基于酞菁和富勒烯的有机太阳电池的研制及其相关系统与控制的研究
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摘要
有机太阳电池作为一种新型的太阳能光伏器件，与无机太阳电池相比，具有原材料广泛、质量轻、成本低、可大面积制作、具有柔性等优点。在能源问题日益突出的当今世界，有机太阳电池作为一种低成本、轻薄型的光电转换器件，具有十分宽广的发展空间、非常重要的实际利用价值和光明的应用前景。
本论文以酞菁铜和富勒烯组成的有机小分子太阳电池作为研究对象，重点研究了基于酞菁铜和碳60的双层异质结太阳电池有源层最佳厚度组合问题、LiF阴极修饰层的使用及其机理、阳极修饰层的工作机理及其改进、电子受主材料的改善、器件的稳定性与衰减情况等。
本论文首先对CuPc/C60电池进行了内部光强分布的研究。在基于光学传输矩阵确定器件内部的光强分布函数后，本论文定义了一个新的参量“有效激子产生速率”——单位时间单位面积上施主/受主界面两侧各一个激子扩散长度内光生激子的产生总量；并且将AM1.5G标准光照下太阳光子流密度谱以及衬底的透射情况都引入到了有效激子产生速率的计算过程中，最终得到在实验中使用的ITO基底上制备的CuPc/C60双层异质结有机太阳电池的最佳有源层厚度组合。经过大量实验对该理论结果进行了验证，理论和实际之间的误差是在可接受的范围内的。故利用有效激子产生速率的方法对有机太阳电池有源层厚度的最佳组合的搜索是可以起到一定的指导作用的。这也是本论文的创新点之一。
在得到最佳有源层厚度组合之后，通过在有机有源层与金属阴极之间插入一层极薄的LiF修饰层可以非常显著地改善有机太阳电池的电性能。本论文对LiF阴极修饰层的厚度进行了优化，发现本实验中LiF阴极修饰层的最优厚度为1.5nm。本论文同时又对LiF阴极修饰层的工作机理进行了分析。在总结文献中常见的LiF阴极修饰层工作机理分析的基础上运用了MIS机理来解释器件性能提高的原因，包括同时可以解释器件短路电流密度和开路电压均得到提高的原因。
在阳极附近同样存在着相当多的缺陷。本论文经过对基于CuPc/C60的有机异质结小分子太阳电池的阳极界面进行多种改善工作，使得器件的性能得到了大幅度的提升。首先在阳极界面处引入LiF薄膜，器件的光电转换效率得到了一定的提升。模仿阴极LiF修饰层工作机理的分析方法，将MIS引入到阳极LiF修饰层工作机理的解释上，发现同样适用。说明MIS结构的解释具有一定的通用性。其次，在阳极界面处引入PEDOT:PSS修饰层，器件的光照特性，特别是短路电流密度得到了大幅度的提高。PEDOT:PSS修饰层的主要作用是平滑界面、改善载流子输出、降低接触电阻。再次，将PEDOT:PSS修饰层和LiF修饰层同时使用，构成PEDOT:PSS/LiF双阳极修饰层系统。该修饰层系统可以综合发挥两种修饰层材料的优势，使得器件的光电转换特性可以进一步得到提高。这是本论文的另一个创新点。
本论文除了在电极界面处进行改进工作外，对器件的材料亦做了相应的改善工作。将富勒烯中的C70用于替换有机小分子太阳电池中的C60，与施主材料CuPc构成新的CuPc/C70异质结。实际结果发现，基于CuPc和C70的有机小分子太阳电池同样表现出光伏特性，并且其电性能比CuPc/C60电池更为优越。C70在可见光范围内具有更优越的吸收特性。同时经过分析在C60分子内部载流子复合几率较高；而且C70的电导率要高于C60两个数量级。这就使得使用C70的有机太阳电池在短路电流密度、开路电压以及填充因子等方面表现得更好。对CuPc/C60和CuPc/C70电池的系统全面的对比研究是本论文第三个创新点。
本论文除了对基于酞菁铜和富勒烯的有机小分子太阳电池的光电转换特性的提高进行改善工作的研究之外，还对论文中进行研究的所有结构的器件的稳定性进行了详细的研究，得出不同器件的稳定性及衰减情况，并对引起稳定性变化的因素进行了分析。
对于无任何电极修饰层的CuPc/C60有机小分子太阳电池，在无封装的条件下，将器件置于洁净的、低湿度干燥的空气中时，器件除填充因子外，短路电流密度、开路电压以及光电转换效率都会先提升后衰减。当距离制备完成后一个小时左右，器件转换效率达到最高值。分析其中的原因，主要是在C60和Al的界面处由于氧气的侵入形成了一层Al2O3层。Al2O3层的作用与LiF层是一致的，起到了阴极修饰层的作用。在本论文中建议对于无任何电极修饰层的CuPc/C60有机小分子太阳电池，其最佳的封装时间是距离制备完成一个小时左右。这是本论文第四个创新点。
其他添加了电极修饰层的电池，性能随时间并未提高，只是简单的衰减。其稳定性从优到差依次为：同时使用PEDOT:PSS/LiF阳极修饰层系统和LiF阴极修饰层的器件、同时使用LiF阳极修饰层和LiF阴极修饰层的器件、仅使用LiF阴极修饰层的器件、同时使用PEDOT:PSS阳极修饰层和LiF阴极修饰层的器件。本论文对引起器件衰减的原因以及引起衰减差异的原因进行了详细的分析并加以实验验证。
最后，本论文还进行了CuPc/C60和CuPc/C70有机小分子太阳电池稳定性的对比研究。研究发现，使用C70作为电子受主材料的电池的稳定性要优于以C60为受主材料的器件。主要原因是C60和C70被氧气侵蚀的程度不同。因此C70相对于C60更合适于有机太阳电池的研究、开发以及制备。
另外，本论文还做了一些与酞菁铜/富勒烯的有机小分子太阳电池相关系统与控制工作的初步研究。比如寻找了实验中材料真空蒸发膜厚监控的参数以及得到这些参数的方法，以实现今后的在线控制；设计了一台LED太阳光模拟器用于低成本检测；建立了有机太阳电池的等效模型，并使用两种方法对等效模型的参数进行辨识拟合，并且辨识出不同器件的模型参数与之前实验结果与分析是相一致的；最后分析了太阳电池组件匹配损失的影响因素，分析了有机太阳电池组件中电池分档的标准。
本论文的重点在于解决电极与有源层界面处激子复合和载流子输运的问题；受主材料的改进问题，即两种富勒烯分子选择的问题；器件衰减机理问题等。论文侧重于对实验现象进行机理性的探索与分析，注重基础问题的研究。希望通过这些基础研究能够对基于酞菁铜/富勒烯的有机小分子太阳电池有更深刻的理解，对今后的研究工作能够提供某些指导性的建议。
Organic solar cells, as a kind of new photovoltaic devices, compared to inorganicsolar cells, have many advantages, such as light weight, low cost, good mechanicalflexibility, large area fabrication, etc. Nowadays, since the power problem is more andmore serious, there is a wide developing space, an important practical value and a brightutilizing foreground for organic solar cells.
The organic solar cells based on copper phthalocyanine and fullerene are studied inthis thesis. The investigation includes the optimization of thickness combination of CuPcand C60, LiF cathode buffer layer and its mechanism, the mechanisms and theirimprovements of the anode buffer layers, the improvements of electron acceptor materials,and the stability and degradation of the cells.
Firstly, the light intensity distribution inside the CuPc/C60cells is studied. Based onthis result, a new parameter called “Effective Exciton Generation Velocity” is defined,which describes the amount of the excitons that can diffuse to the donor/acceptor interfacein a unit area and a unit time. The photon distribution of AM1.5G sunlight and thetransmisstivity of the substrate are introduced into the calculation process. In this thesis,the optimized thickness combination of CuPc and C60is obtained, and it is verified bypractical experiment. The error is in an acceptable range. So it is a useful way to searchingthe best thickness combination of the active layers by utilizing the method of effectiveexciton generation velocity. And this method is one of innovation points in this thesis.
After obtaining the best thickness of CuPc and C60, the cells’ characteristics can beimproved by inserting an ultrathin LiF layer between the cathode and acceptor. In thisthesis, the thickness of LiF cathode buffer layer is optimized and the best thickness is1.5nm. The mechanism of this cathode buffer is also discussed. An MIS structure is used hereto explain the increase of both short circuit current density and open circuit voltage of thedevices.
Actually, a lot of defects also exist in the anode interface. The characteristics of thecells are improved a lot after the utilization of the anode buffer layers. Firstly, LiF anodebuffer layer is introduced. And an MIS structure can also successfully explain themechanism here. So it can be concluded that the MIS method is a universal way to explainthis kind problem. Secondly, a PEDOT:PSS layer is introduced. The characteristics of the cells, especially the short circuit current density are improved a lot. The function of thisPEDOT:PSS layer is to smooth the anode surface, to improve the output of carriers and todecrease the interface resistance. At last, a PEDOT:PSS/LiF anode buffer layer system isused. The performances of the cells with this system are better than those of the cells witha single LiF layer and with a single PEDOT:PSS layer. And this is another innovationpoint in this thesis.
Beside the investigation on the improvements at the electrode interfaces, the work onthe acceptor improvement is also studied. C70is used to replace C60as an acceptor in thisthesis. The cells using C70as an acceptor show higher Jsc, Voc, FF and efficiency than thatof the ones using C60-acceptor, because of its higher responsibility in visible region, betterelectron transport and quantum current distribution in C70molecule, and its higherconductivity. This is the third innovation point in this thesis.
The stability and degradation of the cells in this thesis are also discussed.
For a CuPc/C60cell without any electrode buffers, the performances improve a littleafter placing in the clean air for a while (about an hour). That is caused by an ultrathinAl2O3which is formed between C60and Al. Its function is as a cathode buffer layer. Then,with the increase of the thickness of Al2O3, the performances of the devices degrade. Sothe encapsulation time should be about an hour later after fabrication. This is the fourthinnovation point in this thesis.
Contrary, the performances of the cells with electrode buffers directly and simplydecline. The increase of the performances in the first hour cannot be seen. The order of thestability from the best to the worst is as follow,①the cells with PEDOT:PSS/LiF anodebuffer system and LiF cathode buffer layer;②the cells with LiF anode buffer layer andLiF cathode buffer layer;③the cells only with LiF cathode buffer layer;④the cells withPEDOT:PSS anode buffer layer and LiF cathode buffer layer. The mechanisms whichcause the different stability are discussed.
At last, the stability of the cells based on CuPc/C60and CuPc/C70is comparativelystudied. The cells using C70as an acceptor also show a superior stability than that of thecells using C60-acceptor. This comes from the higher electron affinity and ionizationpotential, and the lower symmetry of C70. Using C70as an acceptor not only can increasethe photovoltaic characteristics, but also can improve the stability of the cells dramatically.
Additionally, some relative jobs based on copper phthalocyanine/fullerene organicsolar cells are also done, such as obtaining the thickness control parameters of theexperimental materials in thermal vacuum evaporation, the design of LED sun simulatorfor low cost test, building the equivalent circuit model of organic solar cells and the modelparameters identification by two different methods, and at the end, analyzing the influencefactors of mismatch in solar cell modules and giving a suggestion of gradating organicsolar cells.
In this thesis, the emphases are focused on the improvements of the interface betweenthe electrode and active layer, the improvement of acceptor material (i.e. the choice of the two kinds of fullerene molecules), and the investigation on the stability and degradation oforganic solar cells. The research and analysis on the mechanisms and some basic problemsof small molecule organic solar cells are the emphases. It is hoped that the understandingof small molecule organic solar cells based on phthalocyanine and fullerene could be moreintensive from this thesis, and some instructional suggestions may be given to the laterinvestigation.
本论文以酞菁铜和富勒烯组成的有机小分子太阳电池作为研究对象，重点研究了基于酞菁铜和碳60的双层异质结太阳电池有源层最佳厚度组合问题、LiF阴极修饰层的使用及其机理、阳极修饰层的工作机理及其改进、电子受主材料的改善、器件的稳定性与衰减情况等。
本论文首先对CuPc/C60电池进行了内部光强分布的研究。在基于光学传输矩阵确定器件内部的光强分布函数后，本论文定义了一个新的参量“有效激子产生速率”——单位时间单位面积上施主/受主界面两侧各一个激子扩散长度内光生激子的产生总量；并且将AM1.5G标准光照下太阳光子流密度谱以及衬底的透射情况都引入到了有效激子产生速率的计算过程中，最终得到在实验中使用的ITO基底上制备的CuPc/C60双层异质结有机太阳电池的最佳有源层厚度组合。经过大量实验对该理论结果进行了验证，理论和实际之间的误差是在可接受的范围内的。故利用有效激子产生速率的方法对有机太阳电池有源层厚度的最佳组合的搜索是可以起到一定的指导作用的。这也是本论文的创新点之一。
在得到最佳有源层厚度组合之后，通过在有机有源层与金属阴极之间插入一层极薄的LiF修饰层可以非常显著地改善有机太阳电池的电性能。本论文对LiF阴极修饰层的厚度进行了优化，发现本实验中LiF阴极修饰层的最优厚度为1.5nm。本论文同时又对LiF阴极修饰层的工作机理进行了分析。在总结文献中常见的LiF阴极修饰层工作机理分析的基础上运用了MIS机理来解释器件性能提高的原因，包括同时可以解释器件短路电流密度和开路电压均得到提高的原因。
在阳极附近同样存在着相当多的缺陷。本论文经过对基于CuPc/C60的有机异质结小分子太阳电池的阳极界面进行多种改善工作，使得器件的性能得到了大幅度的提升。首先在阳极界面处引入LiF薄膜，器件的光电转换效率得到了一定的提升。模仿阴极LiF修饰层工作机理的分析方法，将MIS引入到阳极LiF修饰层工作机理的解释上，发现同样适用。说明MIS结构的解释具有一定的通用性。其次，在阳极界面处引入PEDOT:PSS修饰层，器件的光照特性，特别是短路电流密度得到了大幅度的提高。PEDOT:PSS修饰层的主要作用是平滑界面、改善载流子输出、降低接触电阻。再次，将PEDOT:PSS修饰层和LiF修饰层同时使用，构成PEDOT:PSS/LiF双阳极修饰层系统。该修饰层系统可以综合发挥两种修饰层材料的优势，使得器件的光电转换特性可以进一步得到提高。这是本论文的另一个创新点。
本论文除了在电极界面处进行改进工作外，对器件的材料亦做了相应的改善工作。将富勒烯中的C70用于替换有机小分子太阳电池中的C60，与施主材料CuPc构成新的CuPc/C70异质结。实际结果发现，基于CuPc和C70的有机小分子太阳电池同样表现出光伏特性，并且其电性能比CuPc/C60电池更为优越。C70在可见光范围内具有更优越的吸收特性。同时经过分析在C60分子内部载流子复合几率较高；而且C70的电导率要高于C60两个数量级。这就使得使用C70的有机太阳电池在短路电流密度、开路电压以及填充因子等方面表现得更好。对CuPc/C60和CuPc/C70电池的系统全面的对比研究是本论文第三个创新点。
本论文除了对基于酞菁铜和富勒烯的有机小分子太阳电池的光电转换特性的提高进行改善工作的研究之外，还对论文中进行研究的所有结构的器件的稳定性进行了详细的研究，得出不同器件的稳定性及衰减情况，并对引起稳定性变化的因素进行了分析。
对于无任何电极修饰层的CuPc/C60有机小分子太阳电池，在无封装的条件下，将器件置于洁净的、低湿度干燥的空气中时，器件除填充因子外，短路电流密度、开路电压以及光电转换效率都会先提升后衰减。当距离制备完成后一个小时左右，器件转换效率达到最高值。分析其中的原因，主要是在C60和Al的界面处由于氧气的侵入形成了一层Al2O3层。Al2O3层的作用与LiF层是一致的，起到了阴极修饰层的作用。在本论文中建议对于无任何电极修饰层的CuPc/C60有机小分子太阳电池，其最佳的封装时间是距离制备完成一个小时左右。这是本论文第四个创新点。
其他添加了电极修饰层的电池，性能随时间并未提高，只是简单的衰减。其稳定性从优到差依次为：同时使用PEDOT:PSS/LiF阳极修饰层系统和LiF阴极修饰层的器件、同时使用LiF阳极修饰层和LiF阴极修饰层的器件、仅使用LiF阴极修饰层的器件、同时使用PEDOT:PSS阳极修饰层和LiF阴极修饰层的器件。本论文对引起器件衰减的原因以及引起衰减差异的原因进行了详细的分析并加以实验验证。
最后，本论文还进行了CuPc/C60和CuPc/C70有机小分子太阳电池稳定性的对比研究。研究发现，使用C70作为电子受主材料的电池的稳定性要优于以C60为受主材料的器件。主要原因是C60和C70被氧气侵蚀的程度不同。因此C70相对于C60更合适于有机太阳电池的研究、开发以及制备。
另外，本论文还做了一些与酞菁铜/富勒烯的有机小分子太阳电池相关系统与控制工作的初步研究。比如寻找了实验中材料真空蒸发膜厚监控的参数以及得到这些参数的方法，以实现今后的在线控制；设计了一台LED太阳光模拟器用于低成本检测；建立了有机太阳电池的等效模型，并使用两种方法对等效模型的参数进行辨识拟合，并且辨识出不同器件的模型参数与之前实验结果与分析是相一致的；最后分析了太阳电池组件匹配损失的影响因素，分析了有机太阳电池组件中电池分档的标准。
本论文的重点在于解决电极与有源层界面处激子复合和载流子输运的问题；受主材料的改进问题，即两种富勒烯分子选择的问题；器件衰减机理问题等。论文侧重于对实验现象进行机理性的探索与分析，注重基础问题的研究。希望通过这些基础研究能够对基于酞菁铜/富勒烯的有机小分子太阳电池有更深刻的理解，对今后的研究工作能够提供某些指导性的建议。
Organic solar cells, as a kind of new photovoltaic devices, compared to inorganicsolar cells, have many advantages, such as light weight, low cost, good mechanicalflexibility, large area fabrication, etc. Nowadays, since the power problem is more andmore serious, there is a wide developing space, an important practical value and a brightutilizing foreground for organic solar cells.
The organic solar cells based on copper phthalocyanine and fullerene are studied inthis thesis. The investigation includes the optimization of thickness combination of CuPcand C60, LiF cathode buffer layer and its mechanism, the mechanisms and theirimprovements of the anode buffer layers, the improvements of electron acceptor materials,and the stability and degradation of the cells.
Firstly, the light intensity distribution inside the CuPc/C60cells is studied. Based onthis result, a new parameter called “Effective Exciton Generation Velocity” is defined,which describes the amount of the excitons that can diffuse to the donor/acceptor interfacein a unit area and a unit time. The photon distribution of AM1.5G sunlight and thetransmisstivity of the substrate are introduced into the calculation process. In this thesis,the optimized thickness combination of CuPc and C60is obtained, and it is verified bypractical experiment. The error is in an acceptable range. So it is a useful way to searchingthe best thickness combination of the active layers by utilizing the method of effectiveexciton generation velocity. And this method is one of innovation points in this thesis.
After obtaining the best thickness of CuPc and C60, the cells’ characteristics can beimproved by inserting an ultrathin LiF layer between the cathode and acceptor. In thisthesis, the thickness of LiF cathode buffer layer is optimized and the best thickness is1.5nm. The mechanism of this cathode buffer is also discussed. An MIS structure is used hereto explain the increase of both short circuit current density and open circuit voltage of thedevices.
Actually, a lot of defects also exist in the anode interface. The characteristics of thecells are improved a lot after the utilization of the anode buffer layers. Firstly, LiF anodebuffer layer is introduced. And an MIS structure can also successfully explain themechanism here. So it can be concluded that the MIS method is a universal way to explainthis kind problem. Secondly, a PEDOT:PSS layer is introduced. The characteristics of the cells, especially the short circuit current density are improved a lot. The function of thisPEDOT:PSS layer is to smooth the anode surface, to improve the output of carriers and todecrease the interface resistance. At last, a PEDOT:PSS/LiF anode buffer layer system isused. The performances of the cells with this system are better than those of the cells witha single LiF layer and with a single PEDOT:PSS layer. And this is another innovationpoint in this thesis.
Beside the investigation on the improvements at the electrode interfaces, the work onthe acceptor improvement is also studied. C70is used to replace C60as an acceptor in thisthesis. The cells using C70as an acceptor show higher Jsc, Voc, FF and efficiency than thatof the ones using C60-acceptor, because of its higher responsibility in visible region, betterelectron transport and quantum current distribution in C70molecule, and its higherconductivity. This is the third innovation point in this thesis.
The stability and degradation of the cells in this thesis are also discussed.
For a CuPc/C60cell without any electrode buffers, the performances improve a littleafter placing in the clean air for a while (about an hour). That is caused by an ultrathinAl2O3which is formed between C60and Al. Its function is as a cathode buffer layer. Then,with the increase of the thickness of Al2O3, the performances of the devices degrade. Sothe encapsulation time should be about an hour later after fabrication. This is the fourthinnovation point in this thesis.
Contrary, the performances of the cells with electrode buffers directly and simplydecline. The increase of the performances in the first hour cannot be seen. The order of thestability from the best to the worst is as follow,①the cells with PEDOT:PSS/LiF anodebuffer system and LiF cathode buffer layer;②the cells with LiF anode buffer layer andLiF cathode buffer layer;③the cells only with LiF cathode buffer layer;④the cells withPEDOT:PSS anode buffer layer and LiF cathode buffer layer. The mechanisms whichcause the different stability are discussed.
At last, the stability of the cells based on CuPc/C60and CuPc/C70is comparativelystudied. The cells using C70as an acceptor also show a superior stability than that of thecells using C60-acceptor. This comes from the higher electron affinity and ionizationpotential, and the lower symmetry of C70. Using C70as an acceptor not only can increasethe photovoltaic characteristics, but also can improve the stability of the cells dramatically.
Additionally, some relative jobs based on copper phthalocyanine/fullerene organicsolar cells are also done, such as obtaining the thickness control parameters of theexperimental materials in thermal vacuum evaporation, the design of LED sun simulatorfor low cost test, building the equivalent circuit model of organic solar cells and the modelparameters identification by two different methods, and at the end, analyzing the influencefactors of mismatch in solar cell modules and giving a suggestion of gradating organicsolar cells.
In this thesis, the emphases are focused on the improvements of the interface betweenthe electrode and active layer, the improvement of acceptor material (i.e. the choice of the two kinds of fullerene molecules), and the investigation on the stability and degradation oforganic solar cells. The research and analysis on the mechanisms and some basic problemsof small molecule organic solar cells are the emphases. It is hoped that the understandingof small molecule organic solar cells based on phthalocyanine and fullerene could be moreintensive from this thesis, and some instructional suggestions may be given to the laterinvestigation.
引文
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