Photovoltaic Performance of p-type Dye-Sensitised Solar Cells Based on Solid and Flexible Electrode Systems

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研究生：	Habtamu Fekadu Etefa Habtamu Fekadu Etefa
論文名稱：	Photovoltaic Performance of p-type Dye-Sensitised Solar Cells Based on Solid and Flexible Electrode Systems Photovoltaic Performance of p-type Dye-Sensitised Solar Cells Based on Solid and Flexible Electrode Systems
指導教授：	今榮東洋子 Toyoko Imae
口試委員:	今榮東洋子王丞浩 Wei-Fang Su 陳志明
學位類別：	博士 Doctor
系所名稱：	應用科技學院 - 應用科技研究所 Graduate Institute of Applied Science and Technology
論文出版年：	2020
畢業學年度：	108
語文別：	英文
論文頁數：	149
中文關鍵詞：	氧化鎳、氧化鎳@碳點複合材料、碳點、PV測量、聚吡咯、功率轉換效率、染料敏化太陽能電池、入射光子轉換效率、比表面積、柔性電極、帶隙、氧化銦錫
外文關鍵詞：	Nickel oxide, PV measurement, carbon dot, nickel oxide@carbon dots composite, power conversion efficiency, dye-sensitized solar cell, Bandgap, Incident photon to current conversion efficiency, specific surface area, flexible electrode, polypyrrole, Indium tin oxide
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摘要
如今，由於世界各地具有不同的發展潛力，因此需要不同種類的可再生能源，例如地熱能、風能、波浪能、水力發電和光伏。太陽能是大自然的免費禮物，絕對是最容易獲得和最受歡迎的能源之一，其可以解決目前所面臨有限的化石燃料及其帶來公共衛生，環境污染等問題。光伏利用太陽的能量並將其轉化為電能。因此，染料敏化太陽能電池（DSSCs）的構造使從太陽中捕獲這種自由能成為可能。因此，我們選擇研究基於納米複合材料的光收集系統的改良和電荷分離，以將太陽能有效轉化為可再生能源的研究領域。進一步在這項研究中，研究了碳點（C-dot）對基於氧化鎳納米顆粒（NiO NPs）的DSSCs性能的影響及與N719染料共吸附在p型半導體上的碳點可協同提高太陽能電池的功率轉換效率。
碳點是主要的敏化劑， N719緊密吸附在碳點上，NiO充當正電子轉移的促進劑和電子-空穴複合的抑制劑。將方形（平均大小：11.4 x 16.5 nm）的NiO NP與由檸檬酸（CA）和乙二胺（EDA）合成的碳點混合。然後，使用由碳點與NiO NP的複合物（NiO @ 碳點）組成的光電陰極來測量DSSC的光伏性能。以1.5：1的EDA：CA摩爾比共吸附碳點含量為12.5 wt％的N719敏化劑進行吸附而製成的DSSC達到9.85％（在50m W / cm2的光下為430 nm的光源）功率轉換效率（PCE）。該PCE值遠大於對於分別不含碳點或N719而製備的NiO DSSC獲得的PCE值（2.44或0.152％），結果顯示通過碳點和N719的共同吸附的協同作用。基於NiO@碳點的DSSC的協同增效PCE是由於大量吸附在復合材料上的敏化劑具有較大的比表面積，以及NiO@碳點的工作電極中電荷轉移更快。另外，由於能量轉移，結合在NiO NP上的碳點縮短NiO NP的帶隙，並導致電極中更快的電荷分離。最重要的事實是碳點是主要的敏化劑，N719緊密吸附在碳點上，NiO充當正電子轉移的促進劑和電子-空穴複合的抑制劑。這些結果表明，碳點是DSSC中NiO NP的顯著增強劑，而NiO @碳點是DSSC中有希望的光伏電極材料。
在研究第二部分中，在（2,2,6,6-四甲基哌啶-1-基）氧基或（2,2,6,6-四甲基哌啶-1-基）氧羰基（TEMPO）-氧化的存在下纖維素納米纖維（TOCNF），氫氧化鎳（Ni（OH）2）是透過水熱合成法得到之。其成功地合成具有Ni（OH）2（CNF/Ni（OH）2）的纖維素納米纖維（CNF）和具有氧化銦錫（CNFmod/ITO NP）（光電陰極）的改良CNF作為工作電極（WE）基板。帶有吡咯（CNF @ PPY）的CNF（光陽極）由CNF和吡咯（Py）複合材料製成導電聚合物作為對電極（CE）。這兩種電極都是用於DSSC的新型柔性電極。用於WE的製造基板已用於裝載NiO NP和NiO@C-dots，它們有望取代DSSC系統中的ITO/PET或Pt/電極玻璃。我們優化了裝載在CNF/Ni（OH）2基底上的NiO NP的量（150 mg）。CNF/Ni（OH）2和CNFmod/ITO NP導電聚合物對DSSC顯示出了令人鼓舞的結果。與ITO/PET和ITO/玻璃基基材相比，CNF/Ni（OH）2和CNFmod/ITO NP的結果分別為1.25％和1.45％。因此，在進行其他修飾後，結果已顯示在DSSC系統中成功取代ITO/PET或Pt/玻璃電極。

Nowadays, since different parts of the world have different potentials, there is a need for different kinds of renewable energy sources such as geothermal, wind power, wave power, hydropower energy and photovoltaics (solar cells). Solar energy is a free gift of nature and is definitely one of the most accessible sources of energy that can be addressed a potential solution to the environmental issues resulting from the unsustainable use of fossil fuels. So that it is the most popular energy resource for that, it can be used in any of our everyday life. Photovoltaics use the energy of the sun and converts it into electricity. Therefore, the construction of dye-sensitized solar cells (DSSCs) made it possible to capture this free energy from the sun. In this thesis, the DSSC PCE and its materials applicability have studied. The improvement of light-harvesting systems and charge separation based on nanocomposites for efficient conversion of solar energy to renewable energy is an evolving area of study. Particularly, the effect of carbon dots (C-dots) on the performance of nickel oxide nanoparticles (NiO NPs) based DSSCs was explored in this work. Carbon dots co-adsorbing with N719 dye on p-type semiconductor synergetically enhance the power conversion efficiency of solar cells. Carbon dots are the main sensitizer, and N719 tightly adsorbed on carbon dots and NiO behaves as an accelerator of a positive electron transfer and a restrainer of the electron-hole recombination. The NiO NPs with a rectangular shape (average size: 11.4 x 16.5 nm) were mixed with C-dots, which were synthesized from citric acid (CA) and ethylenediamine (EDA). A photocathode consisting of a composite of C-dots with NiO NPs (NiO@C-dots) was then used to measure the photovoltaic performance of a DSSC. A DSSC fabricated via the adsorption of N719 sensitizer co-adsorbing with a C-dot content of 12.5 wt % at a 1.5:1 EDA: CA molar ratio was achieved a 9.85 % (430 nm of a light source at 50m W/cm2 light of intensity) of power conversion efficiency (PCE). This PCE value was far larger than the PCE value (2.44 or 0.152 %) obtained for a NiO DSSC prepared without the addition of C-dots or N719, respectively, indicating the synergetic effect by the co-adsorption of C-dots and N719. This synergetically higher PCE of the NiO@C-dots-based DSSC was due to the larger amount of sensitizer adsorbed onto the composites with a larger specific surface area and the faster charge transfer in the NiO@C-dots working electrode. In addition, the C-dots bound onto the NiO NPs shorten the bandgap of the NiO NPs due to energy transfer and give rise to faster charge separation in the electrode. The most important fact is that C-dots are the main sensitizer and that N719 tightly adsorbed on C-dots, and NiO behaves as an accelerator of a positive electron transfer and a restrainer of the electron-hole recombination. These results reveal that C-dots are a remarkable enhancer for NiO NPs in DSSCs, and that NiO@C-dots are the promising photovoltaic-electrode materials for DSSCs.
In the second part of this thesis, in the presence of (2,2,6,6-Tetramethylpiperidin-1-yl) oxyl or (2,2,6,6-tetramethylpiperidin-1-yl) oxidanyl (TEMPO)-oxidized cellulose nanofibers (TOCNF), nickel hydroxide (Ni(OH)2 has prepared hydrothermally. The cellulose nanofiber (CNF) with Ni(OH)2 (CNF/Ni(OH)2) & modified CNF with Indium Tin Oxide (CNFmod/ITO NP) (photocathode) were successfully synthesized as the working electrode (WE) substrates. CNF with polpyrrole (CNF@PPY) (photo-anode) Conductive polymer has prepared as the counter electrode (CE) from the CNF and pyrrole(Py) composite. Both of these electrodes introduced as the new type of flexible electrode for the dye-sensitized solar cells (DSSC). The fabricated substrate for WE has used for loading NiO NP and NiO@C-dots, which has expected to replace ITO/PET or Pt/glass of electrode in the DSSC system. The amount of NiO NP loaded on the CNF/Ni(OH)2 substrate was optimized (150 mg). The CNF/Ni(OH)2 and CNFmod/ITO NP conductive polymer has shown a promising results for DSSC. The obtained results 1.25 % and 1.45 % for the CNF/Ni(OH)2 and CNFmod/ITO NP respectively, were remarkable/competitive when compared with ITO/PET and ITO/glass based substrate. Thus, a promising results have been shown to replace instead of ITO/PET or Pt/glass electrode in the DSSC system, after additional modifications.

Table of contents
摘 要    i
Abstract    v
Acknowledgment    viii
Dedication    ix
Table of contents    x
List of figures    xiv
List of Acronym    xx
Chapter 1: Introduction    1
1.1. Background    1
1.2. Nano-materials in different field of studies.    2
1.3. Photovoltaic cells    3
1.4. Dye-Sensitized Solar Cells    4
1.4.1. Components and materials applied to DSSC    5
1.4.1.1. Sensitizer (N719 or cis-diisothiocyanato-bis(2,2'-bipyridyl-4,4'-dicarboxylato) ruthenium(II) bis(tetrabutylammonium))    5
1.4.1.2. Redox couples Electrolyte    7
1.4.1.3. Counter electrode: Platinum    8
1.4.1.4. Working electrode    8
Chapter 2: Review of Literature    11
2.1. Types of photovoltaic cells    11
2.1.1. Crystalline solar cells    11
2.1.2. Thin-film solar cells    11
2.1.3. Quantum dot solar cells    12
2.1.4. Perovskite solar cells    12
2.1.5. Hybrid Solar Cell    13
2.1.6. General overview of dye-sensitized solar cells    14
2.1.6.1. Current-voltage Characteristics    15
2.1.6.2. Nickel oxide semiconductor characteristics    16
2.1.7. Nanostructured metal oxide of DSSC    17
2.1.8. History of Carbon Nanomaterials    19
2.1.9.  Polyethylene terephthalate (PET) Flexible electrode    21
2.1.10. Cellulose and its composites    21
2.1.11. Research Motivation    22
Chapter 3: Enhanced Photosensitization by Carbon Dots Co-Adsorbing with Dye on p-Type Semiconductor (Nickel Oxide) Solar Cells.    25
3.1. Introduction    25
3.2. Experimental    27
3.2.1. Reagents    27
3.2.2. Synthesis of composites of C-dots with NiO NPs (NiO@C-dots)    27
3.2.3. Characterization    29
3.2.4. Measurements of photocurrent (I-V) and electrochemical impedance spectra and incident monochromatic photon-to-current conversion efficiency.    30
3.2.5. Measurements of adsorption amount of dyes    32
3.3. Results and discussion    32
3.3.1. Characterization of materials    32
3.4. DSSC performance    38
3.5. Effect of carbon dots    42
3.6. Conclusions    58
Chapter 4: A New Design of the Flexible Substrate as a Cathode electrode Semiconductor for Dye-Sensitized Solar Cells Based on Cellulose Nano-fiber Composites.    60
4.1. Introduction    60
4.1.1. Motivation    61
4.2. Experimental    62
4.2.1. Reagent    62
4.2.2. Synthesis of TEMPO-Oxidized Cellulose Nanofiber (TOCNF)    63
4.2.3. Synthesis of nickel oxide nanowires (NiONW)    64
4.2.4. Synthesis of Composite composed of TOCNF and Polypyrrole (PPy) (TOCNF@PPy film)    65
4.2.5. Synthesis of Indium tin oxide nanoparticles (ITO NPs)    65
3.2.6. Cellulose nanofiber film surface treated using Octadecylamine (ODA)    66
4.2.7. Characterization measurements    67
4.2.8. Eelectrochemical measurement    68
4.2.8.1. Preparation of TOCNF/Ni(OH)2, TOCNF/Ni(OH) 2@NiONP, TOCNF/Ni(OH) 2/NiO@C-dots) and TOCNF/Ni(OH) 2/NiO@C-dots/NiONW composite film.    68
4.2.8.2. Measurements of electrochemical impedance spectra of TOCNF and TOCNF@PPY    69
4.2.8.3. Assembling the electrode for Dye-sensitized Solar Cells (DSSCs) and its measurement    70
4.3. Result and discussion    70
4.3.1. Characterization of materials    70
4.3.2. Photo-electrochemical performance measurement    75
4.3.3. Current-Voltage measurement performance of DSSC.    79
4.3.4. Impact of NiONP@Cdots deposition on TOCNF/Ni(OH)2 substrate electrode for photo-electrochemical properties.    81
4.3.5. The performance of NiONP@Cdots based on ITO/PET substrate for photo-electrochemical properties.    90
Chapter 5: General Conclusions and future prospective    99
REFERENCE    102
Appendix    125

List of figures
Figure 1: Application of nanostructured and composite materials in energy    3
Figure 2. Photovoltaic effect.    4
Figure 3.The different binding modes for the anchoring group on the NiO surface.    7
Figure 4.Schematic working  Principle of DSSC(P-type)    9
Figure 5. Thin-film solar cells Structure    12
Figure 6. Donor and acceptor energy diagram.    14
Figure 7. I-V characteristics of a DSC device    16
Figure 8. Carbon dots potential applications and their properties in different areas.    20
Figure 9. Eenergy level diagram showing the favorable influence of Green-C-dots as a sensitizer in the photo-anode.    Error! Bookmark not defined.
Figure 10. Preparation of nickel oxide nanoparticles (NiO NPs)    28
Figure 11. Preparation of carbon dots (C-dots)    Error! Bookmark not defined.
Figure 12. Preparation of composites of C-dots with NiO NPs (NiO@C-dots)    29
Figure 13. (Top) TEM images and (bottom) size distribution histograms of NiO NPs and NiO@C-dots.    33
Figure 14. EDS spectra of C-dots@NiO at different (1:1, 1.5:1 and 2:1 of EDA/CA mole ratio).    Error! Bookmark not defined.
Figure 15. FT-IR absorption spectra of NiO NPs, C-dots and NiO@C-dots and (B) XRD spectra of NiO NPs and NiO@C-dots.    35
Figure 16. XPS survey spectra and XPS fine and deconvoluted spectra of C1s, N1s, O1s, Ni2p3/2 and Ni2p1/2 of NiO NPs and NiO@C-dots.    37
Figure 17. I-V curves and calculated electrochemical parameters of NiO@C-dots DSSCs at 1:1 EDA:CA mole ratio at different C-dot contents and sensitizers. Numerals in I-V curves indicate C-dot contents in wt% unit.    Error! Bookmark not defined.
Figure 18. I-V curves and calculated electrochemical parameters of NiO@C-dots DSSCs at different EDA/CA mole ratios at 12.5 wt% C-dot content. Numerals in I-V curves indicate the EDA/CA mole ratio.    41
Figure 19 (A) Nyquist Plots and (B) Bode phase plots of EIS of NiO@C-dots (a) at different C-dots contents at 1:1 EDA: CA mole ratio and (b) at different EDA/CA mole ratios at 12.5 wt% C-dots content. Numerals indicate (a) C-dots content in wt% and (b) EDA/CA mole ratio. (C) Plots of ohmic series resistance, charge transfer resistance and electron lifetime as a function of EDA/CA mole ratio.    42
Figure 20. (A) Tauc’s plots of UV-visible absorption spectra of NiO@C-dots and (B) plots of bandgap (a) at different C-dot contents (at 1:1 EDA: CA mole ratio) and (b) at different EDA/CA mole ratios (at 12.5 wt% C-dot content). Numerals in Tauc’s plots indicate (a) C-dot content in wt% and (b) EDA/CA mole ratio.    45
Figure 21. UV-Vis absorption and PL spectra of aqueous dispersions of NiO, NiO@C-dots and C-dots at concentrations of 0.2 mM. (Red) excitation spectrum and (black) emission spectrum.    48
Figure 22. (A) N2 adsorption-desorption isotherms of NiO@C-dots and (B) plots of parameters from isotherms (a) at different C-dots contents (at 1:1 EDA/CA mole ratio) and (b) at different EDA/CA mole ratios (at 12.5 wt% C-dots content). Numerals in isotherms indicate (a) C-dots content and (b) EDA/CA mole ratio.    49
Figure 23. Adsorption amounts of N719 on NiO@C-dots (a) at different C-dots contents (at 1:1 EDA:CA mole ratio) and (b) at different EDA/CA mole ratios (at 12.5 wt% C-dots content).    50
Figure 24. (A) IPCE plots, (B) UV-visible absorption spectra of ethanol solutions and (C) Infrared absorption spectra of (a) NiO@C-dots/N719 (at 12.5 wt% C-dots content and 1.5:1 EDA:CA molar ratio) and (b) NiO/N719 DSSCs and (c) N719.    53
Figure 25. A schematic illustration of a NiO/C-dots/N719 solar cell.    56
Figure 26. Preparation of TOCNF film    64
Figure 27. Preparation of nickel Oxide nanowire (NiONW)    64
Figure 28. Preparation of TOCNF@PPy film for counter electrode.    65
Figure 29.Contact angle of modified CNF at d/t weight of Octadecylamine (ODA) (A) 2.2 mg (B)3.3 mg and (C) 4.4 mg.    67
Figure 30.NiONP, NiONP@C-dots and NiONP@C-dots/NiONW deposited on the CNF/Ni(OH)2 substrate    69
Figure 31. A) The TEM image of NiO NW at different concentrations of Na2CO3. B) FE-SEM morphology of NiO NW (at 2.94 M Na2CO3).Where L- length and D-diameter    71
Figure 32. FT-IR of TOCNF, Ni(OH)2, TOCNF/Ni(OH)2 @NiONP, and TOCNF/Ni(OH)2 /NiONP@C-dots (B) Indium tin oxide nanoparticles (ITO NPs).    72
Figure 33. XRD of a) NiO NW b) CNF-NiONW/NiONP@C-dots c) CNF-NiONW@NiONP and d) TOCNF    75
Figure 34.The transient photocurrent responses of (A) CNF@Ni(OH)2 film at the different mass of nickel chloride (NiCl2, a s the precursor) (B). CNFmod/ITO NP at different weight of ODA a) 2.2 mg b) 3.3 mg c) 4.4 mg. (C) The comparison different electrodes a) NiO@C-dots/ ITO glass b) NiONP/ITO glass c) ITO/glass d) CNF/Ni(OH)2. (D) photo-current response of (a) NiO@C-dots/ITO/PET (b) NiO/ITO/PET (c) ITO/PET.    78
Figure 35. (A) Nyquist Plots of EIS of Ni(OH)2 (green on ITO glass), NiONW (red on ITO glass), CNF@Ni(OH)2 film (blue) CNF@Ni(OH)2/NiO NP@C-dots film (black).  (B) CV measurement of TOCNF/PPY at different micro litter (μL) of pyrrole (PY).    79
Figure 36. The I-V performance of DSSC NiO NP based on the TOCNF/Ni(OH)2 substrate at the different mass of NiO NP deposited on the substrate as a photocathode.    81
Figure 37. I-V performance of NiO NP@C-dots in DSSC based on the TOCNF/Ni(OH)2 substrate at 150 mg NiO NP mass and at various weights of C-dots as a working electrode deposited on the substrate.    83
Figure 38. I-V measurement of substrate, at different wt% of ITO deposited on CNF/Ni(OH)2 substrate.    85
Figure 39.(A) Transmission of dried CNF film, untreated and treated (B) Tauc’s plots of UV-visible absorption spectra of ITO NP.    87
Figure 40. I-V curve DSSC performance of NiO NP@C-dots/NiO NW based on the TOCNF/Ni(OH)2 substrate as the photocathode at different Wt% of NiO NW added to NiONP@C-dots.    88
Figure 41. I-V curve DSSC performance of (a) CNFmod/ITO NP substrate (b) CNFmod/ITO NP/NiO NP and (c) CNFmod/ITO NP/NiO NP@C-dots.    90
Figure 42.The I-V curves of NiO DSSC and its electrochemical parameters at different content of C-dot and at 1:1 EDA / CA molar ratios.    91
Figure 43.The I-V curves of NiO@C-dots DSSC and its electrochemical parameters at different content of C-dot and at 1:1 EDA / CA molar ratios.    93
Figure 44.The I-V curves of NiO@C-dots DSSC and its electrochemical parameters at 12.5 wt% C-dot content in various EDA / CA molar ratios.    95
List of Tables
Table 1.  Binding energies (BE), their area intensities and their assignments from XPS of NiO NPs and NiO@C-dots.    38
Table 2. Electrochemical parameters calculated from I-V curves of NiO@C-dots DSSCs in Figure 17 (A) at different C-dot contents at 1:1 EDA:CA mole ratio and (B) at different EDA:CA mole ratios at 12.5 wt% C-dot content. Experiments were performed under 430 nm blue LED light excitation with 50 mWcm-2.    40
Table 3. Parameters obtained from EIS, Tauc’s plots, N2 adsorption-desorption isotherms and N719 adsorption of NiO@C-dots (A) at different C-dot contents (at 1:1 EDA:CA mole ratio) and (B) at different EDA:CA mole ratios (at 12.5 wt% C-dot content).    43
Table 4. PL bands of NiO, C-dots@NiO and C-dots    46
Table 5. Comparison of semiconductor solar cells PCE co-adsorbed by quantum dots and N719.    57
Table 6. FT-IR absorption bands of TOCNF, Ni(OH)2, TOCNF/Ni(OH)2 @NiONP, and TOCNF Ni(OH)2 /NiONP@C-dots.    73
Table 7.The DSSC performance of NiO NP based on the TOCNF/Ni(OH)2 substrate as the photocathode    81
Table 8. The DSSC performance of NiO NP@C-dots based on the TOCNF/Ni(OH)2 substrate as the photocathode.    83
Table 9. DSSC parameters values of CNF/Ni(OH)2/ITO substrates at different wt% of ITO Np deposited.    86
Table 10.The DSSC performance of NiO NP@C-dots/NiO NW based on the TOCNF/Ni(OH)2 substrate as the photocathode at different Wt% of NiO NW added to NiONP@C-dots.    89
Table 11.The calculated DSSC performance of different parameters based on the CNF mod/ ITO NP substrate as the photocathode    89
Table 12.NiO NPs Photovoltaic Performance in DSSCs Parameters based on the ITO/PET Substrates treated at different temperature.    92
Table 13.NiO@C-dots Electrochemical Photovoltaic Performance in DSSCs Parameters based on the ITO/PET Substrates determined from I-V curves in Figure 43 (A) for different C-dot content at 1:1 EDA: CA molar ratio and Figure 44 (B) for different EDA: CA molar ratios at 12.5 wt% C-dot content.    94
Table 14. Comparison of PCE performance DSSC Flexible electrode in different materials based on the non-commercialized CNF/ Ni(OH)2 substrate and commercialized substrate.    97


                                

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