comparison, a series of flower-like ZnO materials were successfully synthesized with or without ultrasonic-assistance through changing the dosage of citric acid during hydrothermal synthesis. It is found that both the ultrasonic treatment and the dosage of citric acid have influences on the flower-like structure. The photoluminescence spectra and the photocatalytic activity evaluation show that the employment of ultrasonic treatment during preparation decreases the relative content of oxygen vacancy, thus suppressing green emission and lowering the photocatalytic activity of such flower-like ZnO. However, the ultrasonic treatment can be used for the direct preparation of nano ZnO or Ag/ZnO meterials, whose morphology and photocatalytic activity are obviously influenced by the dosage of Ag~+ and the ultrasonic frequency. The special growth mechanism of such nano ZnO materials with or without Ag~+ involvement under ultrasonic treatment was
investigated in detail. Thirdly, to increase the specific surface area of ZnO materials, P123 was adopted as the template during preparation, as a result, a series of nano ZnO materials with special morphology and larger specific surface area were successfully synthesized. The effects of the concentration of Zn~(2+) and P123 on the morphology and photocatalytic activity of the ZnO materials were also studied.
Finally, a summary about“the Research Methods of Nano ZnO Materials”was made, and the development perspective of nano materials was outlooked.
引文
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