聚酰亚胺/碳纳米复合电极上光电转换、催化材料的制备及分析
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摘要
本硕士学位论文利用电化学原子层沉积(EC-ALD)、循环伏安法(CV)和电流时间法(i-t)等技术在聚酰亚胺(PI)与碳纳米管(CNTs)、石墨烯(GE)等复合材料表面制备了具有光电转换和催化性能的薄膜材料。然后利用形貌、结构与性能等多种表征手段,分析了所制备的材料。主要内容如下：
1. PI/COOH-CNTs导电基底上半导体光电转换材料CuSe的EC-ALD法制备及性能研究
成功制备了PI与羧基化碳纳米管(COOH-CNTs)的导电复合电极材料,然后利用EC-ALD沉积技术,在PI/COOH-CNTs复合电极上制备了具有光电转换性能的半导体纳米CuSe薄膜材料。在通过CV分别确定Cu、Se沉积电位的基础上,采用电流时间曲线法交替沉积了Cu和Se原子层最终获得CuSe化合物；由X射线衍射(XRD)分析结果得知CuSe沉积择优发生在(112)面；扫描电子显微镜(SEM)和能量色散光谱(EDS)数据证明所制备CuSe具有纳米级的棒状结构、Cu:Se比例接近于1：1；由紫外透射数据计算的CuSe半导体带隙为2.0eV,通过开路电位技术(OCP)研究表明CuSe晶体具有p型半导体性质。
2. PI/COOH-CNTs导电基底上半导体光电转换材料In2Te3的EC-ALD和脉冲沉积制备及光电性能研究
分别利用EC-ALD过程(电流时间技术)和脉冲沉积过程(三脉冲电流技术),在PI/COOH-CNTs复合电极上制备了具有光电转换性能的半导体纳米In2Te3薄膜材料。首先采用CV法分别确定In、Te沉积电位,然后用EC-ALD法和脉冲沉积过程实现了In2Te3半导体化合物的沉积；由XRD和EDS的研究结果说明,由EC-ALD法所制备的In2Te3薄膜具有多晶性质,而利用脉冲沉积过程制备的In2Te3薄膜则为无定型态；通过在光照和黑暗下条件下的开路电位技术(OCP)研究表明,用EC-ALD法和脉冲沉积过程制备的In2Te3薄膜均为p型半导体。
3. PI/COOH-CNTs和PI/GE复合导电基底上Pd纳米颗粒的制备及其催化性能研究
利用电化学方法分别在PI/COOH-CNTs和PI/GE电极材料表面制备了Pd纳米催化剂。CV法研究结果得出Pd2+离子在两种电极上的电化学行为基本一致,且在PI/GE电极上的电流密度较大；通过XRD和SEM数据发现,在相同的沉积条件下,两种电极材料上的Pd纳米催化剂均为面心立方晶体,且形貌都是均一的花状结构；通过对甲酸的电化学催化行为研究发现,负载于PI/COOH-CNTs和PI/GE电极材料表面的纳米Pd对甲酸均有明显的催化氧化性能。
In this master's paper, several thin films material possessed photoelectric conversion and catalytic performance is researched and prepared on polyimide (PI) and carbon nanotubes (CNTs), graphene (GE) composite membrane by means of cyclic voltammeter (CV), Amperometric i-t, differential pulse voltammetry (DPV) technology, and so on. The structure, surface morphology, composition and performance of the as-prepared thin films are characteried by X-ray diffraction (XRD), field emission scanning electron microscope (FE-SEM) with an energy dispersive X-ray (EDS) analyzer, and some spectrophotometer. The main contents are as follows:
1. Electrochemical atomic Layer deposition (EC-ALD) of nanosemiconductor CuSe on PI/COOH-CNTs composition membrane and photoelectric property researches
The CuSe thin films were successfully prepared on PI/COOH-CNTs membrane by EC-ALD technology. Through the electrochemcial study of cyclic voltammetric behaviours, the deposition potential of Cu and Se were determined; The Cu and Se atomic layer were alternately deposited by amperometric methods (i-t); According to XRD results, it can be seen that the preferred planes of the as-prepared CuSe thin film is at (112) plane; SEM and EDS analysis indicate that the CuSe film is nanoscale short rod structure, and average atom ratio of Cu:Se is close to1:1. The band gap cauclated from ultraviolet transmission data is calculated to be2.0eV, and the CuSe crystals are domenstrated to have p-type semiconductor property.
2. EC-ALD and codeposition of nanosemiconductor In2Te3on PI/COOH-CNTs composition membrane and photoelectric property researches
The In2Te3thin films were prepared on PI/COOH-CNTs membrane by EC-ALD (amperometric i-t technology) and codeposition (triple pulse current technology) process; Through the electrochemcial study of cyclic voltammetric behaviours to determine the deposition potential of and the underpotional of In and Te in the deposition process. Through XRD and EDS characterization, it is proved that the thin film deposited by EC-ALD is polycrystalline structure, while it is amorphous struture through codeposition process. The OCP and amperometric i-t researches under illumination and dark show that the as-prepared In2Te3thin films using these two methods are both p-type semiconductors, and it is very suitable for semiconductor material.
3. Study of eledtrodoposition of Pd nanoparticles on PI/COOH-CNTs and PI/GE composite substrate and its catalytic performance research
Pd nanocatalysts wree prepared respectively on the surface of PI/COOH-CNTs and PI/GE electrodes by electrochemical method. The CV results indicate that the electrochemcial behaviours of PdCl2solution on PI/COOH-CNTs and PI/GE electrodes were similar, and the current density on the PI/GE electrode is larger than that on the PI/COOH-CNTs electrode. According to XRD and SEM data, it can be observed that the Pd on two kinds of electrode materials are face centered cubic structure nanocatalysts, and the surface morphology are flower structure. Through electrochemical catalytic behavior research for formic acid, it is found that the Pd nanoparticles on the PI/COOH-CNTs/PI and PI/GE electrodes both have obvious catalytic oxidation properties for formic acid.
1. PI/COOH-CNTs导电基底上半导体光电转换材料CuSe的EC-ALD法制备及性能研究
成功制备了PI与羧基化碳纳米管(COOH-CNTs)的导电复合电极材料,然后利用EC-ALD沉积技术,在PI/COOH-CNTs复合电极上制备了具有光电转换性能的半导体纳米CuSe薄膜材料。在通过CV分别确定Cu、Se沉积电位的基础上,采用电流时间曲线法交替沉积了Cu和Se原子层最终获得CuSe化合物；由X射线衍射(XRD)分析结果得知CuSe沉积择优发生在(112)面；扫描电子显微镜(SEM)和能量色散光谱(EDS)数据证明所制备CuSe具有纳米级的棒状结构、Cu:Se比例接近于1：1；由紫外透射数据计算的CuSe半导体带隙为2.0eV,通过开路电位技术(OCP)研究表明CuSe晶体具有p型半导体性质。
2. PI/COOH-CNTs导电基底上半导体光电转换材料In2Te3的EC-ALD和脉冲沉积制备及光电性能研究
分别利用EC-ALD过程(电流时间技术)和脉冲沉积过程(三脉冲电流技术),在PI/COOH-CNTs复合电极上制备了具有光电转换性能的半导体纳米In2Te3薄膜材料。首先采用CV法分别确定In、Te沉积电位,然后用EC-ALD法和脉冲沉积过程实现了In2Te3半导体化合物的沉积；由XRD和EDS的研究结果说明,由EC-ALD法所制备的In2Te3薄膜具有多晶性质,而利用脉冲沉积过程制备的In2Te3薄膜则为无定型态；通过在光照和黑暗下条件下的开路电位技术(OCP)研究表明,用EC-ALD法和脉冲沉积过程制备的In2Te3薄膜均为p型半导体。
3. PI/COOH-CNTs和PI/GE复合导电基底上Pd纳米颗粒的制备及其催化性能研究
利用电化学方法分别在PI/COOH-CNTs和PI/GE电极材料表面制备了Pd纳米催化剂。CV法研究结果得出Pd2+离子在两种电极上的电化学行为基本一致,且在PI/GE电极上的电流密度较大；通过XRD和SEM数据发现,在相同的沉积条件下,两种电极材料上的Pd纳米催化剂均为面心立方晶体,且形貌都是均一的花状结构；通过对甲酸的电化学催化行为研究发现,负载于PI/COOH-CNTs和PI/GE电极材料表面的纳米Pd对甲酸均有明显的催化氧化性能。
In this master's paper, several thin films material possessed photoelectric conversion and catalytic performance is researched and prepared on polyimide (PI) and carbon nanotubes (CNTs), graphene (GE) composite membrane by means of cyclic voltammeter (CV), Amperometric i-t, differential pulse voltammetry (DPV) technology, and so on. The structure, surface morphology, composition and performance of the as-prepared thin films are characteried by X-ray diffraction (XRD), field emission scanning electron microscope (FE-SEM) with an energy dispersive X-ray (EDS) analyzer, and some spectrophotometer. The main contents are as follows:
1. Electrochemical atomic Layer deposition (EC-ALD) of nanosemiconductor CuSe on PI/COOH-CNTs composition membrane and photoelectric property researches
The CuSe thin films were successfully prepared on PI/COOH-CNTs membrane by EC-ALD technology. Through the electrochemcial study of cyclic voltammetric behaviours, the deposition potential of Cu and Se were determined; The Cu and Se atomic layer were alternately deposited by amperometric methods (i-t); According to XRD results, it can be seen that the preferred planes of the as-prepared CuSe thin film is at (112) plane; SEM and EDS analysis indicate that the CuSe film is nanoscale short rod structure, and average atom ratio of Cu:Se is close to1:1. The band gap cauclated from ultraviolet transmission data is calculated to be2.0eV, and the CuSe crystals are domenstrated to have p-type semiconductor property.
2. EC-ALD and codeposition of nanosemiconductor In2Te3on PI/COOH-CNTs composition membrane and photoelectric property researches
The In2Te3thin films were prepared on PI/COOH-CNTs membrane by EC-ALD (amperometric i-t technology) and codeposition (triple pulse current technology) process; Through the electrochemcial study of cyclic voltammetric behaviours to determine the deposition potential of and the underpotional of In and Te in the deposition process. Through XRD and EDS characterization, it is proved that the thin film deposited by EC-ALD is polycrystalline structure, while it is amorphous struture through codeposition process. The OCP and amperometric i-t researches under illumination and dark show that the as-prepared In2Te3thin films using these two methods are both p-type semiconductors, and it is very suitable for semiconductor material.
3. Study of eledtrodoposition of Pd nanoparticles on PI/COOH-CNTs and PI/GE composite substrate and its catalytic performance research
Pd nanocatalysts wree prepared respectively on the surface of PI/COOH-CNTs and PI/GE electrodes by electrochemical method. The CV results indicate that the electrochemcial behaviours of PdCl2solution on PI/COOH-CNTs and PI/GE electrodes were similar, and the current density on the PI/GE electrode is larger than that on the PI/COOH-CNTs electrode. According to XRD and SEM data, it can be observed that the Pd on two kinds of electrode materials are face centered cubic structure nanocatalysts, and the surface morphology are flower structure. Through electrochemical catalytic behavior research for formic acid, it is found that the Pd nanoparticles on the PI/COOH-CNTs/PI and PI/GE electrodes both have obvious catalytic oxidation properties for formic acid.
引文
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