碳纳米管负载半导体纳米晶的光催化聚合与光电转换器件的制备研究
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摘要
由于能源短缺以及可持续发展的要求,将太阳能转化为电能即光电转换器件的研究是目前世界关注的热点。对于光电转换器件的普及应用来说,降低成本以及性能提高是人类面临必须解决的两大问题。为了降低成本,目前功能聚合物/半导体复合材料结构的光伏器件逐渐成为发展的重要方向之一。目前这类复合材料的制备方法比较单一,多主要采用功能聚合物与无机半导体纳米粒子的共混体系,一般会造成纳米粒子的团聚;另外在制备过程中,由于纳米半导体与聚合物之间只是物理接触,复合材料的界面性质得不到改善,光生电子和空穴不能有效进行分离,因此这类光伏器件的性能普遍还不高。
对于光电转换器件来说,提高其性能的根本途径主要有:
1)增大聚合物/无机半导体的界面接触面积,优化复合物界面性质,使得器件中材料的光生电子和空穴能有效分离,可降低复合的几率;
2)采用高载流子迁移率的材料来提高器件中电子和空穴的迁移,从而形成稳定的光电流。
光催化聚合是一种新型的聚合方法,是由半导体纳米粒子在光激发的条件下直接引发合成聚合物,原位合成纳米复合材料。由于纳米粒子直接参与了聚合反应,这样纳米粒子和聚合物之间可能存在较强的相互作用,纳米粒子与聚合物的界面性质得到改善,因此这提供了一种制备纳米复合材料的新方法,具有光明的应用前景。
在本文的研究工作里,选用高载流子迁移率的纳米ZnO半导体作为电子受体,首先将其负载在碳纳米管(CNT)上,然后进行半导体纳米粒子的光催化聚合,制备了新型的碳纳米管-无机半导体纳米粒子-功能聚合物三元纳米复合光电转换材料。本课题主要研究内容和结果如下:
1、采用溶胶-凝胶(Sol-Gel)法制备碳纳米管负载的ZnO纳米粒子。XRD结果表明,ZnO粒子为六角晶系纤锌矿晶型。TEM结果表明纳米粒子沿着CNT管壁生长,形成均匀的纳米粒子层,且粒子尺寸均一,实现了碳纳米管上纳米半导体粒子的高负载量。Raman光谱的研究表明ZnO与CNT间有很强的相互作用,引起了拉曼特征峰的蓝移以及峰强度的显著变化。
2、在紫外辐射条件下,实现了碳纳米管负载的纳米ZnO粒子引发N-乙烯基咔唑单体聚合,首次实现了纳米ZnO-碳纳米管-PVK三元结构纳米复合光电转换材料的制备,未见文献报道。CNT的引入使得复合材料的紫外可见吸收边界发生红移,说明其能够更好地利用太阳能。
3、通过稳态和瞬态荧光分析,证实ZnO与PVK的界面以及ZnO-CNT的界面处发生了光诱导的电荷转移过程。结合XPS与ESR的结果表明,在复合材料中,PVK的光生电子首先向ZnO转移,致使PVK咔唑环被氧化,ZnO粒子被还原,然后ZnO上的电子又进一步向CNT发生转移,从而实现光生空穴和电子分离效率的提高。
4、碳纳米管作为良好的电子传输材料可以在复合材料中形成交联网络,使得通过光诱导电荷转移作用转移到CNT上的电子能够高效地进行传导,减少光生电荷的复合,形成稳定的光电流。实验发现:复合物中引入碳纳米管后,光伏器件的光电转换性能获得了大幅度的提高。瞬态光电流最高可提高为原来的7倍,IPCE%(入射单色光子-电子转化效率)高达30%,开路电压(V_(oc))、短路电流(I_(sc))以及填充因子(FF)都有较大的提高。
5、半导体光催化聚合所制备的ZnO-PVK纳米复合材料的光电转换性能好于简单共混的复合材料。光催化聚合的复合物中ZnO与PVK的界面性质得到改善,可促进光致电荷转移的发生,使材料光电转换性能得以提升。
6、最后本文提出了光伏器件中电荷转移过程的整个机理与模型,为制备高性能的光电转换器件奠定了理论基础。
Along with the worldwide energy shortage problem and the strong demand of sustainable development, higher attention has been paid to the photovoltaic device which can convert the solar energy into electrical energy. To reduce the cost and achieve the large scale commercial effect, the research on inorganic nano semiconductor - conjugated polymer photovoltaic composite materials is on the forefront of photoelectric materials in the current world. At present, such materials are mainly prepared by simple mixing the semiconductor nanoparticles and the polymer which may cause the aggregation of the nanoparticles and the low energy conversion efficiency. Up to now the photovoltaic device based on semiconductor nanoparticle/conjugated polymer is still in the research process and waits for the new breakthrough of the energy conversion efficiency. The main ways to enhance the efficiency of photovoltaic device are as follows:
1) to optimize the interface of semiconductor nanoparticle and conjugated polymer and make the high dispersity of the nanocomposites which can enhance the efficiency of the separation of photo-induced charges and reduce the combination possibilities of the charges;
2) to use the material which has high carrier mobility which could help better transportation of carriers and lead to the higher photo current.
The photo-polymerization induced by nanosemiconductor is a new method to prepare inorganic-polymer nanocomposites. The nanoparticles take the role of initiators, the nature of interface is optimized, which enhances the photovoltaic property of the nanocomposites.
In this study, a novel photovoltaic inorganic-polymer nanocomposite was prepared via the photo-polymerization induced by semiconductor nanoparticles. Firstly the carbon nanotubes were loaded with a layer of ZnO nanoparticles. Then the hybrid was used as initiators to induce the polymerization of N-vinyl carbazole under the UV light and the CNT-ZnO-PVK ternary assemblies were prepared as one novel photovoltaic nanocomposites. The main research contents and the results are as follows:
1. ZnO nanoparticles with a homogeneous size loaded on carbon nanotubes was prepared through sol-gel method. The XRD results indicated that the ZnO nanoparticles were the hexagonal wurtzite crystallites. TEM results showed that the nanoparticles were grown along the CNT. The strong interaction was improved by the Raman spectra change of frequency and peak relative height.
2. It's the first time to photopolymerize the N-vinyl carbazole initiated by the ZnO nanoparticles loaded on carbon nanotubes, and also the first time to prepare the CNT-ZnO-PVK photovoltaic nanocomposites. UV-vis results showed that the nanocomposites' absorbance of solar light was broadened with the introduction of CNT.
3. Through the steady-state and transient fluorescence analysis, a charge transfer process at the interface between ZnO and PVK and also between ZnO and CNT was found. Combined with the results of XPS and ESR, the charge transfer mechanism was indicated as follows: the photo-generated electron was firstly transferred to ZnO nanoparticles from the polymer and then it was further transported to the CNT. The process could enhance the separation efficiency of photo-generated electron and hole.
4. The photovoltaic property of the device was largely enhanced with the introduction of CNT which could form a network in the nanocomposites and help the transportation of electron. The transient photo-current was 7 times as the one which had no CNT. The IPCE% efficiency was improved to 30% and the V_(oc)、I_(sc)、and FF values were largely increased.
5. The nanocomposites prepared through photopolymerization presented the better photovoltaic property, compared with the composites obtained from general radical polymerization. This is because the interface between ZnO and PVK is optimized, which promotes the charge transfer and improves the separation efficiency of the hole- electronic pair.
6. The model was proposed to illustrate the charge transfer mechanism of the photovoltaic device, which provided the theory basis for the enhancement of the photovoltaic property.
对于光电转换器件来说,提高其性能的根本途径主要有:
1)增大聚合物/无机半导体的界面接触面积,优化复合物界面性质,使得器件中材料的光生电子和空穴能有效分离,可降低复合的几率;
2)采用高载流子迁移率的材料来提高器件中电子和空穴的迁移,从而形成稳定的光电流。
光催化聚合是一种新型的聚合方法,是由半导体纳米粒子在光激发的条件下直接引发合成聚合物,原位合成纳米复合材料。由于纳米粒子直接参与了聚合反应,这样纳米粒子和聚合物之间可能存在较强的相互作用,纳米粒子与聚合物的界面性质得到改善,因此这提供了一种制备纳米复合材料的新方法,具有光明的应用前景。
在本文的研究工作里,选用高载流子迁移率的纳米ZnO半导体作为电子受体,首先将其负载在碳纳米管(CNT)上,然后进行半导体纳米粒子的光催化聚合,制备了新型的碳纳米管-无机半导体纳米粒子-功能聚合物三元纳米复合光电转换材料。本课题主要研究内容和结果如下:
1、采用溶胶-凝胶(Sol-Gel)法制备碳纳米管负载的ZnO纳米粒子。XRD结果表明,ZnO粒子为六角晶系纤锌矿晶型。TEM结果表明纳米粒子沿着CNT管壁生长,形成均匀的纳米粒子层,且粒子尺寸均一,实现了碳纳米管上纳米半导体粒子的高负载量。Raman光谱的研究表明ZnO与CNT间有很强的相互作用,引起了拉曼特征峰的蓝移以及峰强度的显著变化。
2、在紫外辐射条件下,实现了碳纳米管负载的纳米ZnO粒子引发N-乙烯基咔唑单体聚合,首次实现了纳米ZnO-碳纳米管-PVK三元结构纳米复合光电转换材料的制备,未见文献报道。CNT的引入使得复合材料的紫外可见吸收边界发生红移,说明其能够更好地利用太阳能。
3、通过稳态和瞬态荧光分析,证实ZnO与PVK的界面以及ZnO-CNT的界面处发生了光诱导的电荷转移过程。结合XPS与ESR的结果表明,在复合材料中,PVK的光生电子首先向ZnO转移,致使PVK咔唑环被氧化,ZnO粒子被还原,然后ZnO上的电子又进一步向CNT发生转移,从而实现光生空穴和电子分离效率的提高。
4、碳纳米管作为良好的电子传输材料可以在复合材料中形成交联网络,使得通过光诱导电荷转移作用转移到CNT上的电子能够高效地进行传导,减少光生电荷的复合,形成稳定的光电流。实验发现:复合物中引入碳纳米管后,光伏器件的光电转换性能获得了大幅度的提高。瞬态光电流最高可提高为原来的7倍,IPCE%(入射单色光子-电子转化效率)高达30%,开路电压(V_(oc))、短路电流(I_(sc))以及填充因子(FF)都有较大的提高。
5、半导体光催化聚合所制备的ZnO-PVK纳米复合材料的光电转换性能好于简单共混的复合材料。光催化聚合的复合物中ZnO与PVK的界面性质得到改善,可促进光致电荷转移的发生,使材料光电转换性能得以提升。
6、最后本文提出了光伏器件中电荷转移过程的整个机理与模型,为制备高性能的光电转换器件奠定了理论基础。
Along with the worldwide energy shortage problem and the strong demand of sustainable development, higher attention has been paid to the photovoltaic device which can convert the solar energy into electrical energy. To reduce the cost and achieve the large scale commercial effect, the research on inorganic nano semiconductor - conjugated polymer photovoltaic composite materials is on the forefront of photoelectric materials in the current world. At present, such materials are mainly prepared by simple mixing the semiconductor nanoparticles and the polymer which may cause the aggregation of the nanoparticles and the low energy conversion efficiency. Up to now the photovoltaic device based on semiconductor nanoparticle/conjugated polymer is still in the research process and waits for the new breakthrough of the energy conversion efficiency. The main ways to enhance the efficiency of photovoltaic device are as follows:
1) to optimize the interface of semiconductor nanoparticle and conjugated polymer and make the high dispersity of the nanocomposites which can enhance the efficiency of the separation of photo-induced charges and reduce the combination possibilities of the charges;
2) to use the material which has high carrier mobility which could help better transportation of carriers and lead to the higher photo current.
The photo-polymerization induced by nanosemiconductor is a new method to prepare inorganic-polymer nanocomposites. The nanoparticles take the role of initiators, the nature of interface is optimized, which enhances the photovoltaic property of the nanocomposites.
In this study, a novel photovoltaic inorganic-polymer nanocomposite was prepared via the photo-polymerization induced by semiconductor nanoparticles. Firstly the carbon nanotubes were loaded with a layer of ZnO nanoparticles. Then the hybrid was used as initiators to induce the polymerization of N-vinyl carbazole under the UV light and the CNT-ZnO-PVK ternary assemblies were prepared as one novel photovoltaic nanocomposites. The main research contents and the results are as follows:
1. ZnO nanoparticles with a homogeneous size loaded on carbon nanotubes was prepared through sol-gel method. The XRD results indicated that the ZnO nanoparticles were the hexagonal wurtzite crystallites. TEM results showed that the nanoparticles were grown along the CNT. The strong interaction was improved by the Raman spectra change of frequency and peak relative height.
2. It's the first time to photopolymerize the N-vinyl carbazole initiated by the ZnO nanoparticles loaded on carbon nanotubes, and also the first time to prepare the CNT-ZnO-PVK photovoltaic nanocomposites. UV-vis results showed that the nanocomposites' absorbance of solar light was broadened with the introduction of CNT.
3. Through the steady-state and transient fluorescence analysis, a charge transfer process at the interface between ZnO and PVK and also between ZnO and CNT was found. Combined with the results of XPS and ESR, the charge transfer mechanism was indicated as follows: the photo-generated electron was firstly transferred to ZnO nanoparticles from the polymer and then it was further transported to the CNT. The process could enhance the separation efficiency of photo-generated electron and hole.
4. The photovoltaic property of the device was largely enhanced with the introduction of CNT which could form a network in the nanocomposites and help the transportation of electron. The transient photo-current was 7 times as the one which had no CNT. The IPCE% efficiency was improved to 30% and the V_(oc)、I_(sc)、and FF values were largely increased.
5. The nanocomposites prepared through photopolymerization presented the better photovoltaic property, compared with the composites obtained from general radical polymerization. This is because the interface between ZnO and PVK is optimized, which promotes the charge transfer and improves the separation efficiency of the hole- electronic pair.
6. The model was proposed to illustrate the charge transfer mechanism of the photovoltaic device, which provided the theory basis for the enhancement of the photovoltaic property.
引文
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