一维TiO_2与ZnO纳米阵列的设计、制备及性能研究
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摘要
纳米有序阵列,尤其是在透明导电基底上制备的无支撑自立纳米棒与纳米管有序阵列可在多种器件上进行应用。当将纳米阵列用于光伏器件时,这些结构可以增加电荷生成层与电荷传递层之间的界面面积,提高提取电荷的效率。本论文选取TiO_2与ZnO两种目前研究最广泛的宽禁带金属氧化物半导体材料,通过不同技术手段制备了TiO_2与ZnO的纳米棒与纳米管阵列,研究探讨了这些纳米阵列在纳米器件领域,尤其是在有机-无机杂化太阳能电池器件领域的应用。
在ITO玻璃表面磁控溅射Al层,然后阳极氧化可制得多孔阳极氧化铝(AAO)膜/ITO玻璃复合模板。为了避免阳极氧化过程中AAO膜的破裂和脱落,在溅射高纯Al前,添加了Ti和W层分别作为连接层和缓冲层。磁控溅射后,通过热处理消除了溅射层的内应力,改善了各溅射层之间的结合力。在阳极氧化过程中,当发展较快的孔洞到达Al层底部时,会氧化底部的W缓冲层,对孔洞的快速发展起到缓冲作用,从而延缓了AAO膜底部的破裂和脱层,使大面积纳米孔洞阵列得以生成。
采用溶胶-凝胶电泳法在AAO/ITO复合模板内填充TiO_2纳米棒与纳米管有序阵列,电泳法制备的TiO_2纳米结构随TiO_2溶胶陈化时间的延长,由纳米棒逐渐转变为纳米管结构。研究发现,在AAO模板孔洞底部的环状W电极是形成不同结构的前提,而溶胶溶液中带电粒子的扩散速度和纳米阵列的沉积速度的竞争则是形成不同结构的原因。将制备的TiO_2纳米阵列与p型聚合物聚3-己基噻酚(P3HT)结合,制成TiO_2纳米阵列/P3HT无机-有机杂化太阳能电池。纳米棒和纳米管太阳能电池的光电转换效率分别是0.38%和0.48%。相比文献中类似方法制备的TiO_2纳米晶结构杂化太阳能电池0.22%的转换效率,本文中制备的TiO_2纳米棒与纳米管阵列太阳能电池效率提高了约73%到118%的效率,显示了纳米有序阵列结构的巨大优势。
通过磁控溅射、热处理二步法在独立AAO模板上制备出TiO_2纳米阵列。AAO模板参数对TiO_2的纳米结构具有决定作用,200 nm的孔径导致纳米管结构的生成,80 nm孔径的双面开孔模板导致纳米棒结构的生成,而80 nm的单孔模板导致闭口纳米管的生成。XRD分析显示TiO_2纳米管阵列为多晶锐钛矿结构,光致发光(PL)谱分析发现制备的纳米管与纳米棒阵列都为间接带隙半导体,纳米棒中的氧空位缺陷多于纳米管结构。将TiO_2纳米管阵列层从AAO模板脱离,转移到ITO玻璃上,旋涂一层P3HT,组成TiO_2纳米管/P3HT杂化太阳能电池。研究发现,具有TiO_2结合层结构的TiO_2纳米管/P3HT杂化太阳能电池性能比无结合层的电池显著提高,光电转换效率提高了8倍,达到0.34%。而采用n型富勒烯衍生物PCBM与P3HT充分混合后,由于电子-空穴对的有效分离,短路电流密度提高了近5倍,达到9.98 mA cm-2;光电转换效率提高了近6倍,达到2.07%。
利用电沉积、热处理二步法在AAO模板中制备出了ZnO纳米管阵列和Cu@ZnO纳米同轴电缆阵列。在光致发光测试中,Cu@ZnO纳米同轴电缆被激发出绿光发射带,说明在Cu@ZnO纳米同轴电缆界面处的ZnO被Cu掺杂。还将独立AAO模板上的ZnO纳米阵列合成技术转移到AAO/ITO复合模板,在ITO玻璃上制备出ZnO纳米棒与纳米管有序阵列,ZnO有序阵列的载流子密度约为2.67×1020 cm-3,在透明导电氧化物领域具有很好的应用前景。
通过一步电沉积法在ITO导电玻璃上制得ZnO纳米棒阵列。在温度为55℃时,得到的是致密的ZnO膜,而在85℃时,得到的是ZnO纳米棒阵列,说明ZnO膜的形貌取决于沉积温度。用85℃电沉积得到的ZnO纳米棒阵列组装的ITO/ZnO/P3HT:PCBM/Ag太阳能电池具有与ZnO纳米棒阵列共型形貌。对于未退火ZnO纳米棒阵列制备的太阳能电池,暴露在ZnO底部的主导缺陷区与共混聚合物直接接触,导致了严重的电流泄露。而通过退火消除ZnO底部暴露在外的缺陷,以及通过沉积更致密的ZnO纳米棒来阻止共混聚合物与主导缺陷区的接触都可以有效避免电流的泄露,从而进一步提高电池的开路电压。由于P3HT与PCBM的混合极其密切,它们的接触面积非常大,P3HT:PCBM混合物生成的光电流在总电流中占主导地位。通过ALD法在ZnO纳米棒表面覆盖一层TiO_2有效减少了电子和空穴的复合几率,进而提高了光电转换效率,电池的转换效率达到2.10%,高于无壳层的ZnO纳米棒阵列组装的太阳能电池。
Ordered nanomaterial arrays, especially arrays of free-standing nanorods and nanotubes on conducting substrates have been applied in many different fields. When implemented in photovoltaics, these structures can increase the surface area between the charge-generating and charge-transporting layers, improving the efficiency of charge extraction. In this study, we choose TiO_2 and ZnO which are two of the most extensively studied wide band gap metallic oxide semiconductors. The nanorod and nanotube arrays of the two materials were prepared by different techniques. The applications of these arrays in nanodevices, especially in organic-inorganic hybrid solar cells were researched in detail.
Porous anodic aluminum oxide (AAO) membrane/ITO glass composite templates were prepared by anodizing the magnetron sputtered Al on the ITO glass. For avoiding the delaminating and cracking of the AAO at the bottom of the pores during anodization, Ti and W layers were sputtered before the magnetron sputtering of Al. Annealing was carried out to eliminate the inner stress of the sputtered layers, improving the connection between these layers. During anodization, the faster developing pores would oxidize the W barrier layer when it reached the bottom. The oxidation of the W slowed down the development of the pores, preventing the cracking of the AAO membrane and ensuring the completion of the whole array of the nanopores.
Arrays of TiO_2 nanorods and nanotubes were embedded in AAO/ITO template by sol-gel electrophoresis. The structure of the TiO_2 changed from nanorod to nanotube with the sol aging time. The W ring electrode was the precondition to the formation of different structures. The competition between the diffusion rate of the charged particles and the deposition rate caused the formation of different structures. The as-prepared TiO_2 arrays were fabricated in hybrid solar cells by spin coating P3HT in the arrays. The conversion efficiencies were up to 0.38% and 0.48% for the TiO_2 nanorod and nanotube solar cells. The efficiency of the nanotube array solar cell was improved by 26% compared to the nanorod cell due to the larger specific surface area.
TiO_2 arrays were also prepared in free-standing AAO template by magnetron sputtering and annealing. The parameters of the porous AAO template were highly influential in determining the nanostructure of the sputtered film. The template with a 200 nm pore diameter would result in the formation of nanotubes, while the double-sided through hole template with a 80 nm pore diameter would result in the formation of nanorods, and the one-sided blind hole template with a 80 nm pore diameter would result in the formation of closed-end tubes. The XRD measurement showed the annealed TiO_2 nanotubular film was polycrystalline anatase phase without preferred orientation. The photoluminescence (PL) spectrum revealed the as-prepared TiO_2 nanostructural film was an indirect bandgap semiconductor with oxygen vacancy defects that exist more in rods than in tubes. Then, the TiO_2 nanotubular film were removed from the AAO and transferred onto an ITO glass. A layer of P3HT was spin coated into the TiO_2 nanotube array to fabricate a hybrid solar cell. By adding a TiO_2 connecting layer between TiO_2 nanotubular film and ITO glass, the performance of the solar cell improved obviously, the conversion efficiency was increased 3.5 times and up to 0.34%. After mixing fullerene derivative PCBM with P3HT, due to the efficient separation of the electron-hole pair, the short circuit current density was improved 8 times and up to 9.98 mA cm-2, and the conversion efficiency was increased 6 times and up to 2.07%.
ZnO nanotube arrays and Cu@ZnO coaxial nanocables were fabricated in free-standing AAO template by electrodeposition and then annealing. During the PL test, a green emission band was excited from the Cu@ZnO coaxial nanocable array, indicating that the ZnO was doped by Cu at the interface of the coaxial heterojunction. ZnO free-standing arrays of nanorods and nanotubes on ITO glass were prepared using similar technique. The carrier density of the ZnO array was 2.67×1020 cm-3, indicating the great potential of application in transparent conducting oxides.
ZnO nanorod arrays were prepared by a simple one-step electrodeposition from aqueous solution. The 55℃deposition produced a dense ZnO film, while the 85℃deposition produced a nanorod array, indicating that the morphology of the deposited film depended on the temperature. The ITO/ZnO/P3HT:PCBM/Ag solar cell fabricated with the 85℃deposited ZnO array had a conformal morphology with the array. For the solar cell using the unannealed ZnO array, the direct contact between the polymer and the dominant defect region at the bottom would cause serious current leakage. By eliminating those defects through annealing, or preventing the direct contact using a denser array, the leakage could be avoided, in turn the open circuit voltage could be increased. The current was mainly generated by the P3HT:PCBM polymer blend. Thus, the effective way to increase the short circuit current density was to increase the density of ZnO rods so as to increase the load of the polymer blend and the interface between the ZnO rods and the polymer. The TiO_2 shell deposited on the ZnO by ALD decreased the rate of recombination between electrons and holes, in turn improved the conversion efficiency, which was up to 2.10% and was higher than all the ZnO array cells without TiO_2 shell.
在ITO玻璃表面磁控溅射Al层,然后阳极氧化可制得多孔阳极氧化铝(AAO)膜/ITO玻璃复合模板。为了避免阳极氧化过程中AAO膜的破裂和脱落,在溅射高纯Al前,添加了Ti和W层分别作为连接层和缓冲层。磁控溅射后,通过热处理消除了溅射层的内应力,改善了各溅射层之间的结合力。在阳极氧化过程中,当发展较快的孔洞到达Al层底部时,会氧化底部的W缓冲层,对孔洞的快速发展起到缓冲作用,从而延缓了AAO膜底部的破裂和脱层,使大面积纳米孔洞阵列得以生成。
采用溶胶-凝胶电泳法在AAO/ITO复合模板内填充TiO_2纳米棒与纳米管有序阵列,电泳法制备的TiO_2纳米结构随TiO_2溶胶陈化时间的延长,由纳米棒逐渐转变为纳米管结构。研究发现,在AAO模板孔洞底部的环状W电极是形成不同结构的前提,而溶胶溶液中带电粒子的扩散速度和纳米阵列的沉积速度的竞争则是形成不同结构的原因。将制备的TiO_2纳米阵列与p型聚合物聚3-己基噻酚(P3HT)结合,制成TiO_2纳米阵列/P3HT无机-有机杂化太阳能电池。纳米棒和纳米管太阳能电池的光电转换效率分别是0.38%和0.48%。相比文献中类似方法制备的TiO_2纳米晶结构杂化太阳能电池0.22%的转换效率,本文中制备的TiO_2纳米棒与纳米管阵列太阳能电池效率提高了约73%到118%的效率,显示了纳米有序阵列结构的巨大优势。
通过磁控溅射、热处理二步法在独立AAO模板上制备出TiO_2纳米阵列。AAO模板参数对TiO_2的纳米结构具有决定作用,200 nm的孔径导致纳米管结构的生成,80 nm孔径的双面开孔模板导致纳米棒结构的生成,而80 nm的单孔模板导致闭口纳米管的生成。XRD分析显示TiO_2纳米管阵列为多晶锐钛矿结构,光致发光(PL)谱分析发现制备的纳米管与纳米棒阵列都为间接带隙半导体,纳米棒中的氧空位缺陷多于纳米管结构。将TiO_2纳米管阵列层从AAO模板脱离,转移到ITO玻璃上,旋涂一层P3HT,组成TiO_2纳米管/P3HT杂化太阳能电池。研究发现,具有TiO_2结合层结构的TiO_2纳米管/P3HT杂化太阳能电池性能比无结合层的电池显著提高,光电转换效率提高了8倍,达到0.34%。而采用n型富勒烯衍生物PCBM与P3HT充分混合后,由于电子-空穴对的有效分离,短路电流密度提高了近5倍,达到9.98 mA cm-2;光电转换效率提高了近6倍,达到2.07%。
利用电沉积、热处理二步法在AAO模板中制备出了ZnO纳米管阵列和Cu@ZnO纳米同轴电缆阵列。在光致发光测试中,Cu@ZnO纳米同轴电缆被激发出绿光发射带,说明在Cu@ZnO纳米同轴电缆界面处的ZnO被Cu掺杂。还将独立AAO模板上的ZnO纳米阵列合成技术转移到AAO/ITO复合模板,在ITO玻璃上制备出ZnO纳米棒与纳米管有序阵列,ZnO有序阵列的载流子密度约为2.67×1020 cm-3,在透明导电氧化物领域具有很好的应用前景。
通过一步电沉积法在ITO导电玻璃上制得ZnO纳米棒阵列。在温度为55℃时,得到的是致密的ZnO膜,而在85℃时,得到的是ZnO纳米棒阵列,说明ZnO膜的形貌取决于沉积温度。用85℃电沉积得到的ZnO纳米棒阵列组装的ITO/ZnO/P3HT:PCBM/Ag太阳能电池具有与ZnO纳米棒阵列共型形貌。对于未退火ZnO纳米棒阵列制备的太阳能电池,暴露在ZnO底部的主导缺陷区与共混聚合物直接接触,导致了严重的电流泄露。而通过退火消除ZnO底部暴露在外的缺陷,以及通过沉积更致密的ZnO纳米棒来阻止共混聚合物与主导缺陷区的接触都可以有效避免电流的泄露,从而进一步提高电池的开路电压。由于P3HT与PCBM的混合极其密切,它们的接触面积非常大,P3HT:PCBM混合物生成的光电流在总电流中占主导地位。通过ALD法在ZnO纳米棒表面覆盖一层TiO_2有效减少了电子和空穴的复合几率,进而提高了光电转换效率,电池的转换效率达到2.10%,高于无壳层的ZnO纳米棒阵列组装的太阳能电池。
Ordered nanomaterial arrays, especially arrays of free-standing nanorods and nanotubes on conducting substrates have been applied in many different fields. When implemented in photovoltaics, these structures can increase the surface area between the charge-generating and charge-transporting layers, improving the efficiency of charge extraction. In this study, we choose TiO_2 and ZnO which are two of the most extensively studied wide band gap metallic oxide semiconductors. The nanorod and nanotube arrays of the two materials were prepared by different techniques. The applications of these arrays in nanodevices, especially in organic-inorganic hybrid solar cells were researched in detail.
Porous anodic aluminum oxide (AAO) membrane/ITO glass composite templates were prepared by anodizing the magnetron sputtered Al on the ITO glass. For avoiding the delaminating and cracking of the AAO at the bottom of the pores during anodization, Ti and W layers were sputtered before the magnetron sputtering of Al. Annealing was carried out to eliminate the inner stress of the sputtered layers, improving the connection between these layers. During anodization, the faster developing pores would oxidize the W barrier layer when it reached the bottom. The oxidation of the W slowed down the development of the pores, preventing the cracking of the AAO membrane and ensuring the completion of the whole array of the nanopores.
Arrays of TiO_2 nanorods and nanotubes were embedded in AAO/ITO template by sol-gel electrophoresis. The structure of the TiO_2 changed from nanorod to nanotube with the sol aging time. The W ring electrode was the precondition to the formation of different structures. The competition between the diffusion rate of the charged particles and the deposition rate caused the formation of different structures. The as-prepared TiO_2 arrays were fabricated in hybrid solar cells by spin coating P3HT in the arrays. The conversion efficiencies were up to 0.38% and 0.48% for the TiO_2 nanorod and nanotube solar cells. The efficiency of the nanotube array solar cell was improved by 26% compared to the nanorod cell due to the larger specific surface area.
TiO_2 arrays were also prepared in free-standing AAO template by magnetron sputtering and annealing. The parameters of the porous AAO template were highly influential in determining the nanostructure of the sputtered film. The template with a 200 nm pore diameter would result in the formation of nanotubes, while the double-sided through hole template with a 80 nm pore diameter would result in the formation of nanorods, and the one-sided blind hole template with a 80 nm pore diameter would result in the formation of closed-end tubes. The XRD measurement showed the annealed TiO_2 nanotubular film was polycrystalline anatase phase without preferred orientation. The photoluminescence (PL) spectrum revealed the as-prepared TiO_2 nanostructural film was an indirect bandgap semiconductor with oxygen vacancy defects that exist more in rods than in tubes. Then, the TiO_2 nanotubular film were removed from the AAO and transferred onto an ITO glass. A layer of P3HT was spin coated into the TiO_2 nanotube array to fabricate a hybrid solar cell. By adding a TiO_2 connecting layer between TiO_2 nanotubular film and ITO glass, the performance of the solar cell improved obviously, the conversion efficiency was increased 3.5 times and up to 0.34%. After mixing fullerene derivative PCBM with P3HT, due to the efficient separation of the electron-hole pair, the short circuit current density was improved 8 times and up to 9.98 mA cm-2, and the conversion efficiency was increased 6 times and up to 2.07%.
ZnO nanotube arrays and Cu@ZnO coaxial nanocables were fabricated in free-standing AAO template by electrodeposition and then annealing. During the PL test, a green emission band was excited from the Cu@ZnO coaxial nanocable array, indicating that the ZnO was doped by Cu at the interface of the coaxial heterojunction. ZnO free-standing arrays of nanorods and nanotubes on ITO glass were prepared using similar technique. The carrier density of the ZnO array was 2.67×1020 cm-3, indicating the great potential of application in transparent conducting oxides.
ZnO nanorod arrays were prepared by a simple one-step electrodeposition from aqueous solution. The 55℃deposition produced a dense ZnO film, while the 85℃deposition produced a nanorod array, indicating that the morphology of the deposited film depended on the temperature. The ITO/ZnO/P3HT:PCBM/Ag solar cell fabricated with the 85℃deposited ZnO array had a conformal morphology with the array. For the solar cell using the unannealed ZnO array, the direct contact between the polymer and the dominant defect region at the bottom would cause serious current leakage. By eliminating those defects through annealing, or preventing the direct contact using a denser array, the leakage could be avoided, in turn the open circuit voltage could be increased. The current was mainly generated by the P3HT:PCBM polymer blend. Thus, the effective way to increase the short circuit current density was to increase the density of ZnO rods so as to increase the load of the polymer blend and the interface between the ZnO rods and the polymer. The TiO_2 shell deposited on the ZnO by ALD decreased the rate of recombination between electrons and holes, in turn improved the conversion efficiency, which was up to 2.10% and was higher than all the ZnO array cells without TiO_2 shell.
引文
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