Cu_2O及In_2O_3基纳米异质结构制备及性能研究
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摘要
复合材料,尤其是纳米尺度下的复合材料具有普通纳米材料所不具有的多功能,高性能等优点。因此,随着纳米科技尤其是半导体微、纳制备技术的进步,纳米复合材料越来越成为科学研究的前沿热点和先进材料的发展方向。在本文中,我们以Cu20和In203两种氧化物为纳米异质结构的基础研究对象,通过水热、热蒸发、原子层沉积等制备方法,分别系统的研究了几种Cu20基和In203基异质纳米结构的可控制备、形貌表征、部分光电学性能及其构效关系,主要研究内容和创新点如下：
1Cu2O/ZnO异质纳米结构的制备及其光致发光、场发射、光催化性能研究
由于Cu20与ZnO的热不稳定性以及晶格常数的差距,常规Cu2O/ZnO异质纳米结构大多以电沉积、电化学沉积或者溅射的方式制备,以薄膜的形式存在,具有形貌单一,结构简单,性能一般等缺陷。通过利用一种有机连结剂聚乙酰亚胺的吸附作用,结合低温水热法和高温热退火分步工艺,我们在国际上首次将Cu20微米结构与ZnO纳米颗粒复合在了一起。我们的结果具有复合结构新颖,复合方法简单并可被应用于各种不同形貌及材料等优点。此外,我们研究了所制备的Cu2O/ZnO异质纳米结构的光致发光谱,发现该纳米异质结构具有一个新的发光峰；测量并比较了所制备纳米异质结构与基础材料的全光谱光催化和室温场发射性能。实验结果证实了所制备的Cu2O/ZnO纳米异质结构具有很好的光催化活性和场发射增强性能；复合较多ZnO纳米颗粒的Cu2O/ZnO样品增强性能要优于复合较少ZnO纳米颗粒的Cu2O/ZnO样品。我们从表面形貌改变、纳米尺寸效应等几个方面分析了增强性能的来源。另从半导体能带理论的角度对新的发光峰和增强的光-电性能进行了初步的解释和可能机理的推断。
2.Cu2O/TiO2/ZnO三元纳米异质结构的制备及其场发射、光催化性能研究
设计并成功制备了Cu2O/TiO2/ZnO三元纳米异质结构。首先利用有机钛前驱体在较低温环境中首次合成了比较均匀的Cu2O/TiO2核壳纳米结构,随后利用有机连结剂在Cu2O/TiO2核壳纳米结构的表面上成功复合ZnO纳米颗粒,形成了Cu2O/TiO2/ZnO二元纳米异质结构。对所制备的Cu2O、Cu2O/TiO2核壳纳米结构以及Cu2O/TiO2/ZnO三元纳米异质结构的室温场发射性能和紫外一可见光催化性能进行了研究和分析。结果证实所有复合结构的样品的场发射和光催化性能一如我们在设计该结构时所预期有显著的增强,Cu2O/TiO2/ZnO三元纳米异质结构的增强性能更佳。从半导体能带理论的角度,我们对增强性能的微观起源做了分析。
3.In2O3/Al2O3核壳纳米异质结构的制备及其场发射增强性能研究
采用热蒸发工艺,使用不同的生长机制合成了四种In203微、纳米结构。选择了其中一种单晶In203纳米棒作为基础材料,利用ALD工艺在其外复合了厚度可控,形状均匀的A1203多晶壳层结构。通过对壳层厚度的调控,对核壳结构进行热退火和氢等离子等不同的后处理,制备了一系列的In2O3/Al2O3核壳纳米异质结构样品,测量了所制备样品的室温场发射性能,较系统的分析了In2O3/Al2O3核壳纳米异质结构的场发射性能的构效关系,并结合实验结果加以了理论分析。对从微观上理解场发射机制及其增强机理具有一定的意义。
4. Cu2O和In203纳米形貌的可控制备以及单根超长In2O3微米棒的湿度传感性能
采用操作简单,成本低廉的水热法、热蒸发等工艺,实现了多种Cu20和In203纳米形貌的可控制备。初步研究了主要工艺参数(反应时间、反应温度和材料配比)对样品形貌的影响。此外,制备了一种具有良好单晶性的In2O3宏观微米结构,成功分散出单根超长In203微米棒并采用丝网印刷的方法制备了接触良好的In2O3-Ag电极并测量了它的湿度传感性能。
Composites, especially nano-composites are often multifunctional and have high performance comparing with ordinary nano-materials. Therefore, nano-composites have gained more and more research attentions and are leading the orientation of advaced materials in pace with the development of semiconductor micro/nano science and techniques. In this dissertation, we focus on the controllable synthesis, morphology characterization, optical and electrical properties and structure-activity relationships of Cu2O and In2O3based nano-heterojunction structures. The main research contents and innovations are listed below:
1. Synthesis of Cu2O/ZnO nano-heterojunction structures and their photoluminescence (PL), photocatalytic (PC) and field emission (FE) properties.
Because of the thermolability of Cu2O and the lattice mismatch between Cu2O and ZnO, Cu2O/ZnO nano-heterojunctions are normally made by electrodeposition, electrochemical deposition or sputtering, which impose restrictions on the nanostructure of the heterojunctions that can only exist in the form of film with a simple planar interface, lead to inadequate minority carrier transport length, high recombination rate of the photogenerated electron-hole pairs and low sunlight utilizing efficiency. We report an easy access route for synthesizing ZnO nanoparticles on different Cu2O micro structures by low temperature hydrothermal and thermal annealing process with the assistance of polyethyleneimine (PEI). Our synthesis route is facile to operate and can be applied to manufacturing a variety of compound materials with various morphologies. Despite the new nano-heterostructure, the PL properties of the Cu2O/ZnO nano-heterojunctions are measured and a new light peak is found. The FE and PC properties of the Cu2O/ZnO nano-heterostructures are tested and compared with those of pure Cu2O samples. We find that the as-prepared Cu2O/ZnO nano-heterojunctions have increased FE and PC properties; those nano-heterojunctions with more ZnO nanoparticles has better FE and PC performance than those with fewer. We analysed the origin of the high performances from the aspects of morphology change and nano-size effect. We also gave out a preliminary interpretation of the new PL peak and the enhanced optical/electrical properties by using semiconductor band theory.
2. Synthesis of Cu2O/TiO2/ZnO tenary nano-heterojunction structures and their field emission and photocatalytic properties.
We designed and successfully prepared Cu2O/TiO2/ZnO tenary nano-heterojunction structures. In the first step, we fabricated Cu2O/TiO2core-shell nanostructure in a low temperature hydrothermal and thermal evaporation process by using Titanium (Ⅳ) oxideacetylacetonate (TiO(acac)2) as precursor. Second, we combined ZnO nanoparticals on Cu2O/TiO2core-shell nanostructure with the assistance of polyethyleneimine (PEI). We tested and compared room temperature field emission and UV-Vis photocatalytic properties of Cu2O, Cu2O/TiO2core-shell nanostructure and CuO/TiO2/ZnO tenary nano-heterojunction structure. The results proved that all the nano composites have enhanced performance as we anticipated. Cu2O/TiO2/ZnO tenary nano-heterojunction structure has better enhancement than Cu2O/TiO2core-shell nanostructure. We gave a theoretical explanation for the enhancement by using semiconductor band theory.
3. Synthesis of In2O3/Al2O3core-shell nano-heterojunction structures and their field emission enhancement.
We synthesized four kinds of In2O3micro/nano-structures via thermal evaporation method and chose In2O3nano-rods as core, coated Al2O3shell on it using atomic layer deposition (ALD) process. We manufactured samples with diffierent shell thickness, treated them with thermal annealing and H2plasma treatment. We measured room temperature field emission properties of all the samples, systematically analysed the structure-activity relationships of In2O3/Al2O3core-shell nano-heterojunction structures and their field emission properties based on the experiment results.
4. Synthesis of Cu2O and In2O3nano structures.
We accomplished the controlled preparation of various Cu2O and InO3nano structures via hydrothermal and thermal evaporation methods. We preliminary studied the influence of main process parameters (reaction time, temperature, source material ratio and so on) to samples' morphologies. Besides, we synthesized a macroscopic In2O3monocrystal microstructure and successfully dispersed it into sigle super-long In2O3micro-rods. In2O3-Ag electrodes of good Ohm contact are fabricated by screen print method and their humidity sensor properties are tested.
1Cu2O/ZnO异质纳米结构的制备及其光致发光、场发射、光催化性能研究
由于Cu20与ZnO的热不稳定性以及晶格常数的差距,常规Cu2O/ZnO异质纳米结构大多以电沉积、电化学沉积或者溅射的方式制备,以薄膜的形式存在,具有形貌单一,结构简单,性能一般等缺陷。通过利用一种有机连结剂聚乙酰亚胺的吸附作用,结合低温水热法和高温热退火分步工艺,我们在国际上首次将Cu20微米结构与ZnO纳米颗粒复合在了一起。我们的结果具有复合结构新颖,复合方法简单并可被应用于各种不同形貌及材料等优点。此外,我们研究了所制备的Cu2O/ZnO异质纳米结构的光致发光谱,发现该纳米异质结构具有一个新的发光峰；测量并比较了所制备纳米异质结构与基础材料的全光谱光催化和室温场发射性能。实验结果证实了所制备的Cu2O/ZnO纳米异质结构具有很好的光催化活性和场发射增强性能；复合较多ZnO纳米颗粒的Cu2O/ZnO样品增强性能要优于复合较少ZnO纳米颗粒的Cu2O/ZnO样品。我们从表面形貌改变、纳米尺寸效应等几个方面分析了增强性能的来源。另从半导体能带理论的角度对新的发光峰和增强的光-电性能进行了初步的解释和可能机理的推断。
2.Cu2O/TiO2/ZnO三元纳米异质结构的制备及其场发射、光催化性能研究
设计并成功制备了Cu2O/TiO2/ZnO三元纳米异质结构。首先利用有机钛前驱体在较低温环境中首次合成了比较均匀的Cu2O/TiO2核壳纳米结构,随后利用有机连结剂在Cu2O/TiO2核壳纳米结构的表面上成功复合ZnO纳米颗粒,形成了Cu2O/TiO2/ZnO二元纳米异质结构。对所制备的Cu2O、Cu2O/TiO2核壳纳米结构以及Cu2O/TiO2/ZnO三元纳米异质结构的室温场发射性能和紫外一可见光催化性能进行了研究和分析。结果证实所有复合结构的样品的场发射和光催化性能一如我们在设计该结构时所预期有显著的增强,Cu2O/TiO2/ZnO三元纳米异质结构的增强性能更佳。从半导体能带理论的角度,我们对增强性能的微观起源做了分析。
3.In2O3/Al2O3核壳纳米异质结构的制备及其场发射增强性能研究
采用热蒸发工艺,使用不同的生长机制合成了四种In203微、纳米结构。选择了其中一种单晶In203纳米棒作为基础材料,利用ALD工艺在其外复合了厚度可控,形状均匀的A1203多晶壳层结构。通过对壳层厚度的调控,对核壳结构进行热退火和氢等离子等不同的后处理,制备了一系列的In2O3/Al2O3核壳纳米异质结构样品,测量了所制备样品的室温场发射性能,较系统的分析了In2O3/Al2O3核壳纳米异质结构的场发射性能的构效关系,并结合实验结果加以了理论分析。对从微观上理解场发射机制及其增强机理具有一定的意义。
4. Cu2O和In203纳米形貌的可控制备以及单根超长In2O3微米棒的湿度传感性能
采用操作简单,成本低廉的水热法、热蒸发等工艺,实现了多种Cu20和In203纳米形貌的可控制备。初步研究了主要工艺参数(反应时间、反应温度和材料配比)对样品形貌的影响。此外,制备了一种具有良好单晶性的In2O3宏观微米结构,成功分散出单根超长In203微米棒并采用丝网印刷的方法制备了接触良好的In2O3-Ag电极并测量了它的湿度传感性能。
Composites, especially nano-composites are often multifunctional and have high performance comparing with ordinary nano-materials. Therefore, nano-composites have gained more and more research attentions and are leading the orientation of advaced materials in pace with the development of semiconductor micro/nano science and techniques. In this dissertation, we focus on the controllable synthesis, morphology characterization, optical and electrical properties and structure-activity relationships of Cu2O and In2O3based nano-heterojunction structures. The main research contents and innovations are listed below:
1. Synthesis of Cu2O/ZnO nano-heterojunction structures and their photoluminescence (PL), photocatalytic (PC) and field emission (FE) properties.
Because of the thermolability of Cu2O and the lattice mismatch between Cu2O and ZnO, Cu2O/ZnO nano-heterojunctions are normally made by electrodeposition, electrochemical deposition or sputtering, which impose restrictions on the nanostructure of the heterojunctions that can only exist in the form of film with a simple planar interface, lead to inadequate minority carrier transport length, high recombination rate of the photogenerated electron-hole pairs and low sunlight utilizing efficiency. We report an easy access route for synthesizing ZnO nanoparticles on different Cu2O micro structures by low temperature hydrothermal and thermal annealing process with the assistance of polyethyleneimine (PEI). Our synthesis route is facile to operate and can be applied to manufacturing a variety of compound materials with various morphologies. Despite the new nano-heterostructure, the PL properties of the Cu2O/ZnO nano-heterojunctions are measured and a new light peak is found. The FE and PC properties of the Cu2O/ZnO nano-heterostructures are tested and compared with those of pure Cu2O samples. We find that the as-prepared Cu2O/ZnO nano-heterojunctions have increased FE and PC properties; those nano-heterojunctions with more ZnO nanoparticles has better FE and PC performance than those with fewer. We analysed the origin of the high performances from the aspects of morphology change and nano-size effect. We also gave out a preliminary interpretation of the new PL peak and the enhanced optical/electrical properties by using semiconductor band theory.
2. Synthesis of Cu2O/TiO2/ZnO tenary nano-heterojunction structures and their field emission and photocatalytic properties.
We designed and successfully prepared Cu2O/TiO2/ZnO tenary nano-heterojunction structures. In the first step, we fabricated Cu2O/TiO2core-shell nanostructure in a low temperature hydrothermal and thermal evaporation process by using Titanium (Ⅳ) oxideacetylacetonate (TiO(acac)2) as precursor. Second, we combined ZnO nanoparticals on Cu2O/TiO2core-shell nanostructure with the assistance of polyethyleneimine (PEI). We tested and compared room temperature field emission and UV-Vis photocatalytic properties of Cu2O, Cu2O/TiO2core-shell nanostructure and CuO/TiO2/ZnO tenary nano-heterojunction structure. The results proved that all the nano composites have enhanced performance as we anticipated. Cu2O/TiO2/ZnO tenary nano-heterojunction structure has better enhancement than Cu2O/TiO2core-shell nanostructure. We gave a theoretical explanation for the enhancement by using semiconductor band theory.
3. Synthesis of In2O3/Al2O3core-shell nano-heterojunction structures and their field emission enhancement.
We synthesized four kinds of In2O3micro/nano-structures via thermal evaporation method and chose In2O3nano-rods as core, coated Al2O3shell on it using atomic layer deposition (ALD) process. We manufactured samples with diffierent shell thickness, treated them with thermal annealing and H2plasma treatment. We measured room temperature field emission properties of all the samples, systematically analysed the structure-activity relationships of In2O3/Al2O3core-shell nano-heterojunction structures and their field emission properties based on the experiment results.
4. Synthesis of Cu2O and In2O3nano structures.
We accomplished the controlled preparation of various Cu2O and InO3nano structures via hydrothermal and thermal evaporation methods. We preliminary studied the influence of main process parameters (reaction time, temperature, source material ratio and so on) to samples' morphologies. Besides, we synthesized a macroscopic In2O3monocrystal microstructure and successfully dispersed it into sigle super-long In2O3micro-rods. In2O3-Ag electrodes of good Ohm contact are fabricated by screen print method and their humidity sensor properties are tested.
引文
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