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研究生：	李瑩聰 Li, Ying-Tsung
論文名稱：	基板曲率、薄膜厚度以及氮氧氣體對於三層透明導電薄膜之光、電性質以及顯微結構之影響 Effects of substrate's radius of curvature, film thickness, and nitrogen/oxygen addition on electrical and optical properties and microstructure of triple layer thin films
指導教授：	林仁輝 Lin, Jen-Fin
學位類別：	碩士 Master
系所名稱：	工學院 - 機械工程學系 Department of Mechanical Engineering
論文出版年：	2019
畢業學年度：	107
語文別：	英文
論文頁數：	117
中文關鍵詞：	曲面石英玻璃、三層薄膜、薄膜厚度、光電性質、鋁氮共摻雜氧化鋅
外文關鍵詞：	Curved glass substrate, triple layer thin film, thin film thickness, optical and electrical properties, (Al,N) codoped ZnO
相關次數：	點閱：118 下載：2
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在第一個實驗中，根據田口式L9(33) 直交表製作九個試件用以探討三層氧化銦鎵鋅/銀/氧化銦鎵鋅鍍製於曲面基板之光學、電學性質以及顯微結構。在此實驗中氧化銦鎵鋅之厚度、銀層厚度、石英玻璃之曲率為實驗之三項變因。由實驗結果得知曲率之變化對於表面顆粒大小以及粗糙度有最大之貢獻率，並且曲率之增加會造成表面顆粒大小以及粗糙度之增加進而引起表面散射而造成載子遷移率之下降和電阻率之上升。然而，曲率之增加亦造成穿透率在 550 nm 波段之增加進而提升了Haack’s figure of merit (FOM)。銀層厚度之增加能夠顯著地提升載子濃度以及載子遷移率，並且提升藍光、綠光、紅光波段之反射率。由於Burstein-Moss effect之影響，載子濃度以及載子遷移率皆隨著氧化銦鎵鋅之厚度提升而增加。適當地選擇氧化銦鎵鋅之厚度、銀層厚度、石英玻璃之曲率能夠顯著提升 FOM。
在第二個實驗中，單層摻鋁氧化鋅以及三層摻鋁氧化鋅/銀/摻鋁氧化鋅之薄膜透過改變氮氣以及氧氣添加含量來探討對於光學、電學性質以及顯微結構之影響。當氮氣含量大於2.5 sccm 時，摻鋁氧化鋅薄膜之粒徑大小以及表面粗糙度會下降，然而殘留應力會增加。氧氣之添加對於鋁氧化鋅薄膜之粒徑大小、表面粗糙度、殘留應力有相同之影響，但是添加氧氣之薄膜會有相對於添加氮氣之薄膜較小之粒徑以及表面粗糙度。實驗結果顯示摻鋁氧化鋅之厚度會和單層以及三層薄膜之粒徑大小以及粗糙度成正相關，但是和殘留應力呈負相關之關係。試件D之三層薄膜有著60 nm厚之摻鋁氧化鋅，並且顯示出在所有試件中最強的抗反射效果。氮氣的添加可以型成p型之摻鋁氧化鋅薄膜，然而氧氣的添加會造成氧空缺之減少進而造成載子濃度以及載子遷移率之下降。在n型三層薄膜試件中，可以觀察到Burstein-Moss effect。

For the first experiment, nine specimens are prepared on the basis of the L9(33) orthogonal array design to evaluate the optical and electrical properties, morphology, and the microstructure of a-IGZO/Ag/a-IGZO (IAI) triple-layer composite films deposited on curved glass substrates with different radius of curvature efficiently. The experiments are arranged for the changes in three controlling factors, namely the IGZO and Ag thicknesses, and substrate’s radius of curvature. Radius of curvature has the highest contribution for the RMS surface roughness (SRq) and the mean particle size (PS). The carrier mobility (CM) and carrier concentration (CC) are proportional to each, irrespective of the controlling factor change in this study. An increase in the radius of curvature can result in the increases of SRq and PS, and therefore brings in a surface scattering effect which can cause the reduction of CM as well as the rise of resistivity (R). In addition, a sufficiently large radius of curvature can elevate the transmittance at 550 nm and Haack’s figure of merit (FOM) effectively, but it can lower the reflectance of blue, green and red. Via the carrier injections, increasing the Ag thickness can elevate the carrier mobility and concentration significantly. The reflectance for blue, green, and red are also risen by increasing the Ag thickness. As a result of Burstein-Moss effect, carrier concentration and optical bandgap are elevated by increasing the IGZO thickness. Additionally, the reflectance of blue, green, and red are also risen. Appropriate choices in the IGZO and Ag thicknesses and the radius of curvature can obtain the transmittance >80 %, and elevate the FOM significantly. For the second set of experiments, AZO and AZO/Ag/AZO (AAA) specimens are prepared by varying O2 and N2 flow rates to investigate the gas effects on the microstructure, and the optical and electrical properties. The AZO specimens are found to have the decreases in grain size and SRq, and an increase in the compressive residual stress when N2 flow rate increases higher than 2.5 sccm. The addition of O2 can contribute to a similar tendency for grain size, SRq and residual stress; the grain size and SRq are always smaller, while residual stress is larger than that prepared with N2. The thickness of AZO is proportional to the grain size and SRq, whereas it is inversely proportional to the residual stress of AZO, they are valid for both AZO and AAA thin films. Specimen D with 60-nm AZO thickness possesses the strongest anti-reflection effect of the AAA structure, and therefore suppresses the reflection from the Ag interlayer significantly. P-type conductivity is achieved by introducing the N2 into AZO layers. The carrier mobility and carrier concentration are lowered by increasing the amount of O2 because the oxygen vacancies are reduced. The Burstein-Moss effect is observed for the n-type AAA thin films where a decrease in optical bandgap along with an increase in carrier concentration is found for the p-type AAA films. Specimen D possesses the highest FOM value and relative high T at 550 nm because the 60-nm AZO can contribute to the strongest anti-reflection effect.

Table of Contents
Abstract………………………………………………………………………………Ⅱ
Acknowledgement………………………………………………………………….. Ⅵ
Table of Contents…………………………………………………………………... Ⅶ
List of Tables………………………………………………………………………...Ⅸ
List of Figures………….……………………………………………………..…..….Ⅹ

Chapter 1 - Introduction	1
1.1. Literature review	1
1.2. Motivations	4
1.3. Thesis writing methodology	6
Chapter 2 - Basic Theories	7
2.1. Introduction of TCOs	7
2.2. Deposition Method	8
2.2.1. Physical Vapor Deposition (PVD)	8
2.3. Theory of Residual Stress	8
2.3.1. Introduction of residual stress	8
2.3.2. The calculation of residual stress	9
2.4. Theory of grain size	10
2.5. Theory of electrical properties	10
2.5.1. Relationship between carrier mobility, carrier concentration, and resistivity	10
2.5.2. Theory of conducting mechanism for TCO/metal/TCO thin film	11
2.5.3. Theory of scattering	12
2.6. Theory of optical properties	12
2.7. Figure of merit	13
2.8. Theory of Taguchi method	13
2.9. Theory of Instrument	14
2.9.1. Theory of Scanning Electron Microscope	14
2.9.2. Theory of Transmission Electron Microscopy	14
2.9.3. Theory of Hall effect measurement	15
Chapter 3 - Experimental Details	22
3.1. Main objective	22
3.2. Specimens preparation	22
3.3. Experimental instruments	24
3.3.1. Co-sputtering system.	24
3.3.2. UV/Visible/NIR spectrophotometer.	24
3.3.3. Hall effect analyzer	24
3.3.4. Transmission Electron Microscopy (TEM)	25
3.3.5. X-ray Diffractometer (XRD)	25
3.3.6. Atomic Force Microscope (AFM)	26
3.3.7. Scanning Electron Microscope (SEM)	26
3.3.8. X-ray photoelectron spectroscopy (XPS)	26
Chapter 4 - Results and Discussions	37
4.1. The result of a-IGZO/Ag/a-IGZO triple layer thin film	37
4.1.1. Morphological analysis	37
4.1.2. Structural analysis	38
4.1.3. Electrical analysis	40
4.1.4. Optical analysis	41
4.1.5. Effect of substrate’s radius of curvature	41
4.1.6. Effect of Ag thickness	44
4.1.7. Effect of IGZO thickness	45
4.1.8. Figure of merit	46
4.2. The result of single layer AZO thin film	47
4.2.1. Structural analysis	47
4.2.2. Influence of nitrogen flow rate on microstructural properties	48
4.2.3. Influence of oxygen flow rate on microstructural properties	49
4.2.4. Influence of nitrogen and oxygen mixed flow rate on microstructural properties	50
4.2.5. Dependence of surface roughness, residual stress and grain size on the thin film thickness	51
4.2.6. TEM analysis	52
4.3. Results of AZO/Ag/AZO thin film with the AZO layers deposited with N2 and O2	53
4.3.1. Structural analysis of AZO/Ag/AZO thin films	53
4.3.2. Optical analysis of AZO/Ag/AZO thin films	54
4.3.3. Electrical analysis of AZO/Ag/AZO thin films	56
4.3.4. Figure of merit of AZO/Ag/AZO thin films	60
Chapter 5 - Conclusion	109
Reference	111

List of Tables
Table 2.1 Applications of TCOs materials…………………………………………...17
Table 3.1. The mixed gas flow rates for the deposition of single AZO layer………...27
Table 3.2. The mixed gas flow rates for the deposition of AZO layer for AZO/Ag/AZO triple layer thin film.………………………………………………………………….27
Table 3.3. Design of the controlling factor…………………………………………...28
Table 3.4. L9 (33) orthogonal table……………………………………………………28
Table 4.1. The morphological parameters for IGZO/Ag/IGZO specimens. …………61
Table 4.2. The surface roughness parameters for IGZO/Ag/IGZO specimens………62
Table 4.3. Electrical properties of the IGZO/Ag/IGZO thin films. ………………….63
Table 4.4. Optical properties of the IGZO/Ag/IGZO thin films……………………. 64
Table 4.5. The structural parameters for the single layer AZO specimens. …………65
Table 4.6. The structural parameters of the AZO layers for AZO/Ag/AZO triple layer specimens…………………………………………………………………….………66
Table 4.7. Optical properties for AZO/Ag/AZO specimens…………………………66
Table 4.8. Comparisons of the electrical properties of triple layer thin films……….67
Table 4.9. Electrical properties and FOM of specimens A-G………………………..67

List of Figures
Fig.2.1. Crystal structure of IGZO [43] ……………………………………………..18
Fig.2.2. (a) ZnO unit cell with Wurtzite structure (b) different types of crystal plans of ZnO Wurtzite structure [44] …………………………………………………..….….18
Fig.2.3. Thin film under tensile stress or compressive stress [45] …………….…….19
Fig.2.4. The carrier mobility of IGZO as a function of In2O3, Ga2O3, and ZnO [8]…...………………………………………………………………………………..19
Fig.2.5. Schematic representation of the electrical behavior of TCO/metal/TCO triple layer thin film [46]….. ………………………………………………………………20
Fig.2.6. The incident electron beam bombard on the specimen[42]…. ……………..20
Fig.2.7. Set up of Hall effect measurement…………………………………………..21
Fig.3.1. (a) Triple-layer thin films deposited on a curved glass substrate with the radius of curvature of (b) 35 mm, (c) 45 mm, (d) 55 mm. …………. ………………29
Fig.3.2. Steps of substrate cleaning.. ………………………………………………...30
Fig.3.3. Co-sputtering system………………………………………………………..31
Fig.3.4. Characterizations of thin film……………………………………………….32
Fig.3.5. The UV/Visible/NIR spectrophotometer…………………………………....33
Fig.3.6. Hall effect analyzer…. ……………………………………………………...33
Fig.3.7. Transmission Electron Microscopy (TEM)………………………………....34
Fig.3.8. Multipurpose X-ray Diffractometer (XRD)…. ……………………………..34
Fig.3.9. Atomic Force Microscope (AFM)…………………………………………..35
Fig.3.10. Scanning Electron Microscope (SEM)…………………………………….35
Fig.3.11. The X-ray photoelectron spectroscopy (XPS) system……………………..36
Figs.4.1.(a-i).The 3D surface morphology, RMS surface roughness, kurtosis, and skewness for specimen 1-9…………………………………………………………...72
Figs.4.2.(a-i) SEM images and histograms of specimen 1-9…………………………81
Figs.4.3 (a) Results of the kurtosis and skewness of particle size distribution as a function of mean particle size; (b) plot of skewness vs kurtosis for particle size distribution (c) variations of kurtosis and skewness with SRq…………….…………83
Fig.4.4. GID-XRD analyses of the IAI structures………………………………….....83
Fig.4.5. Cross-sectional TEM images for (a) specimens4, (b) 5, and (c) 6 and their SAED analyses for Ag and IGZO layer, respectively….………………………..……85
Fig.4.6. The correlation among Hall carrier mobility, resistivity, and carrier concentration of the IAI thin films…………………………………………………....86
Fig.4.7. The (a) Transmittance and (b) reflectance for 9 specimens in the visible light region….. …………………………………………………………………………….87
Fig.4.8. The absorption coefficient of IAI thin films on curved quartz slides as a function of bandgap energy….……………………………………………………….87
Fig.4.9. (a) Mean optical bandgap and mean particle size as a function of substrate’s radius of curvature; (b) mean resistivity as a function of mean SRq and mean optical bandgap with the variation of substrate’s radius of curvature………………………...88
Fig.4.10. The mean reflectance and transmittance as a function of substrate’s radius of curvature….…………………………………………………..………………………89
Fig.4.11. (a) Mean optical bandgap and mean carrier concentration as a function of IGZO thickness; (b) mean resistivity, carrier mobility, and carrier concentration as a function of IGZO thickness….……………………………………………………….90
Fig.4.12. The mean reflectance and transmittance as a function of Ag thickness……..91
Fig.4.13. (a) Mean optical bandgap and mean carrier concentration as a function of IGZO thickness; (b) mean resistivity, carrier mobility, and carrier concentration as a function of IGZO thickness…………………………………………………………...92
Fig.4.14. The mean reflectance and transmittance as a function of IGZO thickness……………………………………………………………………………...93
Fig.4.15. XRD patterns for the AZO single layer specimens 1-12…………………….94
Fig.4.16. (a). FWHM and grain size; (b) SRq and grain size; (c) lattice constant and residual stress as a function of nitrogen flow rate…………….………………………96
Fig.4.17. (a) FWHM and grain size; (b) SRq and grain size; (c) lattice constant and residual stress as a function of oxygen flow rate………………………………………97
Fig.4.18. (a) FWHM and grain size; (b)SRq and grain size; (c) lattice constant and residual stress as a function of nitrogen and oxygen mixed flow rate……………….99
Fig.4.19. Grain size, SRq, and residual stress for monolayer AZO thin film as a function of AZO thickness…. ………………………………………………………………....99
Fig.4.20. TEM images and SAED patterns for single layer AZO specimens (a) 1, (b) 5, and (c) 9…………………………………………………………………………..101
Fig.4.21. XRD patterns for the AZO/Ag/AZO triple layer specimens A-G. ………...101 
Fig.4.22. The grain size, RMS surface roughness, and compressive residual stress for the AZO/Ag/AZO thin films as a function of the AZO thickness……………………102
Fig.4.23. (a)Transmittance, (b) reflectance, and (c) absorptance spectrum for triple layer AZO/Ag/AZO specimens A-G…. …………………..………………………………103
Fig.4.24. Transmittance, reflectance, and absorptance of red, green, and average light regions for AZO/Ag/AZO triple layer specimens A-G…. …………………………105
Fig.4.25. The reflectance of AZO/Ag/AZO thin films as a function of AZO thickness…………………………………………………………………………….106
Fig.4.26. The absorptance coefficient of triple layer specimens A-G as a function of bandgap energy……………………………………………………………………...106
Fig.4.27. Carrier mobility, carrier concentration, and resistivity for triple layer specimens as a function of (a) N2 flow rate; (b) O2 flow rate; and (C) N2 and O2 mixed gas flow rate………………………………………………………………………....108
Fig.4.28. Optical bandgap as a function of carrier concentration……………………108

                                    

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