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研究生：	蔡秉樺 Tsai, Ping-Hua
論文名稱：	金屬氧化物電荷傳輸層製作量子點電致發光二極體之研究 Investigation of Electroluminescent Quantum Dot Light-Emitting Diodes with Metal-Oxide Carrier Transport Layers
指導教授：	蘇炎坤 Su, Yan-Kuin
學位類別：	碩士 Master
系所名稱：	電機資訊學院 - 微電子工程研究所 Institute of Microelectronics
論文出版年：	2013
畢業學年度：	101
語文別：	英文
論文頁數：	66
中文關鍵詞：	金屬氧化物、電致發光、量子點、量子點發光二極體
外文關鍵詞：	metal oxides, electroluminescence, quantum dots, quantum dot light-emitting diodes
相關次數：	點閱：133 下載：7
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在本論文中主要使用無機金屬氧化物作為多層結構中的電荷傳輸層並與無機硒化鎘/硫化硒-核/殼型量子點製作反置型量子點電致發光二極體。該元件基本架構為氧化銦錫(ITO)/氧化鋅(ZnO)/緩衝層/量子點(QDs)/4,4'-二(9-咔唑)聯苯(CBP)/三氧化鉬(MoO3)/金(Au)。本實驗中所有元件皆製作於玻璃基板上，氧化銦錫當作陰極，並運用不同製程方式製作氧化鋅作為電子傳輸層，而結構中緩衝層主要利用碳酸銫來製作，紅光發光層材料則為溶膠狀量子點，熱蒸鍍有機材料CBP作為電洞傳輸層，電洞注入層則為三氧化鉬，最後鍍上功函數較高的金來當作陽極。
傳統量子點發光二極體結構大多以有機聚合物作為電洞傳輸層材料，製作於陽極與量子點之間，由於溶膠狀量子點多分散於有機溶劑(甲苯、氯仿)之中，而有機溶劑大多會對其他薄膜造成破壞，為使得電洞傳輸介面品質不受到影響，其材料的選擇性受到限制，導致不同材料中電洞之位能障礙成為主要影響元件效率的關鍵，因此我們採用了新式的反置結構來製作量子點發光二極體。以穩定的金屬氧化物-氧化鋅作為量子點薄膜下方之電子傳輸層，如此一來便可使用與量子點之間電洞能障較小的有機材料CBP來當作電洞傳輸層，並搭配強鹼型金屬化合物作為緩衝層來改善元件效率，使元件增加了約135倍的亮度而效率也提升了將近38倍。接著我們運用溶膠凝膠法、濺鍍法、氧化鋅奈米粒子三種不同方式製作電子傳輸層，經量測比較後發現，使用溶膠凝膠法製作非結晶氧鋅薄膜作為電子傳輸層可達到最佳元件特性。有鑑於此，我們對溶膠凝膠法製作之氧化鋅薄膜施以不同回火溫度，於回火溫度200 ℃時元件達到最大亮度195 cd/m2以及最佳電流效率0.039 cd/A。
我們成功地製作出像素均勻的紅光量子點電致發光二極體，結構中運用簡易、低成本溶膠凝膠法製作氧化鋅薄膜作為電子傳輸層和高色彩純度的發光材料量子點。相較於有機聚合物作為電荷傳輸層的傳統結構，起始驅動電壓由原本的6.5伏特下降了13.85%至5.6 V，而最大電流效率也從原本的0.029 cd/A上升34.48 %到達將近0.04 cd/A。

In this thesis, the inorganic metal oxides as carrier transport layers in multilayer structure and the inorganic CdSe/ZnS core/shell type quantum dots (QDs) were mainly employed to fabricate the inverted electroluminescent quantum dot light-emitting diodes (QD-LEDs). The concept structure was indium tin oxide (ITO)/zinc oxide (ZnO)/buffer layers/QDs/4,4'-Bis(carbazol-9-yl)biphenyl (CBP)/ molybbdenum(VI) oxide (MoO3)/gold (Au). All of the devices were fabricated on the transparent glass substrates. ITO was cathode, and ZnO was used as electron transport layers (ETLs). The cesium carbonate (Cs2CO3) was buffer layers while QDs were red light-emitting materials, and CBP was hole transport layer (HTL). Moreover, MoO3, and Au with high work function were used as hole injection layer (HIL), and anode, respectively.
Traditional structure have made use of the polymer materials to be hole transport layer inserted between QDs and anode. Colloidal quantum dots were dispersed in organic solvent, such as toluene or chloroform. Thus, the material selection of hole transport layer must be limited to prevent the damage of QDs and polymer, leading to the difficult confronting of hole barrier. As a result, a novel inverted structure was used to fabricate our QD-LEDs. Air-stable and inorganic metal oxides (ZnO) were employed to be the tolerant ETLs against the QD solution. Therefore, we chose the CBP material with lower highest occupied molecular orbital (HOMO) for diminishing the hole barrier height between QDs and HTLs. Due to the cooperation of ZnO and alkali metal compounds in QD-LEDs, the luminance intensity and current efficiency would be significantly increased by approximately 135 and 38 times, respectively. There were three different fabrication methods, such as sol-gel method, sputtering, and ZnO nanoparticles to be used to deposit ETLs. By X-ray diffraction (XRD) spectrum, the amorphous crystallinity could be detected in the ZnO thin film deposited by sol-gel method and QD-LEDs using this deposition method showed the best performance. Moreover, by means of treating sol-gel-derived ZnO layers with different annealing temperature, we found that the maximum luminance and current efficiency of the device could reach levels of 195 cd/m2 and 0.039 cd/A, respectively, at 200 ℃ treatment.
Eventually, we have successfully fabricated the red light electroluminescent QD-LEDs with uniform pixels, and the device especially contain the easy and low-cost sol-gel-derived ZnO and QDs with high color purity. From the comparison with inverted and conventional polymer-based structure, the turn on voltage for inverted structure with respect to normal structure device decreased from 6.5 to 5.6 V by 13.85 % and the maximum efficiency raised from 0.029 up to approximately 0.04 cd/A by 34.48 %.

Content
Abstract (in Chinese)	I
Abstract (in English)	III
Acknowledgement	V
Content	VI
Table captions	VIII
Figure captions	IX
Chapter 1 Introduction	1
1.1 Colloidal quantum dots	1
1.2 Colloidal quantum dots for light-emitting device	2
1.3 Properties of metal oxides	3
1.4 Motivation	4
References-Chapter 1	5
Chapter 2 Theory of quantum dot light-emitting diodes	8
2.1 The characteristics of organic materials and quantum dots	8
2.1.1 Fluorescence and Phosphorescence	8
2.1.2 Quantum dots as exciton acceptors	11
2.2 Mechanisms of quantum dot light-emitting diodes	13
2.2.1 Energy transfer vs. charge injection	13
2.2.2 Classification of four QD-LEDs types	14
2.3 Zinc oxide (ZnO) sol-gel method	17
References-Chapter 2	19
Chapter 3 Experimental processes and measurements	24
3.1 Materials in the experiments	24
3.2 Substrate treatment	28
3.3 Fabrication process	29
3.4 Measurement and characteristics analysis	32
References-Chapter 3	35
Chapter 4 Experimental results and discussions	36
4.1 The effect of cesium carbonate (Cs2CO3) on QD-LEDs 	36
4.2 Comparison of different ZnO preparations in QD-LEDs	42
4.2.1 Analysis of ZnO films (amorphous and crystalline)	42
4.2.2 Electronic characteristics	45
4.3 Comparison of ZnO with different annealing temperature	51
4.3.1 Analysis of ZnO films	51
4.3.2 Electronic characteristics	55
4.3.3 Comparison of inverted and traditional structure	59
References-Chapter 4	61
Chapter 5 Conclusion and future work	65
5.1 Conclusion	65
5.2 Future work	66

Table captions
Table 4-1: The turn on voltage at 100 mA/cm2, luminance at 8 V, maximum current efficiency, and wavelength of maximum EL peak at 3 mA of all devices	41
Table 4-2: The turn on voltage at 100 mA/cm2, maximum luminance, maximum current efficiency, and wavelength of maximum EL peak at 3 mA of all devices	50
Table 4-3: The turn on voltage at 100 mA/cm2, maximum luminance, maximum current efficiency, and wavelength of maximum EL peak at 3 mA of all devices 	58
Table 4-4: Comparison of the turn on voltage at 100 mA/cm2, maximum luminance, maximum current efficiency, and wavelength of maximum EL peak at 3 mA	60

Figure captions
Fig. 1-1 Market research of QD-based products	2
Fig. 2-1 Process of radiative energy transfer	9
Fig. 2-2 Process of Förster energy transfer	10
Fig. 2-3 Process of Dexter energy transfer	10
Fig. 2-4 The schematic diagram of excited QD states	11
Fig. 2-5 Schematic diagram illustrates two proposed mechanism of QD-LED operation. (a) Schematic structure, (b) energy band diagram of general QD-LED	14
Fig. 2-6 Progression of QD-LED performance over time in terms of peak EQE and the inset are four architecture types	14
Fig. 3-1 Absorption and PL spectra of the QDs film	26
Fig. 3-2 Photolithography process for the patterned ITO-glass substrates	28
Fig. 3 3 Cleaning process for the patterned ITO-glass substrates	28
Fig. 3 4 The flow chart of the procedure for preparing ZnO layers	29
Fig. 3 5 Photographs of the thermal vacuum evaporation system	31
Fig. 3 6 Chamber of the thermal evaporation system	31
Fig. 3 7 Different patterns for (a) ITO, (b) buffer/ organic layer, (c) Gold (Au)	32
Fig. 3 8 Measurement systems of optical and electrical characteristics	33
Fig. 3 9 Agilent 8453 UV-Vis spectrophotometer	34
Fig. 3 10 Measurement system of PL spectra for sample solutions	34
Fig. 4-1 (a) Scheme of QD-LEDs with buffer layers, (b) energy band diagram	37
Fig. 4-2 Current density-voltage characteristics	38
Fig. 4-3 (a) Luminance-voltage, (b) current efficiency-current density curves	40
Fig. 4-4 EL spectra of the five devices biased at 3 mA	41
Fig. 4-5 Scheme of QD-LEDs with different preparations of ZnO	43
Fig. 4-6 XRD spectra of sol-gel-derived ZnO films	43
Fig. 4-7 AFM and SEM of (a) ZnO (non-crystalline), (b) ZnO (crystalline)	44
Fig. 4-8 Current density-voltage characteristics	45
Fig. 4-9 (a) Luminance-voltage, (b) current efficiency-current density curves	47
Fig. 4-10 EL spectra of (a) all devices, (b) normalization of device E and F, inset is the PL of organic CBP	49
Fig. 4-11 TEM of ZnO nanoparticles (a) fresh, (b) store for days	50
Fig. 4-12 Scheme of QD-LEDs with different annealing temperature of ZnO	51
Fig. 4-13 Spectra of (a) absorbance, (b) transmittance (normalized to glass)	53
Fig. 4-14 XRD spectra of different annealing temperature ZnO	54
Fig. 4-15 AFM images of different annealing temperature ZnO	54
Fig. 4-16 Current density-voltage characteristics	55
Fig. 4-17 (a) Luminance-voltage, (b) current efficiency-current density curves	57
Fig. 4-18 EL spectra of the devices with ZnO annealed from 100 ℃ to 400 ℃	58
Fig. 4-19 Schematic and energy band diagrams of (a) inverted, (b) conventional structure	60

                                    

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