電沉積電子傳輸層應用於鈣鈦礦太陽能電池之研究

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研究生：	蘇子森 Su, Tzu-Sen
論文名稱：	電沉積電子傳輸層應用於鈣鈦礦太陽能電池之研究 Electrodeposition of electron-transporting layers for perovskite solar cells
指導教授：	衛子健 Wei, Tzu-Chien
口試委員:	宮坂力賴志煌何國川葉鎮宇 Miyasaka, Tsutomu
學位類別：	博士 Doctor
系所名稱：	工學院 - 化學工程學系 Department of Chemical Engineering
論文出版年：	2019
畢業學年度：	107
語文別：	英文
論文頁數：	116
中文關鍵詞：	二氧化鈦、電沉積、電極動力學、電子傳輸層、鈣鈦礦太陽能電池
外文關鍵詞：	Titanium dioxide, Electrodeposition, Kinetics of electrode reactions, Electron-transporting layer, Perovskite solar cell
相關次數：	點閱：2 下載：0
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本研究著重於開發三氯化鈦水溶液為前驅物的二氧化鈦電沉積技術，並且成功將製備之二氧化鈦薄膜應用在鈣鈦礦太陽能電池的電子傳輸層上。起初第三章中，藉由了解此電沉積反應的電極動力學後，進一步透過簡易的調控電流密度與操作電壓來控制電沉積薄膜的形貌與厚度。
第四章中，以定電流沉積鈣鈦礦太陽能電池之緻密層，並與浸泡法、旋轉塗佈法和熱噴霧裂解法製作之緻密層相比較，發現以電沉積技術製作的緻密層不僅覆蓋率佳和厚度薄，甚至可以長出類似苔癬的三維結構，實驗證實除了薄且密的緻密層能有效降低界面再結合外，更因為該三維結構提供的低接觸電阻，使鈣鈦礦太陽能元件的內電阻(series resistance)降低，提升元件填充因子(Fill factor)值。
第五章中，在成功利用電沉積法製備高效能緻密層後，並藉由多重階段(multi-steps)電壓沉積參數，以一鍋法(one-pot)一道次依序完成緻密層與支架層的沉積。其中，結果顯示當過電位小於0.15V時為動力學控制區，可沉積較為緻密之結構；當過電位介於0.15-0.25 V時，為動力學控制與質傳控制區間的轉折區，可得到較為多孔的結構。以此電沉積一鍋法製備之電子傳輸層相較傳統旋塗法有較優異的元件表現。再者，此方法不僅可以大幅縮短含支架層之鈣鈦礦太陽能電池製程，同時達到全製程中單一次燒結的節能目標。
第六章中，於三氯化鈦水溶液加入錫異質金屬進行共鍍，將電沉積的二氧化鈦進行金屬摻雜並改善其自身電性差的缺陷，由XPS數據分析與電性量測，結果證實錫金屬確實摻雜入二氧化鈦中，且薄膜電性隨著摻雜濃度而上升，製備之元件效能亦有所提升，此共鍍技術將大幅開闊電沉積二氧化鈦的應用面向，使電沉積技術更加多元全面。
最後章節嘗試以自行設計之環保循環鍍槽進行二氧化鈦的大面積電沉積，並應用於鈣鈦礦模組之緻密層，相較於旋轉塗佈法，大面積電沉積的二氧化鈦薄膜具備較優良的均勻性且模組效能較高，此結果顯示電沉積二氧化鈦為一極具開發潛力之技術可用於大面積鈣鈦礦模組電子傳輸層之製備。

Abstract
TiO2 is widely employed in photovoltaic cells because of its suitable band position, good optical property and chemical stability. In this study, electrodeposited TiO2 system from aqueous TiCl3 solution and its relevant electrochemical kinetics is first investigated. It is found the morphology of electrodeposited TiO2 could be well-controlled by manipulating either deposited current or voltage and this finding becomes a cornerstone throughout the whole thesis. With this controllability, a series of studies of applying anodic electrodeposition (ED) TiO2 films as the electron-transporting material (ETL) in perovskite solar cells (PSCs) are conducted.
In chapter 4, a mossy and compact structure of TiO2 film is galvanostatically deposited and used as the compact layer (CL) in mesoporous-typed PSCs. In comparison with other three commonly used methods namely dip-coating (DC), spin-coating (SC) and spray-pyrolysis (SP), the ED could create a thin, pinhole-less and mossy-structured CL which not only inhibits the recombination reaction at the interface of FTO and perovskite efficiently, but also improves the contact between the CL and mesoporous scaffold (MS) due to its mossy structure.
In chapter 5, we report the compact and porous structure electrodeposited TiO2 layer can be sequentially deposited at different potential from a single bath. It is shown the morphology is densely compact at the low overpotential region (η < 0.15 V versus Ag/AgCl), which is located in the kinetic-controlled zone on the Tafel plot. On the other hand, the resultant TiO2 film become loosely porous when the overpotential is in the transition region of the kinetic-controlled and mass-transfer-controlled (η =0.15-0.25 V versus Ag/AgCl) zone on the Tafel plot. In contrast to conventional SC process, this procedure of electrodeposited TiO2 bilayer as an efficient ETL in PSCs is more time-saving and energy-saving.
In chapter 6, we add SnCl2 into pristine TiCl3 bath to electrodeposit Sn-doped TiO2 films from a single step. The effects of Sn on the electrical properties, absorption behavior, surface morphology and power conversion efficiency are systemically elucidated. The carrier concentration and surface morphology are significantly related to the Sn doping concentration. In this work, the 5% molar ratio Sn-doped TiO2 based PSCs shows better performance, which is due to the improved electron-extraction capability and conductivity in Sn-doped TiO2 ETLs.
In the last chapter, we upscale the ED system by designing a bi-functional container for the purpose to fabricate perovskite module. The uniformity of ED-TiO2 in large area deposition significantly outperforms the SC-TiO2. The ED-TiO2 provides a facile and potential method to fabricate an efficient large-area ETL for PSC modules.

Abstract    I
摘要    III
致謝    IV
Table of contents    V
Content of figures    VIII
Content of tables    XII
Chapter 1. General introduction    1
1-1.    Semiconductor introduction    1
1-2.    Electrodeposition of semiconductor    2
1-2-1.    Oxidation and reduction    3
1-2-2.    Electrodeposition of TiO2    4
1-2-3.    Application of electrodeposited TiO2 in solar cells    6
1-3.    Perovskite solar cells    7
1-3-1.    Mesoporous type    9
1-3-2.    Meso-superstructured type    10
1-3-3.    Planar type    11
1-4.    Electron-transporting layer in perovskite solar cells    12
1-4-1.    TiO2 Compact layer    12
1-4-2.    TiO2 Mesoporous scaffold layer    15
1-5.    Motivation of this study    16
Chapter 2. Materials, Equipment and Methodology    17
2-1.    Materials and chemical    17
2-2.    Equipment and methodology    19
2-2-1.    Equipment    19
2-2-2.    Methodology    19
Chapter 3.Fundamental study and experimental setup of electrodeposited TiO2 apparatus    28
3-1.    Introduction    29
3-2.    Experimental apparatus steup    30
3-3.    Kinetics of Electrode Reactions    31
3-4.    Results and Discussion    34
3-3-1.    Anodic TiO2 deposition mechanism    34
3-3-2.    Galvanostatic deposition    35
3-3-3.    Potentiostatic deposition    38
3-5.    Summary    40
Chapter 4. Galvanostatic deposition TiO2 film with mossy nanostructure as a compact layer for scaffold-type perovskite solar cells    41
4-1.    Introduction    42
4-2.    Experimental Section    43
4-2-1.    Compact layer preparation    43
4-2-2.    Perovskite solar cell fabrication    43
4-3.    Results and discussion    44
4-3-1.    Morphology of different CLs    44
4-3-2.    Optical and electronic properties    47
4-3-3.    Hole Blocking Properties    50
4-3-4.    Performance of PSCs    52
4-4.    Summary    61
Chapter 5. One-pot electrodeposition of compact layer and mesoporous scaffold for perovskite solar cells    62
5-1.    Introduction    63
5-2.    Experimental Section    64
5-3.    Results and Discussion    65
5-4.    Summary    71
Chapter 6. Co-electrodeposition of Sn-doped TiO2 electron-transporting Layers for Perovskite Solar Cells    72
6-1.    Introduction    73
6-2.    Experimental section    74
6-2-1.    Substrate and Sn-doped TiO2 preparation    74
6-2-2.    Perovskite solar cell fabrication    75
6-3.    Results and Discussion    76
6-3-1.    Kinetics of co-electrodeposited Sn-doped TiO2    76
6-3-2.    Morphology of different Sn-doped TiO2 film    77
6-3-3.    Characterization of Sn-doped ED-TiO2    79
6-3-4.    Performance of PSCs    85
6-4.    Summary    88
Chapter 7. Electrodeposited TiO2 films for perovskite modules    89
7-1.    Introduction    90
7-2.    Experimental section    93
7-2-1.    Design of the large area electrodeposited bath    93
7-2-2.    Perovskite module fabrication    94
7-3.    Results and Discussion    95
7-3-1.    Uniformity of large-area TiO2 film    95
7-3-2.    Modification of interconnection region (P1-P2-P3)    97
7-3-3.    Comparison the electrodeposited and spin-coated compact layer in perovskite module    98
7-4.    Summary    101
Chapter 8. Conclusion and Outlook    102
References    104
CV and Publications    114

                                

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