全寡分子聚合物電解質於染料敏化太陽能電池之研究

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研究生：	朱家□ Chu, Chia-Hsien
論文名稱：	全寡分子聚合物電解質於染料敏化太陽能電池之研究 Study of Solvent-Free Oligomer Electrolytes for Dye-Sensitized Solar Cells
指導教授：	萬其超 Wan, Chi-Chao 王詠雲 Wang, Yung-Yun 王復民 Wang, Fu-Ming
口試委員:
學位類別：	碩士 Master
系所名稱：	工學院 - 化學工程學系 Department of Chemical Engineering
論文出版年：	2010
畢業學年度：	98
語文別：	英文
論文頁數：	118
中文關鍵詞：	染料敏化太陽能電池、固態高分子、電解質、聚矽氧烷
外文關鍵詞：	dye-sensitized solar cells, solvent-free, solid-state, polymer electrolytes, PMHS
相關次數：	點閱：2 下載：0
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本論文研究一系列含氧烷基(ethylene oxide)官能基之聚合物作為染料敏化太陽能電池(Dye-sensitized solar cells, DSSC)之非揮發性、高穩定性電解液。此高分子以氧烷基作為電子提供者，藉由和帶正電金屬離子例如鋰離子產生凡得瓦力吸引，幫助碘負離子解離出來。此高分子不僅有助於離子傳遞及氧化還原進行，並且扮以一¨溶劑¨之角色，電解質中毋須再加入其他溶劑來幫助解離，同時保留聚合物之高機械性質、高穩定性、低揮發性且利於加工之諸多優點，別於其他固態(不含溶劑)電解質，其優勢在於原物料便宜且合成容易。因此，此乃極具潛力作為DSSCs中之非揮發性固態電解質。
本研究首先開發出兩種新型固態高分子電解質，主要以聚矽氧烷(poly(methyl hydrosiloxane), PMHS) 為主鏈與含氧烷基之壓克力型寡聚物(Poly(ethyl glycol) methyl ether methacrylate, PEGMEMA)所構成之共聚物(PSEO)，利用聚矽氧烷之低玻璃轉移溫度特性來修飾並改善聚氧烷聚合物高結晶度問題，幫助離子可以在不含溶劑時順利傳遞。合成之固態共聚物其黏度為10.48 Pa-S(為水之三百萬倍)，黏度太高嚴重造成離子傳遞困難，使得導電度在常溫下只有10-5 S/cm，遠低於傳統有機溶劑(~10-2 S/cm)。為了改善此情況，於是藉重複單位(repeating unit)較少之PMHS合成出較小黏度之新共聚物(NPSEO)，其黏度大幅降低至115.94 Pa-S，將其與氧化還原對混合成電解質並實際組成DSSC以測試其光電轉換效能，發現仍然成效不佳，室溫效率僅為0.3%，仍然無法擺脫固態高分子文獻中低轉換效率的困境。
為了擺脫高分子固化造成黏度過高的缺點，改以僅用PEGMEMA混以氧化還原對及PMII(3-propyl-methylimidazolium chloride)成二元電解質。其實驗結果顯示：目前電池效能最高可達Jsc=9.89 mAcm-2, Voc=0.62 mV, ff=0.57,η= 3.51 %，其室溫下導電度約為1.16 mS/cm，I3-之擴散係數高達4.98*10-7cm2/S，其兩項指標可比擬文獻中以EMIBCN/PMII混合之二元離子液體電解質以及其他以純聚合物加上PMII混參之類似系統。在經過室溫下的長效測試後，電池性能也具有一定穩定性。除此之外，論文中並將這一系列聚氧烷聚合物電解質做研究，包含黏度、導電度以及I3-之擴散係數等。綜合以上成果，本研究最後成功開發出一種新型無任何溶劑添加之聚合物電解質，其高導電度以及高穩定性以及物料便宜之特性，實為一極具潛力之電解質。

A series of polymers with ethylene oxide (EO) functional group were synthesized and analyzed as non-volatile and highly stable electrolyte for dye-sensitized solar cells (DSSCs). The oxide atoms of EO group can coordinate to lithium ions and facilitate ion-pair separation, which favors ionic conduction. In this way, polymer with EO group plays a role as not only ionic transport and reduction helper but also as “solvent,” which can dissolve ions without adding other real solvents. Meanwhile, using polymers as electrolyte take an advantage of high mechanical properties, high stability, extremely low volatility and also being favor of commercial use and so on. Compared with other solvent-free and solid-state electrolytes, this polymer electrolyte is easily synthesized and costs low. Therefore, this EO-containing polymer possesses a great potential candidate as solvent-free and solid-state electrolyte.
In our study, we synthesized two novel solid-state co-polymer electrolytes (PSEO) at first, which contain Poly (methyl hydrosiloxane) (PMHS) as main back bone and Poly (ethyl glycol) methyl ether methacrylate (PEGMEMA) as side chain. To solve the high crystallization of Poly (ethylene oxide) (PEO), PMHS, which has a low Tg (Tg= -138oC), was used to modify PEGMEMA so that the ion transport can conduct favorably without solvent. Unfortunately, the viscosity of PSEO is as high as 310.48 Pa-S, about three hundred times higher than water at room temperature. High viscosity makes it difficult for ion transport, so the ionic conductivity of PSEO is only around 10-5 S/cm, which is much lower than conventional organic solvent (~10mS). In order to improve the problem of high viscosity, we used PMHS with less repeating units to obtian a new EO-containing co-polymer (NPSEO) with viscosity as low as 115.94 Pa-S. Mixing NPSEO and redox pairs together and fabricating into DSSCs to observe the cell performance and we found an unexpected results: the conversion efficiency is as low as 0.3%.
To get rid of the drawback of high viscosity for solidlike polymers, we used only PEGMEMA instead of using co-polymers and form a binary electrolyte with redox pairs. The results that cell performance of PEGMEMA-based electrolytes in DSSCs presented are η= 3.51%, Jsc= 9.89 mA/cm2, Voc= 0.62 mV, ff= 0.57. Their ambient ionic conductivity is 1.16 mS/cm and the diffusion coefficient of tri-iodide dominates at around 4.98×10-7cm2/S. These two indexed can be compared to EMIBCN/PMII mixing binary ionic liquid reported or other similar PMII-doping system. After long-term stability at room temperature, the cell performance keeps at a stable condition. Except for that, we study the series EO-containing polymers in this study including viscosity, ionic conductivity and diffusion coefficient of tri-iodide and so on. In conclusion, we developed a novel solvent-free polymer-based electrolyte successfully, which has a great potential due to its high ionic conductivity, high stability and cheap properties.

摘要    I
Abstract    III
Acknowledge    V
Table of Contents    VII
List of Tables    X
List of Figures    VII

Chapter1、Introduction---------------------------------------------------------1
1    Overview of Dye-sensitized solar cells    2
2    Structures and Operational principles of DSSC    3
3    Development of hole conductors employed in solid-state DSSCs    5
4    Motivation of The Study    8
Chapter2、A Literature Survey on polymer electrolytes-----------------10
1    The generation of polymer electrolytes    10
2    Review of Polymer Electrolytes based DSSCs    14
3    Recent progress of polymer electrolytes in DSSCs    16
4    Properties of polymer electrolytes    22
4.1Physical and chemical properties of polymer electrolyte----------19
4.2Electrochemical properties of polymer electrolyte------------------27
4.2.1    Preparation of Photoanodes --------------------------------23
4.2.2 Electrochemical measurements of the diffusion coefficient of triiodide(DI3-)--------------------------------------------------29
4.2.3    AC impedance analysis-------------------------------------31
5    The major challenges of a solvent-free polymer based electrolytes    33
5.1 Poor contact with TiO2 electrode ------------------------------------33
5.2 High viscosity and low conductivity ---------------------------------33
Chapter3、A Literature Survey on polymer electrolytes    34
1 Synthesis of Polysiloxane with EO group----------------------------------34
1.1 Materials -------------------------------------------------------------34
1.2Synthesis Methods----------------------------------------------------35
2 Measurement of ionic conductivity------------------------------------------38
3 Measurement of viscosity----------------------------------------------------39
4Preparation of DSSC----------------------------------------------------------40
4.1 Materials --------------------------------------------------------------40
4.2 Preparation and Assembly of DSSC ---------------------------------42
4.2.1 Preparation of Photoanodes ------------------------------------42
4.2.2 Preparation of Pt-Catalyzed Counter Electrodes --------------43
4.2.3DSSC Assembly--------------------------------------------------44
4.2.4 Photocurrent Measurements------------------------------------46
5 Positron Annihilation Lifetime Spectroscopy (PALS) Measurement --------------------------------------------------------------------------------------47
6 Experiment Design ---------------------------------------------------------49
Chapter4、Results and Discussions    49
Part A. Development of a Solvent-Free Polysiloxane-based Polymer Electrolyte(PSEO)     50
1 A suitable I-/I3- ratio Addition Used in Polysiloxane-based Electorlytes-50
1.1    The Effect of I-/I2 ratio on Ionic Conductivity----------------------53
1.1.1 I-/I2 effects on ionic conductivity of polymer electrolyte-------------------------------------------------53
1.2 The Effect of I-/I2 on Bulk Viscosity--------------------------------56
2 Evaluation of the performances of Polymer Based DSSCs-----------------60
2.1 Cell Performances of Electrolytes based on EO Group-Containing
Polymer Electrolyte---------------------------------------------------60
3 Analysis of Wettability in the Interfaces between Electrolytes and TiO2 Electrode----------------------------------------------------------------------63
4 Selective of PMII as Additive---------------------------------------------66
Part B. Development of a Solvent-Free Polysiloxane-based Polymer Electrolyte with a Low-Molecular-Weight (NPSEO)     68
5 Strategies to Improve the Penetration of PSEO-Based Electrolyte System inside the Nanopore of TiO2 Layer---------------------------68
5.1 Modification of Polymer Electrolytes-NPSEO------------69
5.2 Characterization of Modified Polysiloxane----------------71
5.3 Ionic Conductivity and Viscosity Measurements of NPSEO
--------------------------------------------------------------------75
5.3.1 Viscosity Measurement----------------------------------76
5.3.2 Ionic conductivity Measurement-----------------------79
5.4Evaluations of Modified Polymer Electrolytes(NPSEO)-81
Part C. Development of a Solvent-Free PEGMEMA based Polymer Electrolyte( without polysiloxane) ------------------------------------------83
6 PEGMEMA-based Polymer Electrolyte without Polysiloxane ------83
6.1 Structure of PEGMEMA and Composition of PEGMEMA-Based Polymer Electrolytes---------------85
6.2   Viscosity of the PEGMEMAs-----------------------------88
6.3   Ionic Conductivity of the PEGMEMAs------------------89
6.4 Cell Performances of PEGMEMA-Based Polymer Electrolytes-------------------------------------------------89
6.4.1 Cell performances of PEGMEMA-based polymer electrolytes ---------------------------------------------89
6.4.2 Using Thinner Polymer Electrolyte Film to Improve the Cell Performance----------------------91
6.4.3 Long-term Stability of PEGMEMA188-based electrolytes for DSSCs ------------------------------94
6.5 Electrochemical Measurements of the Diffusion Coefficient of triiodide(DI3-)-------------------------------------------------96
6.6   EIS Analysis on PEGMEMAs electrolytes-------------100
7Free Volume Studies of the Series of PEGMEMAs ------------------104
Chapter5、Conclusions    102
Chapter6、Future Works    103
Reference---------------------------------------------------------------------104

                                

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