CuPc/TiO_2纳米有序复合材料的制备与光电性能研究
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摘要
通过控制纳米材料的形貌和结构对材料的性能进行调控已经成为光电功能材料及器件当前研究的一个新的热点。对光电复合材料的结构与性能之间的关系和物理机制进行深入研究将有助于对其工作原理的进一步理解、新现象的发现和新概念的提出。光电功能材料中的光致电荷转移可显著提高载流子的解离和传输效率，是优化光电器件性能的有效途径。通过有机和无机半导体材料的纳米有序复合以及微观形貌的调控，形成拥有大面积接触界面、分子级别的紧密接触且有序定向排布的有机／无机电子给体-受体纳米有序复合体系可显著提高复合材料的光致电荷转移效率。本论文以电化学阳极氧化法和溶胶凝胶法结合真空蒸镀及电泳沉积法制备了CuPc／TiO_2纳米有序复合材料，并研究了其光电性能。
本文首先综述了有机／无机纳米复合材料在光电导、光伏、传感器等各个领域的研究进展，并介绍了几种典型的有机、无机半导体材料在光电领域的应用，以及本文所采用的用于制备纳米复合材料的各种方法的研究进展。
通过电化学阳极氧化法在Ti片上获得了尺寸可控且高度有序的TiO_2纳米管阵列，不同晶型的TiO_2纳米管阵列可以通过控制热处理温度得到。利用真空蒸镀法将CuPc填入TiO_2纳米管管内，通过调节CuPc的蒸镀速度以及厚度，可以获得不同形貌的CuPc／TiO_2纳米有序复合材料。并以此为光活化层制备了结构为Au／PEDOT：PSS／CuPc／TiO_2／Ti的光电器件，通过I-V特性曲线研究了其光电性能。在CuPc的蒸镀厚度为100 nm，TiO_2纳米管管径为70 nm的条件下，纳米有序复合材料的光电流较暗电流高出2-3个数量级，且有序材料的光电性能明显优于基于TiO_2无序纳米颗粒制备的复合材料。I-V测试结果表明，有序复合材料中的纳米结构为激子离解为自由载流子提供了较大的分离界面，而TiO_2纳米管阵列垂直于基底生长的特点促使光生载流子沿着纳米管的纵轴向Ti电极定向传输，使得载流子传输和收集效率大大增加，进而促使光电流大幅上升。光电器件在亮态／暗态之间转换时电流出现“滞后”现象是由于材料内部缺陷对多数载流子的捕获和释放过程有效地延缓了载流子的收集和淬灭所造成的。
根据酞菁类物质在酸性溶液中易被质子化，质子化后的分子在外加电场作用下可定向迁移的特点，利用电泳沉积的方法在TiO_2纳米管阵列表面电泳沉积CuPc制备了CuPc／TiO_2纳米复合薄膜。通过改变沉积条件对CuPc薄膜的微观形貌和聚集态结构进行了调控。利用UV-vis吸收光谱和XRD等手段研究了CuPc薄膜的聚集态结构，薄膜中CuPc分子聚集体类型的转变是造成其Q带吸收峰发生移动的根源。不断沉积的CuPc分子的堆积方式主要受到下层分子性质的影响，并借助等离子体基元耦合模型和激子理论对其聚集态结构的演变进行了分析。而CuPc溶液和薄膜的电致变色现象也正是源于H聚体与J聚体之间的转变。以CuPc／TiO_2纳米复合薄膜为光活化层制备了双层感光体，通过改变CuPc薄膜形貌可以对感光体的光电性能进行调控，光电导测试结果表明，只有厚度适当的CuPc薄膜才能充分利用入射的光能，在产生足够多的激子的同时，保证产生的激子可以迁移到CuPc／TiO_2界面处解离形成自由载流子，从而大大提高复合薄膜的光电导性能。
以高度有序的AAO为模板，使用溶胶．凝胶法和电泳沉积法分别制备了TiO_2和CuPc纳米线阵列，并结合两种方法通过二次沉积技术，将CuPc沉积在TiO_2纳米线和AAO模板孔壁之间的空隙处，得到了CuPc包覆的TiO_2纳米有序复合阵列。借助于瞬态荧光光谱证实了在复合纳米线中CuPc和TiO_2两者之间存在着光致电荷转移作用，通过改变EPD条件控制复合纳米线的形貌，可以调控复合纳米线的光电导性能。复合纳米线的光电导性能较单组分纳米线高出1-2个数量级。复合结构中酞菁铜包覆层与氧化钛纳米线之间较大的界面接触面积以及分离后的载流子定向连续传输通道是复合纳米线光电导性能提高的主要原因。
Tailoring the performance of materials via changing the morphologies and structures of materials has emerged as a new and important activity in optoelectronic functional materials and devices. The investigation of the relationship between structure and performance of optoelectronic composites would help to apprehend the optoelectronic mechanism, discover novel phenomenon, and raise new ideas. Photo-induced charge transfer in optoelectronic materials can be enhanced in one dimensional ordered nanocomposites and thus greatly improve the separation and transportation of charge carriers which are the key factors influencing optoelectronic device performance. The efficiency of photo-induced charge transfer in organic/inorganic nanocomposites can be effectively improved due to the effective contact in molecular level, larger contact area, and ordered directional donor/accepter nanocomposites construction which can be achieved through the ordered composite of organic and inorganic semiconductors and controlling the morphology of organic/inorganic ordered nanocomposites. In this dissertation, several approaches, anodic oxidation, sol-gel, vacuum thermal evaporation, and electrophoretic deposition, were carried out to fabricate high photosensitive CuPc/TiO_2 ordered nanocomposites. The optoelectronic property of the nanocomposites was investigated in details as well.
The recent progress on the application of organic/inorganic nanocomposites in the area of photoconductivity, photovoltaic characteristic, sensors, etc. was reviewed firstly. A detailed description was covered on optoelectronic field based on copper phthalocyanine (CuPc), phthalocyanine dyes and titania, including the preparation methods of nanocomposites used in this dissertation.
Size-controllable and high ordered vertically-oriented TiO_2 nanotube arrays were fabricated using anodic oxidation of pure titanium sheets in electrolyte solutions, and the crystallization of TiO_2 nanotubes could be tuned by altering annealing temperature. CuPc was filled into TiO_2 nanotubes by vacuum deposition at various deposition rates, a series of CuPc/TiO_2 ordered nanocomposites with various morphologies were achieved by tailoring the thickness of CuPc and the diameter of the TiO_2 nanotubes. A double-layered photoconductive device (Au/CuPc/TiO_2 nanotubes/titanium) was designed and fabricated with the CuPc/TiO_2 nanocomposites as photoactive layer. The photoconductive property of devices was studied via current-voltage(I-V) curves, and the current value increased by 2 or 3 orders of magnitude when exposed to light from dark, depending on the thickness of CuPc layer (100 nm for the best) and the diameter of TiO_2 nanotubes (70 nm for the best). For a control experiment, the I_l/I_d ratio of the device with disordered TiO_2 nanoparticles (TNPs) is obviously lower than that with ordered nanotube arrays. Several factors contribute to the improvement of photoconductive property of devices: the nanoarrays of TiO_2 nanotubes can enormously increase the contact area between CuPc and TiO_2, which offers much more sites for the exciton dissociation, and the one-dimensional and well-ordered structure of TiO_2 nanotube arrays can act as efficient transport channels. With the help of the aligned TiO_2 nanotubes, the collection and transfer efficiency of electrons is greatly enhanced, leading to an evident increase of photocurrent. The capturing and releasing majority carriers by traps or recombination centers at the donor/acceptor interface could effectively delay the process of collection or annihilation of charged carriers, which results in the hysteretic phenomenon of current change as device switches from light to dark and the reverse.
Phthalocyanine, a p-type organic semiconductor, contains bridging nitrogen atoms and can be easily protonated in organic acid solution. The protonated phthalocyanine molecules can orientationally migrate and nucleate on the negative electrode under external electric field. Basing on these considerations, CuPc/TiO_2 nanocomposites were fabricated by the electrophoretic deposition method (EPD) from the mixed solution of chloroform and trifluoroacetic acid containing the protonated CuPc. The morphology of the CuPc nanofilms can be manipulated by deposition time, concentration of CuPc, and applied voltage. The aggregation structure of the CuPc nanofilms was investigated by UV-vis spectroscopy and X-ray diffraction (XRD). The shift of Q-band absorption of CuPc nanofilms was resulted from the transition of aggregated structure of CuPc molecules. The XRD patterns demonstrated that the stack style of the deposited CuPc molecules is influenced by the property of the underlayer molecules. The evolvement of CuPc molecular aggregated structure was investigated by molecular exciton model and plasmon coupling, and the electrochromatic property of CuPc nanofilms and solution is derived from the transition of H- and J-aggregates. A dual-layered photoreceptors containing CuPc/TiO_2 nanocomposites as the charge generation layer (CGL) were designed and fabricated. The photoconductive property of photoreceptors was tailored via changing the morphology of the CuPc nanofilms. It was found that, to guarantee the adequate utilization of light energy, the thickness of the CuPc layer must be appropriate to efficiently absorb incident photons as well as to favor the migration of the excitons, which improved the photoconductivities of photoreceptors greatly.
Using highly-ordered porous anodic aluminum oxide (AAO) with nanopores perpendicular to the conductive substrate as the template, highly-ordered and well-aligned TiO_2 and CuPc nanowire arrays were prepared by assembly of TiO_2 precursors and CuPc in the AAO templates via sol-gel and EPD method, respectively. Coupling these two methods, a series of CuPc-coated TiO_2 ordered nanowire arrays were achieved via this secondary deposition technique. The photoluminescence spectra and the time-resolved fluorescence spectra of CuPc/TiO_2 nanowires confirmed the photoinduced charge transfer occurs between CuPc and TiO_2 nanowires, which contributes to the photoconductivity enhancement of CuPc/TiO_2 nanowires compared to pure CuPc or TiO_2 nanowires. The photoconductivity of the CuPc/TiO_2 nanowires can be tailored by changing the morphologies of CuPc/TiO_2 nanowires. It was found that the CuPc/TiO_2 nanowires arrays exhibited one or two orders of magnitude higher photoconductivity than that of pristine TiO_2 or CuPc nanowire arrays due to the large donor-acceptor (CuPc-TiO_2) contact area and the directional alignment of TiO_2 nanowires.
本文首先综述了有机／无机纳米复合材料在光电导、光伏、传感器等各个领域的研究进展，并介绍了几种典型的有机、无机半导体材料在光电领域的应用，以及本文所采用的用于制备纳米复合材料的各种方法的研究进展。
通过电化学阳极氧化法在Ti片上获得了尺寸可控且高度有序的TiO_2纳米管阵列，不同晶型的TiO_2纳米管阵列可以通过控制热处理温度得到。利用真空蒸镀法将CuPc填入TiO_2纳米管管内，通过调节CuPc的蒸镀速度以及厚度，可以获得不同形貌的CuPc／TiO_2纳米有序复合材料。并以此为光活化层制备了结构为Au／PEDOT：PSS／CuPc／TiO_2／Ti的光电器件，通过I-V特性曲线研究了其光电性能。在CuPc的蒸镀厚度为100 nm，TiO_2纳米管管径为70 nm的条件下，纳米有序复合材料的光电流较暗电流高出2-3个数量级，且有序材料的光电性能明显优于基于TiO_2无序纳米颗粒制备的复合材料。I-V测试结果表明，有序复合材料中的纳米结构为激子离解为自由载流子提供了较大的分离界面，而TiO_2纳米管阵列垂直于基底生长的特点促使光生载流子沿着纳米管的纵轴向Ti电极定向传输，使得载流子传输和收集效率大大增加，进而促使光电流大幅上升。光电器件在亮态／暗态之间转换时电流出现“滞后”现象是由于材料内部缺陷对多数载流子的捕获和释放过程有效地延缓了载流子的收集和淬灭所造成的。
根据酞菁类物质在酸性溶液中易被质子化，质子化后的分子在外加电场作用下可定向迁移的特点，利用电泳沉积的方法在TiO_2纳米管阵列表面电泳沉积CuPc制备了CuPc／TiO_2纳米复合薄膜。通过改变沉积条件对CuPc薄膜的微观形貌和聚集态结构进行了调控。利用UV-vis吸收光谱和XRD等手段研究了CuPc薄膜的聚集态结构，薄膜中CuPc分子聚集体类型的转变是造成其Q带吸收峰发生移动的根源。不断沉积的CuPc分子的堆积方式主要受到下层分子性质的影响，并借助等离子体基元耦合模型和激子理论对其聚集态结构的演变进行了分析。而CuPc溶液和薄膜的电致变色现象也正是源于H聚体与J聚体之间的转变。以CuPc／TiO_2纳米复合薄膜为光活化层制备了双层感光体，通过改变CuPc薄膜形貌可以对感光体的光电性能进行调控，光电导测试结果表明，只有厚度适当的CuPc薄膜才能充分利用入射的光能，在产生足够多的激子的同时，保证产生的激子可以迁移到CuPc／TiO_2界面处解离形成自由载流子，从而大大提高复合薄膜的光电导性能。
以高度有序的AAO为模板，使用溶胶．凝胶法和电泳沉积法分别制备了TiO_2和CuPc纳米线阵列，并结合两种方法通过二次沉积技术，将CuPc沉积在TiO_2纳米线和AAO模板孔壁之间的空隙处，得到了CuPc包覆的TiO_2纳米有序复合阵列。借助于瞬态荧光光谱证实了在复合纳米线中CuPc和TiO_2两者之间存在着光致电荷转移作用，通过改变EPD条件控制复合纳米线的形貌，可以调控复合纳米线的光电导性能。复合纳米线的光电导性能较单组分纳米线高出1-2个数量级。复合结构中酞菁铜包覆层与氧化钛纳米线之间较大的界面接触面积以及分离后的载流子定向连续传输通道是复合纳米线光电导性能提高的主要原因。
Tailoring the performance of materials via changing the morphologies and structures of materials has emerged as a new and important activity in optoelectronic functional materials and devices. The investigation of the relationship between structure and performance of optoelectronic composites would help to apprehend the optoelectronic mechanism, discover novel phenomenon, and raise new ideas. Photo-induced charge transfer in optoelectronic materials can be enhanced in one dimensional ordered nanocomposites and thus greatly improve the separation and transportation of charge carriers which are the key factors influencing optoelectronic device performance. The efficiency of photo-induced charge transfer in organic/inorganic nanocomposites can be effectively improved due to the effective contact in molecular level, larger contact area, and ordered directional donor/accepter nanocomposites construction which can be achieved through the ordered composite of organic and inorganic semiconductors and controlling the morphology of organic/inorganic ordered nanocomposites. In this dissertation, several approaches, anodic oxidation, sol-gel, vacuum thermal evaporation, and electrophoretic deposition, were carried out to fabricate high photosensitive CuPc/TiO_2 ordered nanocomposites. The optoelectronic property of the nanocomposites was investigated in details as well.
The recent progress on the application of organic/inorganic nanocomposites in the area of photoconductivity, photovoltaic characteristic, sensors, etc. was reviewed firstly. A detailed description was covered on optoelectronic field based on copper phthalocyanine (CuPc), phthalocyanine dyes and titania, including the preparation methods of nanocomposites used in this dissertation.
Size-controllable and high ordered vertically-oriented TiO_2 nanotube arrays were fabricated using anodic oxidation of pure titanium sheets in electrolyte solutions, and the crystallization of TiO_2 nanotubes could be tuned by altering annealing temperature. CuPc was filled into TiO_2 nanotubes by vacuum deposition at various deposition rates, a series of CuPc/TiO_2 ordered nanocomposites with various morphologies were achieved by tailoring the thickness of CuPc and the diameter of the TiO_2 nanotubes. A double-layered photoconductive device (Au/CuPc/TiO_2 nanotubes/titanium) was designed and fabricated with the CuPc/TiO_2 nanocomposites as photoactive layer. The photoconductive property of devices was studied via current-voltage(I-V) curves, and the current value increased by 2 or 3 orders of magnitude when exposed to light from dark, depending on the thickness of CuPc layer (100 nm for the best) and the diameter of TiO_2 nanotubes (70 nm for the best). For a control experiment, the I_l/I_d ratio of the device with disordered TiO_2 nanoparticles (TNPs) is obviously lower than that with ordered nanotube arrays. Several factors contribute to the improvement of photoconductive property of devices: the nanoarrays of TiO_2 nanotubes can enormously increase the contact area between CuPc and TiO_2, which offers much more sites for the exciton dissociation, and the one-dimensional and well-ordered structure of TiO_2 nanotube arrays can act as efficient transport channels. With the help of the aligned TiO_2 nanotubes, the collection and transfer efficiency of electrons is greatly enhanced, leading to an evident increase of photocurrent. The capturing and releasing majority carriers by traps or recombination centers at the donor/acceptor interface could effectively delay the process of collection or annihilation of charged carriers, which results in the hysteretic phenomenon of current change as device switches from light to dark and the reverse.
Phthalocyanine, a p-type organic semiconductor, contains bridging nitrogen atoms and can be easily protonated in organic acid solution. The protonated phthalocyanine molecules can orientationally migrate and nucleate on the negative electrode under external electric field. Basing on these considerations, CuPc/TiO_2 nanocomposites were fabricated by the electrophoretic deposition method (EPD) from the mixed solution of chloroform and trifluoroacetic acid containing the protonated CuPc. The morphology of the CuPc nanofilms can be manipulated by deposition time, concentration of CuPc, and applied voltage. The aggregation structure of the CuPc nanofilms was investigated by UV-vis spectroscopy and X-ray diffraction (XRD). The shift of Q-band absorption of CuPc nanofilms was resulted from the transition of aggregated structure of CuPc molecules. The XRD patterns demonstrated that the stack style of the deposited CuPc molecules is influenced by the property of the underlayer molecules. The evolvement of CuPc molecular aggregated structure was investigated by molecular exciton model and plasmon coupling, and the electrochromatic property of CuPc nanofilms and solution is derived from the transition of H- and J-aggregates. A dual-layered photoreceptors containing CuPc/TiO_2 nanocomposites as the charge generation layer (CGL) were designed and fabricated. The photoconductive property of photoreceptors was tailored via changing the morphology of the CuPc nanofilms. It was found that, to guarantee the adequate utilization of light energy, the thickness of the CuPc layer must be appropriate to efficiently absorb incident photons as well as to favor the migration of the excitons, which improved the photoconductivities of photoreceptors greatly.
Using highly-ordered porous anodic aluminum oxide (AAO) with nanopores perpendicular to the conductive substrate as the template, highly-ordered and well-aligned TiO_2 and CuPc nanowire arrays were prepared by assembly of TiO_2 precursors and CuPc in the AAO templates via sol-gel and EPD method, respectively. Coupling these two methods, a series of CuPc-coated TiO_2 ordered nanowire arrays were achieved via this secondary deposition technique. The photoluminescence spectra and the time-resolved fluorescence spectra of CuPc/TiO_2 nanowires confirmed the photoinduced charge transfer occurs between CuPc and TiO_2 nanowires, which contributes to the photoconductivity enhancement of CuPc/TiO_2 nanowires compared to pure CuPc or TiO_2 nanowires. The photoconductivity of the CuPc/TiO_2 nanowires can be tailored by changing the morphologies of CuPc/TiO_2 nanowires. It was found that the CuPc/TiO_2 nanowires arrays exhibited one or two orders of magnitude higher photoconductivity than that of pristine TiO_2 or CuPc nanowire arrays due to the large donor-acceptor (CuPc-TiO_2) contact area and the directional alignment of TiO_2 nanowires.
引文
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