金屬硫族化合物奈米材料之合成與其太陽能電池應用

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研究生：	張恕豪 Chang, Shu-Hao
論文名稱：	金屬硫族化合物奈米材料之合成與其太陽能電池應用 Synthesis and Photovoltaic Applications of Metal Chalcogenide Nanomaterials
指導教授：	段興宇 Tuan, Hsing-Yu
口試委員:	周更生黃暄益吳文偉曾院介
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：	2014
畢業學年度：	102
語文別：	英文
論文頁數：	159
中文關鍵詞：	奈米材料、金屬硫族化合物、太陽能電池
外文關鍵詞：	Nanomaterials, Metal Chalcogenide, Photovoltaic
相關次數：	點閱：2 下載：0
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本論文主要研究金屬硫族化合物奈米材料之合成與其太陽能電池之應用。本論文分成四個部分: (1)三元素、四元素、五元素銅銦鎵硫硒(CuIn1-xGax(SySe1-y)2)奈米粒子合成與鑑定分析。(2) 銅鎵硫(CuGaS2) 奈米材料之大小、形狀、與晶體結構之控制。(3) 銅銦鎵硫硒類薄膜太陽能電池製備。(4)二元素金屬硫族奈米化合物米材料於染料敏化太陽能電池之應用。
三元素、四元素、五元素銅銦鎵硫硒合金奈米粒子合成採用熱溶劑升溫法，於高沸點溶劑中反應形成約15~30奈米之合金奈米化合物。此方法有別於熱注射法之合成，可大量生產奈米粒子，且大量生產之奈米粒子無論大小、形狀或光學性質與小量生產皆類似。銅銦鎵硫硒奈米粒子之可藉由改變前驅物的比例，控制奈米粒子之組成同時控制其能階，其大小可介於 0.98 eV~2.40 eV之間。另外，我們提出其理論計算，比較我們以儀器量測出之能階大小與理論計算之能階大小之差異。
銅鎵硫奈米材料可藉由實驗條件的改變，獲得不同大小、形狀與晶相之晶體。搭配粒徑選擇法(size-selection method)，不同大小之奈米粒子可被分離。隨著反應物與介面活性劑之不同，我們可以獲得不同晶相與不同形狀之晶體。我們同時藉由改變不同的反應溫度，探討其生長機制。
我們將銅銦鎵硫硒合金奈米粒子以各種常見的濕式塗佈方法，包括刮刀法、滴擲法與噴塗法將奈米粒子塗佈於基板上，並觀察其薄膜品質。最後我們選擇噴塗法將合成之奈米粒子塗佈於鉬玻璃基板上，配合後段製程如硒化、緩衝層製作、與上電極製作等步驟，將此奈米粒子應用於薄膜太陽能電池中。我們目前以五元素銅銦鎵硫硒合金奈米粒子做太陽能電池吸收層，最高效率已超過1.0 %。
二元素金屬硫族化物Co9S8奈米粒子與FeSe2奈米薄片被證明可應用於染料敏化太陽能電池對電極上。藉由非真空塗佈製程，包括噴塗法與電沉積法，金屬硫族化合物可塗佈於電極之上。透過電化學循環伏安法分析，我們可知此兩種材料對於I-/I3-電解液有良好催化性。並將以此兩種材料製備之對電極應用於染料敏化太陽能電池中，並獲得超過7 %轉換效率。

In this dissertation, we describe the synthesis and applications of metal chalcogenide nanocrystals. To give a clear picture of this dissertation, the main contents are summarized as follows: (1) Ternary, quaternary and quinary CuIn1-xGax(SySe1-y)2 nanocrystals were synthesized and investigated. (2) CuGaS2 nanomaterials were prepared with size, morphology and crystal phase control. (3) CuIn1-xGax(SySe1-y)2-based (CIGSSe-based) thin film solar cell preparation. (4) Binary metal chalcogenide nanocrystals for dye-sensitized solar cells (DSSC) applications.
We have developed a heating-up method to synthesize high quality nanocrystals. Using this method, 15~30 nm nanocrystals in oleylamine were synthesized and the quantity could be easily scaled up by this approach. The nanoparticles were analyzed by several instruments. The composition of nanoparticles can be tuned through the change of the element precursor ratios in the synthesis. The colloidal synthesis of quinary nanocrystals with entire composition tuning was achieved and band gap engineering could be tuned in the range from 0.98 eV to 2.40 eV. We have also characterized the band gap energy of CuIn1-xGax(SySe1-y)2 nanoparticles in both experimental and theoretical ways.
Size, shape and crystal phase of CuGaS2 nanomaterials can be manipulated by changing the experimental parameters. With the size-selection approach, different sizes of nanoparticles can be separated. By exploiting different reactants and capping agents, different shapes of nanomaterials were obtained. We also discussed the growth mechanism by changing the reaction temperature at the last part.
A variety of solution-based coating methods, such as spray deposition, dip-coating, and doctor blade coating have been applied for film deposition in this study. The qualities of thin films deposited from different methods were compared. Finally, CuIn1-xGax(SySe1-y)2 nanoparticles were coated on the Mo substrate by spraying deposition. After selenization process, buffer layer deposition, and top electrode sputtering, CuIn1-xGax(SySe1-y)2 nanocrystals as optical absorbing materials for solar cell devices were demonstrated. The devices had the cell efficiency over 1%, proving that these nanoparticles are promising precursors for photovoltaic devices.
Binary metal chalcogenides nanocrystals, Co9S8 and FeSe2, were proved to be the materials of counter electrode for DSSC. Through non-vacuum deposition methods, spray coating and electrophoretic deposition, binary metal chalcogenides nanocrystals can be deposited onto the conductive substrates. According to the analysis of cyclic voltammetry, Co9S8 and FeSe2 have good catalytic ability toward I-/I3- redox reaction. In addition, the DSSC assembled with Co9S8 and FeSe2 counter electrodes were demonstrated and the cell efficiencies of over 7 % were obtained.

Abstract    I
中文摘要    III
誌謝 V
Table of Contents    VI
List of Tables    IX
List of Figures    X
Chapter 1 Thesis Introduction    1
1    Introduction    1
2    Introduction on CIGS-Based Nanomaterials    5
2.1  Hot solvent methods    6
2.2    Hot-injection method    6
2.3    Heating-up method    7
2.4    Hydrothermal and solvothermal method (Autoclave method)    8
3 Introduction on CIGS-Based Thin Film Solar Cells    8
4 Introduction on Metal Chalcogenide Counter-Electrode for Dye-Sensitized Solar cells    13
5 Reference    15
Chapter 2 Synthesis of CIGS-Based Nanocrystals with Control of Physical and Optical Properties    18
1 Introduction    18
2 Experimental Section    19
2.1 Chemicals    19
2.2    Synthesis of CuIn(S1−xSex)2 nanocrystals    19
2.3    Synthesis of CuInxGa1-x(SySe1-y)2 nanocrystals    21
2.4 Characterization    22
3 Results and Discussion.    25
3.1 Quaternary CuIn(S1−xSex)2 nanocrysals    25
3.2 Quinary CuIn1-xGax(SySe1-y)2 nanocrystals    38
4 Conclusion    59
5 Reference    60
Chapter 3 Copper Gallium Sulfide (CuGaS2) Nanocrystals with Different Sizes, Crystal Phases, and Morphologies    65
1 Introduction    65
1.1 Size control of the CIGS-based nanomaterials    66
1.2 Shape control of nanomaterials    67
1.3 Phase control of nanomaterials    69
2 Experimental Section    70
2.1 Chemicals    70
2.2 Synthesis of 5.6 nm to 10.9 nm chalcopyrite type CuGaS2 nanocrystals    70
2.3 Synthesis of 3 nm chalcopyrite CuGaS2 nanocrystals    71
2.4 Syntheisis of wurtzite type CuGaS2 nanocrystals and nanowires    72
2.5 Characterization    73
3 Result and Discussion    75
3.1 Synthesis of chalcopyrite CuGaS2 nanocrystals    75
3.2 Synthesis of wurtzite CuGaS2 nanocrystals    80
4 Conclusion    88
5 Reference    89
Chapter 4 CIGSSe-Based Thin Film Solar Cells    95
1    Introduction    95
1.1 Particulate ink deposition    98
1.2 Molecular-level precursors deposition    100
2 Experimental Section    104
2.1 CIGSSe absorber layer deposition    104
2.2 CIGSSe-based thin film solar cell fabrication  105
2.3 Characterization    106
3 Result and Discussion    107
3.1 Drop-casting    108
3.2 Doctor blade coating    109
3.3 Spray coating    110
3.4 Solar cell fabrication    112
4 Conclusion    115
5 Reference    116
Chapter 5 Metal Chalcogenide Nanomaterials as the Counter-Electrode for Dye-Sensitized Solar Cell Applications    122
1 Introduction    122
1.1 Co9S8 Counter electrodes for DSSC applications    124
1.2 FeSe2 Counter electrodes for DSSC applications    126
2 Experimental Section    128
2.1 Chemicals    128
2.2 Cobalt sulfide nanocrystal synthesis    128
2.3 Counter electrode fabrication    129
2.4 Dye-sensitized solar cell assembly    130
2.5 Characterization and Measurement    131
3 Result and Discussion    133
4 Conclusion    150
5 Reference    151
Curriculum Vitae    157

                                

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Chapter 3
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Chapter 4
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17. Stolle, C. J.; Panthani, M. G.; Harvey, T. B.; Akhavan, V. A.; Korgel, B. A., Comparison of the Photovoltaic Response of Oleylamine and Inorganic Ligand-Capped CuInSe2 Nanocrystals. Acs Appl Mater Inter 2012, 4, 2757-2761.
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19. Todorov, T. K.; Gunawan, O.; Gokmen, T.; Mitzi, D. B., Solution-processed Cu(In,Ga)(S,Se)2 absorber yielding a 15.2% efficient solar cell. Progress in Photovoltaics: Research and Applications 2013, 21, 82-87.
20. Li, L.; Coates, N.; Moses, D., Solution-Processed Inorganic Solar Cell Based on in Situ Synthesis and Film Deposition of CuInS2 Nanocrystals. Journal of the American Chemical Society 2010, 132, 22
21. Uhl, A. R.; Fella, C.; Chirila, A.; Kaelin, M. R.; Karvonen, L.; Weidenkaff, A.; Borca, C. N.; Grolimund, D.; Romanyuk, Y. E.; Tiwari, A. N., Non-vacuum deposition of Cu(In,Ga)Se2 absorber layers from binder free, alcohol solutions. Prog Photovoltaics 2012, 20, 526-533.
22. Wang, W.; Han, S.-Y.; Sung, S.-J.; Kim, D.-H.; Chang, C.-H., 8.01% CuInGaSe2 Solar Cells Fabricated by Air-Stable Low-Cost Ink. Physical Chemistry Chemical Physics 2012.
23. Cho, A.; Ahn, S.; Yun, J. H.; Eo, Y.-J.; Song, H.; Yoon, K., Carbon layer reduction via a hybrid ink of binary nanoparticles in non-vacuum-processed CuInSe2 thin films. Sol Energ Mat Sol C 2013, 110, 126-132.
24. Lee, E.; Park, S. J.; Cho, J. W.; Gwak, J.; Oh, M. K.; Min, B. K., Nearly carbon-free printable CIGS thin films for solar cell applications. Sol Energ Mat Sol C 2011, 95, 2928-2932.
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Chapter 5
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