面向光催化和光伏器件的氧化锌纳米线制备与集成
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摘要
氧化锌(ZnO)是一种重要的Ⅱ-Ⅵ族直接带隙半导体材料,它具有较宽的带隙和较高的激子结合能。纳米结构的ZnO具有优异的电学、光学、气敏和光催化氧化等特性,在透明电极、发光二极管、太阳能电池、紫外探测器、压电器件、声表面波器件、气敏传感器、光催化降解等领域得到了广泛应用。尤其是ZnO纳米材料作为一种高效、无毒、价格低廉的光催化剂,在光催化降解有机污染物和矿化环境污染物等领域备受关注。同时,纳米结构的ZnO具有高的比表面积、高的电子迁移率、对可见光透明、纳米形貌丰富等特点,成为染料敏化太阳能电池领域的一个研究热点。目前,国内外研究人员在ZnO纳米材料的结构和特性等方面开展了大量的研究工作,但在器件化和实用化方面,仍存在许多的问题需要解决,比如工艺的集成性和重复性较低,工艺过程复杂且成本较高等。因此,研究ZnO纳米材料的制备方法,将其与微纳米加工技术相结合,开发具有实用价值的新型器件,探索微观结构与器件性能之间的内在联系,具有十分重要的意义。
本论文研究工作主要以一维ZnO纳米线为研究对象,将其与传统的微加工和微流体等技术相集成,重点研究其在光催化和光伏电池中的应用问题。围绕此内容,具体开展了以下几个方面的工作：
(1)通过采用溶胶-凝胶工艺与旋涂工艺相结合的方法在硅基底上制备了高质量的ZnO种子层,从而对水热法合成ZnO纳米线的工艺进行了改进。利用该方法制备的ZnO种子层是由粒度均匀的ZnO纳米颗粒构成,具有明显的纤锌矿结构和良好的c轴择优取向,而且对设备要求不高、工艺简单、重复性好,满足了大面积制备ZnO纳米线的需要；研究了生长液中的不同添加剂的含量以及生长时间对纳米线形貌的影响,结果表明,氨水和聚醚酰亚胺(PEI)对于获得高长径比的纳米线具有直接的影响,而随着生长时间的增加,ZnO纳米线快速且近乎呈线性的增长；通过将改进的水热法与光刻工艺相结合制备了长且垂直对准的ZnO纳米线阵列,并明显改善了纳米线的底部融合问题,从而有利于将ZnO纳米线集成到实用化器件之中。
(2)提出了一种面向光催化应用的新型微流体反应器。通过采用水热法与光刻工艺相结合的方法在玻璃基底上制备了大面积垂直对准的ZnO纳米线,然后利用软光刻技术制备了带有微流体沟道的PDMS壳体,将两者键合形成一个平面微流体反应器；ZnO纳米线作为固定型光催化剂,具有明显的纤锌矿结构以及良好的紫外吸收特性,同时也避免了催化剂从处理后的溶液中分离回收的难题；通过光催化降解亚甲基蓝的实验对微流体反应器的光催化性能进行了研究,结果表明,该反应器具有稳定而高效的光催化性能,通过对ZnO纳米线退火以及染料溶液冲洗等预处理均能有效地增强反应器的光催化能力；与其它对照实验相比,该平面微流体反应器也显示出了优异的光催化性能。可见,该反应器具有制备工艺简单,光催化效率高,适合于规模化生产等优点,因此,它具有非常广阔的应用前景。
(3)研究了钯掺杂对ZnO纳米纤维的光催化增强效应。以聚乙烯吡咯烷酮为纤维模板、醋酸锌/氯化钯为前驱体、一定体积比的乙醇/醋酸/水等为混合溶剂,利用静电纺丝技术制备了复合纳米纤维；通过在600℃下煅烧2小时得到了钯掺杂的ZnO纳米纤维,它们是具有超高长径比的纳米线：利用SEM、TEM、XRD和FTIR等技术对ZnO纳米纤维的结构和特性进行了表征,测试结果表明,煅烧后的纳米纤维呈纤锌矿结构,由几纳米到几十纳米的晶粒构成,由于钯掺杂量相对较小,其未对纳米纤维的形貌产生明显影响；通过光催化降解亚甲基蓝,实验研究了钯掺杂对ZnO纳米纤维的光催化性能的影响,结果表明,与纯ZnO纳米纤维相比,一定量的钯掺杂可以显著提高其光催化性能,并分析了可能的影响机制。
(4)研究了ZnO纳米线形貌和微流体电解质对光伏器件性能的影响。结合水热法和光刻工艺在FTO玻璃基底上制备了垂直对准的ZnO纳米线,对比研究了定时更换生长液对ZnO纳米线形貌的影响,结果表明,定时更换生长液对于提高纳米线的生长速率以及获得高长径比的纳米线非常重要：研究了纳米线长度对光伏器件性能的影响,测试结果表明,随着纳米线长度增加,光伏器件的性能不断提高,这主要归因于纳米线上染料吸附量的增加；首次将微流电解质的概念引入到光伏器件之中,并初步研究了不同的电解质流速对光伏器件性能的影响,测试结果表明,随着电解质流速的降低,光伏器件的短路电流逐渐降低,而开路电压缓慢增加,从而对光伏器件的能量转换效率产生一定程度的影响。
Zinc oxide (ZnO) is a remarkable Ⅱ-Ⅵ semiconductor material with a wide direct bandgap of3.37eV and a large exciton binding energy of60meV at room temperature. Nanostructured ZnO has received much attention over the past few years due to its distinguished performance in electronics, optics, gas sensing and photocatalytic oxidation, making it suitable for a wide range of applications such as solar cells, light emitting diodes, transparent electrodes, surface acoustic wave devices, ultraviolet photodetectors, gas sensors, photocatalytic degradation and so on. In particular, ZnO nanomaterial as an efficient photocatalyst has the advantages of low cost, non-toxicity, higher photocatalytic activity for the degradation of various kinds of organic pollutants in both acidic and basic medium than titanium oxide (TiO2). On the other hand, ZnO presents excellent bulk electron mobility, high surface-to-volume ratio, high transparency to visible light and the richest family of nanostructures. The unique combination of these properties opens, in principle, wide possibilities in terms of dye-sensitized solar cells (DSSCs) design. Although a great deal of research work has been conducted on the structures and properties of ZnO nanomaterials, there are still many issues for applying ZnO nanomaterials into practical devices, such as the low integratability, low reproducibility, complex procedure and high cost. Thus, it is of great importance to develop novel strategies such as integrating ZnO nanomaterials with other micro/nano fabrication techniques, in order to develop novel practical devices, and to explore the connections between the microscopic structures and the device performance.
In this thesis, we mainly focus on the fabrication and integration of one-dimensional (1-D) ZnO nanowire materials. A lot of effort has been devoted to combine the conventional microfabrication process and microfluidic technology with the improved hydrothermal method of synthesizing1-D ZnO nanowires, aiming to explore their potentials in photocatalytic and photovoltaic applications. The details of our work are as follows:
Firstly, the hydrothermal method of synthesizing ZnO nanowires had been improved by adopting a novel method for preparing ZnO seed layer on the substrate, which combined a sol-gel process and a spin-coating technique. The ZnO seed layer was composed of ZnO nanoparticles that were uniform in size and highly c-axis oriented. This approach could simplify the manufacturing process and improve the process reliability, so it was suitable for scale-up production of ZnO nanowires on different substrates. Furthermore, the effect of the growth duration and various contents of additives in the growth solution on the ZnO nanowire morphology had been investigated. The results indicated that the contents of ammonia and polyethyleneimine (PEI) in the growth solution played a key role in obtaining vertically aligned ZnO nanowires with high aspect ratio. The nanowire length increased fast even linearly with the increase of growth duration. Ultralong and well-aligned ZnO nanowire arrays were selectively grown on the substrate by combining the general photolithography with the improved hydrothermal method. Meantime, the bottom fusion at the foot of nanowires had been improved obviously. The results showed that the combination method was favorable to integrate the ZnO nanomaterials into practical devices.
Secondly, a novel microfluidic reactor with integrated ZnO nanowires as immobilized photocatalyst for the degradation of organic dyes had been developed. Large-area and well-aligned ZnO nanowires were grown on glass substrate through the combination of the improved hydrothermal method and photolithographic technique. The microfluidic reactor was prepared by bonding the ZnO nanowire-coated glass slide with a PDMS chip that was fabricated by soft lithography. As the immobilized catalyst, ZnO nanowires exhibited obvious wurtzite structure and excellent UV absorption performance. More importantly, it could avoid the troublesome process of recycling ultrafine catalyst from the disposed solution. The photocatalytic activity of the reactor was evaluated by the decomposition of methylene blue under UV irradiation. The results of cyclic photodegradation showed that our microfluidic device possessed good stability and high photocatalytic performance. In addition, the pretreatments such as flushing the device with dye solution and annealing the ZnO nanowires could enhance the photocatalytic activity of microfluidic reactor obviously. Compared to the control experiments, the microfluidic reactor with integrated ZnO nanowires also exhibited much better catalytic performance. Hence the microfluidic reactor we proposed was of great practical value due to its simple fabrication process and high photocatalytic efficiency.
Thirdly, the effect of doping of noble metal palladium (Pd) on the photocatalytic activity of1-D ZnO nanofibers had been investigated. The composited nanofibers were synthesized via an electrospinning technique, in which polyvinylpyrrolidone (PVP) was used as the fiber template, zinc acetate/palladium chloride as the precursors, and a mixture of ethanol/acid acetate/water at a ratio of8:5:2(v/v/v) as the co-solvent. Pd-doped ZnO nanofibers were obtained after calcinating the as-spun nanofibers at600℃in air for2h. The measurement results showed that the Pd doping had little effect on the morphology of ZnO nanofibers due to its very small amount. After calcination, the nanofibers exhibited wurtzite structure and they were composed of ultrafine ZnO nanocrystals. The effect of Pd doping on the photocatalytic activity of ZnO nanofibers had been evaluated by the degradation of methylene blue under UV irradiation. The results showed that a certain amount of Pd doping could enhance the photocatalytic efficiency of ZnO nanofibers obviously and the possible influencing mechanism had been discussed. Moreover, as a subset of ZnO nanowires, doped ZnO nanofibers could be collected easily from the disposed solution, so it had a great potential in photocatalytic applications.
Finally, the effects of ZnO nanowire morphology and microfluidic electrolyte on the photovoltaic performance of DSSCs had been investigated. The combination of the improved hydrothermal method and general photolithography was adopted to synthesize well-aligned ZnO nanowires on FTO glass substrate. The effect of refreshing growth solution on the growth of ZnO nanowires was investigated. The results showed that it was crucial to refreshing the growth solution for obtaining high growth rate and high aspect ratio of nanowires. Furthermore, the effect of nanowire length on the photovoltaic performance of solar cells had been examined. The results showed that the DSSC performance was improved dramatically with the increase of nanowire length, which was ascribed to the increase of dye loading on the nanowire surface. The conception of microfluidic electrolyte was successfully introduced into the DSSC devices for the first time and the effect of the flowing rates of microfluidic electrolyte had been examined preliminarily. The results showed that, with the decrease of flowing rates, the short-circuited current (JSC) decreased while the open-circuited voltage (VOC) increased, imposing a certain effect on the solar energy conversion efficiency. The possible influencing mechanism of the microfluidic electrolyte on the DSSC photovoltaic performance was also discussed.
本论文研究工作主要以一维ZnO纳米线为研究对象,将其与传统的微加工和微流体等技术相集成,重点研究其在光催化和光伏电池中的应用问题。围绕此内容,具体开展了以下几个方面的工作：
(1)通过采用溶胶-凝胶工艺与旋涂工艺相结合的方法在硅基底上制备了高质量的ZnO种子层,从而对水热法合成ZnO纳米线的工艺进行了改进。利用该方法制备的ZnO种子层是由粒度均匀的ZnO纳米颗粒构成,具有明显的纤锌矿结构和良好的c轴择优取向,而且对设备要求不高、工艺简单、重复性好,满足了大面积制备ZnO纳米线的需要；研究了生长液中的不同添加剂的含量以及生长时间对纳米线形貌的影响,结果表明,氨水和聚醚酰亚胺(PEI)对于获得高长径比的纳米线具有直接的影响,而随着生长时间的增加,ZnO纳米线快速且近乎呈线性的增长；通过将改进的水热法与光刻工艺相结合制备了长且垂直对准的ZnO纳米线阵列,并明显改善了纳米线的底部融合问题,从而有利于将ZnO纳米线集成到实用化器件之中。
(2)提出了一种面向光催化应用的新型微流体反应器。通过采用水热法与光刻工艺相结合的方法在玻璃基底上制备了大面积垂直对准的ZnO纳米线,然后利用软光刻技术制备了带有微流体沟道的PDMS壳体,将两者键合形成一个平面微流体反应器；ZnO纳米线作为固定型光催化剂,具有明显的纤锌矿结构以及良好的紫外吸收特性,同时也避免了催化剂从处理后的溶液中分离回收的难题；通过光催化降解亚甲基蓝的实验对微流体反应器的光催化性能进行了研究,结果表明,该反应器具有稳定而高效的光催化性能,通过对ZnO纳米线退火以及染料溶液冲洗等预处理均能有效地增强反应器的光催化能力；与其它对照实验相比,该平面微流体反应器也显示出了优异的光催化性能。可见,该反应器具有制备工艺简单,光催化效率高,适合于规模化生产等优点,因此,它具有非常广阔的应用前景。
(3)研究了钯掺杂对ZnO纳米纤维的光催化增强效应。以聚乙烯吡咯烷酮为纤维模板、醋酸锌/氯化钯为前驱体、一定体积比的乙醇/醋酸/水等为混合溶剂,利用静电纺丝技术制备了复合纳米纤维；通过在600℃下煅烧2小时得到了钯掺杂的ZnO纳米纤维,它们是具有超高长径比的纳米线：利用SEM、TEM、XRD和FTIR等技术对ZnO纳米纤维的结构和特性进行了表征,测试结果表明,煅烧后的纳米纤维呈纤锌矿结构,由几纳米到几十纳米的晶粒构成,由于钯掺杂量相对较小,其未对纳米纤维的形貌产生明显影响；通过光催化降解亚甲基蓝,实验研究了钯掺杂对ZnO纳米纤维的光催化性能的影响,结果表明,与纯ZnO纳米纤维相比,一定量的钯掺杂可以显著提高其光催化性能,并分析了可能的影响机制。
(4)研究了ZnO纳米线形貌和微流体电解质对光伏器件性能的影响。结合水热法和光刻工艺在FTO玻璃基底上制备了垂直对准的ZnO纳米线,对比研究了定时更换生长液对ZnO纳米线形貌的影响,结果表明,定时更换生长液对于提高纳米线的生长速率以及获得高长径比的纳米线非常重要：研究了纳米线长度对光伏器件性能的影响,测试结果表明,随着纳米线长度增加,光伏器件的性能不断提高,这主要归因于纳米线上染料吸附量的增加；首次将微流电解质的概念引入到光伏器件之中,并初步研究了不同的电解质流速对光伏器件性能的影响,测试结果表明,随着电解质流速的降低,光伏器件的短路电流逐渐降低,而开路电压缓慢增加,从而对光伏器件的能量转换效率产生一定程度的影响。
Zinc oxide (ZnO) is a remarkable Ⅱ-Ⅵ semiconductor material with a wide direct bandgap of3.37eV and a large exciton binding energy of60meV at room temperature. Nanostructured ZnO has received much attention over the past few years due to its distinguished performance in electronics, optics, gas sensing and photocatalytic oxidation, making it suitable for a wide range of applications such as solar cells, light emitting diodes, transparent electrodes, surface acoustic wave devices, ultraviolet photodetectors, gas sensors, photocatalytic degradation and so on. In particular, ZnO nanomaterial as an efficient photocatalyst has the advantages of low cost, non-toxicity, higher photocatalytic activity for the degradation of various kinds of organic pollutants in both acidic and basic medium than titanium oxide (TiO2). On the other hand, ZnO presents excellent bulk electron mobility, high surface-to-volume ratio, high transparency to visible light and the richest family of nanostructures. The unique combination of these properties opens, in principle, wide possibilities in terms of dye-sensitized solar cells (DSSCs) design. Although a great deal of research work has been conducted on the structures and properties of ZnO nanomaterials, there are still many issues for applying ZnO nanomaterials into practical devices, such as the low integratability, low reproducibility, complex procedure and high cost. Thus, it is of great importance to develop novel strategies such as integrating ZnO nanomaterials with other micro/nano fabrication techniques, in order to develop novel practical devices, and to explore the connections between the microscopic structures and the device performance.
In this thesis, we mainly focus on the fabrication and integration of one-dimensional (1-D) ZnO nanowire materials. A lot of effort has been devoted to combine the conventional microfabrication process and microfluidic technology with the improved hydrothermal method of synthesizing1-D ZnO nanowires, aiming to explore their potentials in photocatalytic and photovoltaic applications. The details of our work are as follows:
Firstly, the hydrothermal method of synthesizing ZnO nanowires had been improved by adopting a novel method for preparing ZnO seed layer on the substrate, which combined a sol-gel process and a spin-coating technique. The ZnO seed layer was composed of ZnO nanoparticles that were uniform in size and highly c-axis oriented. This approach could simplify the manufacturing process and improve the process reliability, so it was suitable for scale-up production of ZnO nanowires on different substrates. Furthermore, the effect of the growth duration and various contents of additives in the growth solution on the ZnO nanowire morphology had been investigated. The results indicated that the contents of ammonia and polyethyleneimine (PEI) in the growth solution played a key role in obtaining vertically aligned ZnO nanowires with high aspect ratio. The nanowire length increased fast even linearly with the increase of growth duration. Ultralong and well-aligned ZnO nanowire arrays were selectively grown on the substrate by combining the general photolithography with the improved hydrothermal method. Meantime, the bottom fusion at the foot of nanowires had been improved obviously. The results showed that the combination method was favorable to integrate the ZnO nanomaterials into practical devices.
Secondly, a novel microfluidic reactor with integrated ZnO nanowires as immobilized photocatalyst for the degradation of organic dyes had been developed. Large-area and well-aligned ZnO nanowires were grown on glass substrate through the combination of the improved hydrothermal method and photolithographic technique. The microfluidic reactor was prepared by bonding the ZnO nanowire-coated glass slide with a PDMS chip that was fabricated by soft lithography. As the immobilized catalyst, ZnO nanowires exhibited obvious wurtzite structure and excellent UV absorption performance. More importantly, it could avoid the troublesome process of recycling ultrafine catalyst from the disposed solution. The photocatalytic activity of the reactor was evaluated by the decomposition of methylene blue under UV irradiation. The results of cyclic photodegradation showed that our microfluidic device possessed good stability and high photocatalytic performance. In addition, the pretreatments such as flushing the device with dye solution and annealing the ZnO nanowires could enhance the photocatalytic activity of microfluidic reactor obviously. Compared to the control experiments, the microfluidic reactor with integrated ZnO nanowires also exhibited much better catalytic performance. Hence the microfluidic reactor we proposed was of great practical value due to its simple fabrication process and high photocatalytic efficiency.
Thirdly, the effect of doping of noble metal palladium (Pd) on the photocatalytic activity of1-D ZnO nanofibers had been investigated. The composited nanofibers were synthesized via an electrospinning technique, in which polyvinylpyrrolidone (PVP) was used as the fiber template, zinc acetate/palladium chloride as the precursors, and a mixture of ethanol/acid acetate/water at a ratio of8:5:2(v/v/v) as the co-solvent. Pd-doped ZnO nanofibers were obtained after calcinating the as-spun nanofibers at600℃in air for2h. The measurement results showed that the Pd doping had little effect on the morphology of ZnO nanofibers due to its very small amount. After calcination, the nanofibers exhibited wurtzite structure and they were composed of ultrafine ZnO nanocrystals. The effect of Pd doping on the photocatalytic activity of ZnO nanofibers had been evaluated by the degradation of methylene blue under UV irradiation. The results showed that a certain amount of Pd doping could enhance the photocatalytic efficiency of ZnO nanofibers obviously and the possible influencing mechanism had been discussed. Moreover, as a subset of ZnO nanowires, doped ZnO nanofibers could be collected easily from the disposed solution, so it had a great potential in photocatalytic applications.
Finally, the effects of ZnO nanowire morphology and microfluidic electrolyte on the photovoltaic performance of DSSCs had been investigated. The combination of the improved hydrothermal method and general photolithography was adopted to synthesize well-aligned ZnO nanowires on FTO glass substrate. The effect of refreshing growth solution on the growth of ZnO nanowires was investigated. The results showed that it was crucial to refreshing the growth solution for obtaining high growth rate and high aspect ratio of nanowires. Furthermore, the effect of nanowire length on the photovoltaic performance of solar cells had been examined. The results showed that the DSSC performance was improved dramatically with the increase of nanowire length, which was ascribed to the increase of dye loading on the nanowire surface. The conception of microfluidic electrolyte was successfully introduced into the DSSC devices for the first time and the effect of the flowing rates of microfluidic electrolyte had been examined preliminarily. The results showed that, with the decrease of flowing rates, the short-circuited current (JSC) decreased while the open-circuited voltage (VOC) increased, imposing a certain effect on the solar energy conversion efficiency. The possible influencing mechanism of the microfluidic electrolyte on the DSSC photovoltaic performance was also discussed.
引文
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