染料敏化太阳电池的电子传输—复合模型与等效电路解析及其性能优化
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摘要
染料敏化太阳电池（dye-sensitized solar cells, DSSCs）是高性能低成本太阳电池的重要发展方向之一。由于DSSCs的光电转换受到一系列电子的产生、传输、聚集和复合过程的共同作用，深入研究电子在纳米多孔薄膜中的传输-复合过程，可以揭示影响DSSCs电性能的关键因素，从而为优化电池性能提供依据。电化学阻抗图谱(electrochemical impedance spectroscopy，EIS)与单二极管模型是分析DSSCs电流-电压特性影响因素的两种重要方法。准确获取单二极管模型参数，并借助EIS来建立单二极管模型参数与DSSCs内部微观过程的关联，有助于揭示电池电性能的限制因素并由此提出优化电池性能的具体措施。将二氧化钛介晶用于构筑双层复合膜光阳极，可以借助介晶的有序构造和光散射能力来进一步提升电池性能。
本文的第一部分内容提出了一种两步法以精确获取DSSCs单二极管等效电路模型参数。即通过作图法对电池的I-V特性曲线进行特定数据区域的线性化处理，从而获取具有一定精度的模型参数，以之设为最小二乘拟合过程的初值，经过多次迭代计算获取具有较高精度的拟合结果。在作图法的应用过程中发现，理论推导的线性函数关系，实际表现为离散性。本文采用对I-V特性曲线进行多项式近似处理的方法，获得了该线性关系和相应的模型参数值。拟合结果显示作图法的拟合误差约4%，经最小二乘法进一步精确后，拟合误差减小至低于1%。为了进一步验证提出的两步法的精确性，选取文献中I-V特性曲线进行拟合分析，并与文献中的拟合结果和精度进行了对比。拟合结果显示，两步法得到的模型参数值与文献中的结果有较大差别。拟合误差分析显示，文献中的拟合方法的误差约为5%，其拟合精度远低于本文提出的两步法。
本论文的第二部分内容为采用EIS图谱对DSSCs的单二极管等效电路模型参数进行解析。通过分析DSSCs在三个特征工作状态下的EIS图谱，研究了单二极管模型参数的物理和电化学意义。分析显示，DSSCs中与复合过程相关的总复合电阻Rct值与电池旁路电阻Rp值较好的吻合。在最大功率点和开路电压点，电池中的复合过程主要表现为电子从TiO_2导带向电解液的转移过程；Rp主要由二极管电阻Rdiode主导。而因此可以推论，TiO_2/电解液界面的电子转移过程具有二极管单向性的特性。在短路电流点，电池中的复合过程主要表现为电子从未被TiO_2覆盖的TCO向电解液的转移过程；Rp主要由并联电阻Rsh主导。因此，并联电阻Rsh可用于表征TCO/电解液界面的电流损失。通过较高工作电压时lnRct与电极电势的线性关系获得了理想因子n值，说明二极管理想因子n主要由较高工作电压时TiO_2/电解液界面的复合特性决定。验证了串联电阻Rs由TCO衬底欧姆电阻及电荷的传输、转移、扩散电阻共四部分构成。在此基础上，模拟了DSSCs的电性能随单二极管模型参数的变化，结果显示：串联电阻Rs和理想因子n对DSSCs的填充因子FF有显著作用，进而影响电池转换效率；随着DSSCs面积的增大，串联电阻Rs和并联电阻Rsh也将分别影响电池的短路电流Isc和开路电压Voc。根据单二极管模型参数的物理和电化学意义，探讨了DSSCs性能优化的一些可行性方案。
本文的第三部分内容研究了一种基于纳米多孔锐钛矿TiO_2介晶的双层复合膜光阳极DSSCs，并利用前二章发展的EIS和单二极管模型分析方法揭示了电子在多孔膜中的传输、复合过程对DSSCs性能的影响机制。首先，通过在TiO_2纳米晶水热合成中加入不同浓度的二乙烯三胺(Diethylenetriamine, DETA)来调控合成的TiO_2纳米晶的形貌，考察了TiO_2纳米晶形貌对纳米晶膜电池性能的影响。结果显示，随着DETA添加量的增加，部分纳米晶粒增大，纳米晶粒的不均匀性增高，导致纳米晶中缺陷密度的升高和薄膜中电子复合的加剧，但较快的电子传输速率仍使电池的收集效率得到改善。进一步增加DETA的添加量，染料吸附量的减小对电池性能的影响占主导地位，因此电池的性能反而随之下降。然后，采用溶剂热法合成了由纳米晶粒为基本结构单元有序聚集而成的纳米多孔锐钛矿TiO_2介晶。通过钛酸丁酯和乙酸的配比调控TiO_2介晶的形貌。选取最大比表面积的TiO_2介晶制备了多孔膜，使其覆盖在经过性能优化的纳米晶膜上，制备了双层复合膜光阳极DSSCs。考察了双层复合膜结构对电池性能的影响，并与单层纳米晶膜电池进行了对比。结果显示，由于TiO_2介晶为纳米晶粒的密集堆积，染料吸附量较小，但是介晶的三维有序结构和较少的晶界暴露使双层复合膜光阳极DSSCs具有较高的电子传输速率和电子寿命，从而获得了较大的电子收集效率。当总膜厚L同为15μm时，通过在膜厚为11μm的单层纳米晶膜上增加一层膜厚为4μm的纳米多孔锐钛矿TiO_2介晶层，得到的双层复合膜DSSCs相对单层纳米晶膜DSSCs，电池的转换效率由5.97%提升至6.35%。
Dye-sensitized solar cells (DSSCs) have been developed owing to the prospects of highperformance and low cost. The energy conversion procedure in DSSCs is affected by a seriesof electron processes such as generation, transport, accumulation and recombination.Therefore, electron transport-recombination processes in DSSCs should be investigated indetail to analyze the influencing factors of cell performance. Electrochemical impedancespectroscopy (EIS) and the single-diode model are two important methods to analyze theinfluencing factors of DSSCs’ current-voltage characterizations. Precise determination of themodel parameters as well as building a correlation between model parameters and internal cellprocesses by EIS interpretation will contribute to analyze limiting factors on cell performanceand explore specific strategies for cell optimization. A novel double-layered compound filmprepared by TiO_2mesocrystals with ordered structure and high light scattering property willalso help to further improve the performance of DSSCs.
In the first part of this dissertation, a two-step method was proposed to preciselydetermine the parameters of the single-diode model for DSSCs. By using the graphic method,model parameters were extracted with proper precision from the linearized current-voltagecharacterizations and subsequently were set as the initial values for non-linear least squares(NLLS) fitting. Model parameters with high precision were obtained by the two-step fittingmethod. In the graphic fitting step, linearity deduced form the implicit equation of thesingle-diode model turned to express quite scattered plot. In this work, polynomial expressionwas applied to approximate experimental data to derive the linearity and the correspondingparameters. It was testified the error of the graphic fitting was about4%which was futurereduced by NLLS fitting to less than1%. The two-step method was also applied to analyzethe I-V characterizations extracted from references. It was shown parameter values fit by thetwo-step method are different form those reported in reference. The accuracy of the two-stepmethod was validated since the fitting method reported in some references was about5%.
In the second part of this dissertation, the precisely determined parameters of thesingle-diode model were interpreted of their physical and electrochemical origins byanalyzing the EI spectra measured under three characteristic working conditions, the maximum-power point (MPP), the open-circuit voltage point (OCVP), and the short-circuitcurrent point (SCCP). It was shown, the total recombination resistance, Rct, coincided with theparallel resistance, Rp. When cells are operated at OCVP and MPP, electrons recombinemainly at TiO_2/electrolyte interface and Rpis dominated by the resistance of the diode, Rdiode.Therefore, the process of electron charge-transfer at TiO_2/electrolyte interface is considered toperform as the diode element of the single-diode model. In the case of operated at SCCP,electrons turn to recombine on TCO/electrolyte interface and Rpis dominated by shuntresistance, Rsh. Therefore, the shunt resistance can be used to characterize the current leakagefrom uncovered layer of TCO to electrolyte. The ideality factor n was obtained from thelinearity of lnRctas a function of cell potential and agreed with those fits of the single-diodemodel. This indicates ideality factor is dominated by the characterizations of electroncharge-transfer on TiO_2/electrolyte interface. The series resistance, Rswas verified to beconstituted by four electron process. Subsequently, the model parameters were evaluated interms of their effects on I-V characteristics of DSSCs via a single-diode model simulation.This simulation demonstrated that series resistance Rsand ideality factor n play crucial rolesin limiting fill factor FF of DSSCs; Upon up-scaled DSSCs, Rsand Rshvalues will also affectthe short-circuit current Iscand the open-circuit voltage Voc, respectively. Finally, strategiesare proposed to optimize DSSCs based on the physical and electrochemical interpretations oflimiting factors of cell performance.
In the third part of this dissertation, a novel kind of double-layered photoanode film wasprepared by nanoporous anatase TiO_2mesocrystals for the purpose to improve theperformance of DSSCs. EIS and the single-diode model were applied to investigate themechanisms of how electron transport-recombination processes influence on cell performance.In the first step, TiO_2nanocrystals were synthesized by controlling diethylenetriamine(DETA)/Ti molar ratio in hydrothermal system and DSSCs prepared by the synthesized TiO_2nanocrystals were investigated. It was shown, when more DETA was added in thehydrothermal system, parts of nanoparticles grow bigger leading to nonuniformity of TiO_2nanocrystals and aggravated electron recombination. Whereas, electron collection efficiencieswere improved attributing to faster electron transport in nanocrystalline films. However,further increasing DETA addition will result in decrease of dye adsorption and decline of cell performance. In the next step, one kind of TiO_2mesocrystals was synthesized with differentmorphologies by controlling tetrabutyl titanate (TBT)/acetic acid (HAc) volume ratio. TheTiO_2mesocrystals with highest surface area were used to prepare a layer of film covering ontop of a TiO_2nanocrystalline film to construct a novel double-layered photoanode structure.The DSSSs constructed by the double-layered photoanode film were characterized andcompared with cells based on a single-layered nanocrystalline film. It was shown, tightaggregation of nanocrystals in TiO_2mesocrystalline network resulted in low dye adsorption,whereas,3-D ordered structure in TiO_2mesocrystals contributed to high electron transportand electron lifetime. Therefore, when the thickness of nanocrystalline film and ofdouble-layered compound film is same of15μm, introducing a mesocrystalline film of4μmon top of a nanocrystalline film of11μm contributed to improve the efficiency from5.97%to6.36%.
本文的第一部分内容提出了一种两步法以精确获取DSSCs单二极管等效电路模型参数。即通过作图法对电池的I-V特性曲线进行特定数据区域的线性化处理，从而获取具有一定精度的模型参数，以之设为最小二乘拟合过程的初值，经过多次迭代计算获取具有较高精度的拟合结果。在作图法的应用过程中发现，理论推导的线性函数关系，实际表现为离散性。本文采用对I-V特性曲线进行多项式近似处理的方法，获得了该线性关系和相应的模型参数值。拟合结果显示作图法的拟合误差约4%，经最小二乘法进一步精确后，拟合误差减小至低于1%。为了进一步验证提出的两步法的精确性，选取文献中I-V特性曲线进行拟合分析，并与文献中的拟合结果和精度进行了对比。拟合结果显示，两步法得到的模型参数值与文献中的结果有较大差别。拟合误差分析显示，文献中的拟合方法的误差约为5%，其拟合精度远低于本文提出的两步法。
本论文的第二部分内容为采用EIS图谱对DSSCs的单二极管等效电路模型参数进行解析。通过分析DSSCs在三个特征工作状态下的EIS图谱，研究了单二极管模型参数的物理和电化学意义。分析显示，DSSCs中与复合过程相关的总复合电阻Rct值与电池旁路电阻Rp值较好的吻合。在最大功率点和开路电压点，电池中的复合过程主要表现为电子从TiO_2导带向电解液的转移过程；Rp主要由二极管电阻Rdiode主导。而因此可以推论，TiO_2/电解液界面的电子转移过程具有二极管单向性的特性。在短路电流点，电池中的复合过程主要表现为电子从未被TiO_2覆盖的TCO向电解液的转移过程；Rp主要由并联电阻Rsh主导。因此，并联电阻Rsh可用于表征TCO/电解液界面的电流损失。通过较高工作电压时lnRct与电极电势的线性关系获得了理想因子n值，说明二极管理想因子n主要由较高工作电压时TiO_2/电解液界面的复合特性决定。验证了串联电阻Rs由TCO衬底欧姆电阻及电荷的传输、转移、扩散电阻共四部分构成。在此基础上，模拟了DSSCs的电性能随单二极管模型参数的变化，结果显示：串联电阻Rs和理想因子n对DSSCs的填充因子FF有显著作用，进而影响电池转换效率；随着DSSCs面积的增大，串联电阻Rs和并联电阻Rsh也将分别影响电池的短路电流Isc和开路电压Voc。根据单二极管模型参数的物理和电化学意义，探讨了DSSCs性能优化的一些可行性方案。
本文的第三部分内容研究了一种基于纳米多孔锐钛矿TiO_2介晶的双层复合膜光阳极DSSCs，并利用前二章发展的EIS和单二极管模型分析方法揭示了电子在多孔膜中的传输、复合过程对DSSCs性能的影响机制。首先，通过在TiO_2纳米晶水热合成中加入不同浓度的二乙烯三胺(Diethylenetriamine, DETA)来调控合成的TiO_2纳米晶的形貌，考察了TiO_2纳米晶形貌对纳米晶膜电池性能的影响。结果显示，随着DETA添加量的增加，部分纳米晶粒增大，纳米晶粒的不均匀性增高，导致纳米晶中缺陷密度的升高和薄膜中电子复合的加剧，但较快的电子传输速率仍使电池的收集效率得到改善。进一步增加DETA的添加量，染料吸附量的减小对电池性能的影响占主导地位，因此电池的性能反而随之下降。然后，采用溶剂热法合成了由纳米晶粒为基本结构单元有序聚集而成的纳米多孔锐钛矿TiO_2介晶。通过钛酸丁酯和乙酸的配比调控TiO_2介晶的形貌。选取最大比表面积的TiO_2介晶制备了多孔膜，使其覆盖在经过性能优化的纳米晶膜上，制备了双层复合膜光阳极DSSCs。考察了双层复合膜结构对电池性能的影响，并与单层纳米晶膜电池进行了对比。结果显示，由于TiO_2介晶为纳米晶粒的密集堆积，染料吸附量较小，但是介晶的三维有序结构和较少的晶界暴露使双层复合膜光阳极DSSCs具有较高的电子传输速率和电子寿命，从而获得了较大的电子收集效率。当总膜厚L同为15μm时，通过在膜厚为11μm的单层纳米晶膜上增加一层膜厚为4μm的纳米多孔锐钛矿TiO_2介晶层，得到的双层复合膜DSSCs相对单层纳米晶膜DSSCs，电池的转换效率由5.97%提升至6.35%。
Dye-sensitized solar cells (DSSCs) have been developed owing to the prospects of highperformance and low cost. The energy conversion procedure in DSSCs is affected by a seriesof electron processes such as generation, transport, accumulation and recombination.Therefore, electron transport-recombination processes in DSSCs should be investigated indetail to analyze the influencing factors of cell performance. Electrochemical impedancespectroscopy (EIS) and the single-diode model are two important methods to analyze theinfluencing factors of DSSCs’ current-voltage characterizations. Precise determination of themodel parameters as well as building a correlation between model parameters and internal cellprocesses by EIS interpretation will contribute to analyze limiting factors on cell performanceand explore specific strategies for cell optimization. A novel double-layered compound filmprepared by TiO_2mesocrystals with ordered structure and high light scattering property willalso help to further improve the performance of DSSCs.
In the first part of this dissertation, a two-step method was proposed to preciselydetermine the parameters of the single-diode model for DSSCs. By using the graphic method,model parameters were extracted with proper precision from the linearized current-voltagecharacterizations and subsequently were set as the initial values for non-linear least squares(NLLS) fitting. Model parameters with high precision were obtained by the two-step fittingmethod. In the graphic fitting step, linearity deduced form the implicit equation of thesingle-diode model turned to express quite scattered plot. In this work, polynomial expressionwas applied to approximate experimental data to derive the linearity and the correspondingparameters. It was testified the error of the graphic fitting was about4%which was futurereduced by NLLS fitting to less than1%. The two-step method was also applied to analyzethe I-V characterizations extracted from references. It was shown parameter values fit by thetwo-step method are different form those reported in reference. The accuracy of the two-stepmethod was validated since the fitting method reported in some references was about5%.
In the second part of this dissertation, the precisely determined parameters of thesingle-diode model were interpreted of their physical and electrochemical origins byanalyzing the EI spectra measured under three characteristic working conditions, the maximum-power point (MPP), the open-circuit voltage point (OCVP), and the short-circuitcurrent point (SCCP). It was shown, the total recombination resistance, Rct, coincided with theparallel resistance, Rp. When cells are operated at OCVP and MPP, electrons recombinemainly at TiO_2/electrolyte interface and Rpis dominated by the resistance of the diode, Rdiode.Therefore, the process of electron charge-transfer at TiO_2/electrolyte interface is considered toperform as the diode element of the single-diode model. In the case of operated at SCCP,electrons turn to recombine on TCO/electrolyte interface and Rpis dominated by shuntresistance, Rsh. Therefore, the shunt resistance can be used to characterize the current leakagefrom uncovered layer of TCO to electrolyte. The ideality factor n was obtained from thelinearity of lnRctas a function of cell potential and agreed with those fits of the single-diodemodel. This indicates ideality factor is dominated by the characterizations of electroncharge-transfer on TiO_2/electrolyte interface. The series resistance, Rswas verified to beconstituted by four electron process. Subsequently, the model parameters were evaluated interms of their effects on I-V characteristics of DSSCs via a single-diode model simulation.This simulation demonstrated that series resistance Rsand ideality factor n play crucial rolesin limiting fill factor FF of DSSCs; Upon up-scaled DSSCs, Rsand Rshvalues will also affectthe short-circuit current Iscand the open-circuit voltage Voc, respectively. Finally, strategiesare proposed to optimize DSSCs based on the physical and electrochemical interpretations oflimiting factors of cell performance.
In the third part of this dissertation, a novel kind of double-layered photoanode film wasprepared by nanoporous anatase TiO_2mesocrystals for the purpose to improve theperformance of DSSCs. EIS and the single-diode model were applied to investigate themechanisms of how electron transport-recombination processes influence on cell performance.In the first step, TiO_2nanocrystals were synthesized by controlling diethylenetriamine(DETA)/Ti molar ratio in hydrothermal system and DSSCs prepared by the synthesized TiO_2nanocrystals were investigated. It was shown, when more DETA was added in thehydrothermal system, parts of nanoparticles grow bigger leading to nonuniformity of TiO_2nanocrystals and aggravated electron recombination. Whereas, electron collection efficiencieswere improved attributing to faster electron transport in nanocrystalline films. However,further increasing DETA addition will result in decrease of dye adsorption and decline of cell performance. In the next step, one kind of TiO_2mesocrystals was synthesized with differentmorphologies by controlling tetrabutyl titanate (TBT)/acetic acid (HAc) volume ratio. TheTiO_2mesocrystals with highest surface area were used to prepare a layer of film covering ontop of a TiO_2nanocrystalline film to construct a novel double-layered photoanode structure.The DSSSs constructed by the double-layered photoanode film were characterized andcompared with cells based on a single-layered nanocrystalline film. It was shown, tightaggregation of nanocrystals in TiO_2mesocrystalline network resulted in low dye adsorption,whereas,3-D ordered structure in TiO_2mesocrystals contributed to high electron transportand electron lifetime. Therefore, when the thickness of nanocrystalline film and ofdouble-layered compound film is same of15μm, introducing a mesocrystalline film of4μmon top of a nanocrystalline film of11μm contributed to improve the efficiency from5.97%to6.36%.
引文
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