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研究生：	施若梅 Rosmaidah, Stella
論文名稱：	溫度效應對於AZO透明導電膜品質之影響 Effect of annealing temperatures on the quality of Al doped ZnO thin film characteristics prepared by sol-gel method
指導教授：	賴啟銘 Lai, Chi-Ming
學位類別：	碩士 Master
系所名稱：	工學院 - 土木工程學系 Department of Civil Engineering
論文出版年：	2011
畢業學年度：	99
語文別：	英文
論文頁數：	116
中文關鍵詞：	氧化鋅-鋁、快速熱退火、溶膠凝膠法、奈米壓痕、光譜儀、X光繞射、殘留應力
外文關鍵詞：	Al-ZnO (AZO) thin film, rapid thermal annealing (RTA), sol-gel method, nanoindentation, SEM, spectrophotometer, XRD, GIXRD, residual stress
相關次數：	點閱：147 下載：3
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薄膜沉積過程中，常因薄膜與基板界面晶格不匹配，造成殘留應力導致薄膜損壞。本研究利用溫度效應降低於製備薄膜過程中所產生之殘留應力。並採用溶膠凝膠法(sol-gel)方式製備AZO薄膜。
本研究分別利用350℃、450℃、600℃三種不同溫度值，來進行AZO薄膜於物理、光學和結構等性質的探討。首先，利用奈米壓痕試驗來求得薄膜之機械性質，接著使用SEM觀察薄膜結構於不同溫度下其晶體成長情形，而對於光學性質的探討則使用分光光譜儀。最後，採用X-Ray方式來分析薄膜殘留應力。
實驗結果顯示出隨著熱處理溫度上升，薄膜楊氏係數和硬度值隨之增加，且晶粒成長過程結晶性質較好，亦即尺寸越大。然而，薄膜厚度和剪應力則會隨著熱處理溫度增加而遞減。對於薄膜應力在經過這三種不同熱處理溫度實驗後，不論在張應力和壓應力的結果，均會隨著薄膜厚度的增加而逐漸地降低。由本研究最後的結果可以發現到較高的熱處理溫度確實可以有效地降低薄膜殘留應力。

Rapid thermal annealing (RTA) method has been successfully minimized the residual stress formed in AZO thin film due to the lattice mismatch between the films and the substrate. In brief, AZO thin films were synthesized on glass substrate by using sol-gel method.
In this work, three different RTA temperatures were used to study about the physical, optical, and structure of the AZO thin film. The RTA temperatures were varied as 350oC, 450oC, and 600oC. The physical properties of AZO thin film were analyzed by nanoindentation method. The film structure was analyzed by SEM. Spectrophotometer was used to determine the optical properties of the film. Finally, XRD and GIXRD method were used to analyze the film stress.
The results show that the increasing of RTA temperature increases the Young’s modulus and hardness of the films. The grain size of the films also increases with increasing of RTA temperature. However, the film thickness and shear stress component decrease with increasing of RTA temperature. Both compressive and tensile stress decreases gradually with increasing the film thickness after RTA treatment. It can be seen that higher RTA temperature can effectively relax the residual stress.

TABLE OF CONTENTS
ACKNOWLEDGEMENTS	I
ABSTRACT……………	II
摘要……………	III
TABLE OF CONTENTS	IV
LIST OF TABLES	VIII
LIST OF FIGURES	IX
CHAPTER I INTRODUCTION	1
1.1 	Research Background	1
1.2 	Objectives	2
1.3 	Thesis Structure	3
CHAPTER II LITERATURE REVIEW	4
2.1 	Sol-Gel Method	4
        2.1.1 Sol-gel Hydrolysis and Polycondensation Reactions 5
              2.1.1.1 The Sol-Gel Process With Organic Salt as Precursor 5
              2.1.1.2 The Sol-Gel Process With Inorganic Salt as Precursor 5
        2.1.2 	Coating	7
	        2.1.2.1 Dip Coating Process Theory 7
	        2.1.2.2 Spin Coating Process Theory 8 
2.2 Effect of Rapid Thermal Annealing (RTA)10
2.3 Nanoindentation Measurements	14
        2.3.1 	Nanoindentation Structure 15
	2.3.2	Nanoindentation Characteristic of The Diamond Probe 16
	2.3.3 	Basic Theory of Nanoindentation 16
2.4 	Scanning Electron Microscopy (SEM) 	20
2.5 	The Optical Characteristic Measurements	24
        2.5.1 	Spectrophotometer	24
        2.5.2 	The Four-point Probe25
2.6 	The Theory and Application of X-ray Diffraction	27
	2.6.1	X-Ray Diffraction (XRD)	27
	2.6.2	Basic Crystallography   29
	2.6.3	Reciprocal Lattice Space32
	2.6.4	XRD Analysis for Al-Doped ZnO Thin Film	33
2.7 The Phase Transition From Amorphous to Crystalline of ZnO Thin Films	34
	2.7.1	The Phase Transition From Amorphous to Crystalline of ZnO Thin Films 34
        2.7.2	Optical Properties of Amorphous and  Recrystallized ZnO  40
CHAPTER III THIN FILM STRESS MEASUREMENT	42
3.1 Thin Film Stress 42
	3.1.1	Residual Stress 42
	3.1.2	Film Stress Definition	43
	3.1.3	Thermal Stress (σth)	45
	3.1.4	Stress Induced Phase change (σph)	45
	3.1.5	Epitaxial Stress (σep)	45
3.2 Thin Film Stress Measurement Techniques 	45
	3.2.1 	Cantilever Beam	46
	3.2.2	Newton's Ring Method	47
	3.2.3	X-Ray Diffraction	47
	3.2.4	GIXRD Thin Film Residual Stress Measurement	49
	3.2.5	Plane Stress Transformation and Mohr's Circle Analysis	54
		3.3.5.1 Mohr's Circle Mapping	55
CHAPTER IV EXPERIMENTAL METHOD	57
4.1 	Experimental Procedure	57
        4.1.1 	Solution Preparation	57
        4.1.2 	Thin Film Process and Analysis	58
4.2 	Experimental Equipment and Solutions	58
        4.2.1	Experimental Equipment	58
        4.2.2	Experimental Solution	59
4.3 	Film Production	59
        4.3.1	Substrate Cleaning	60
        4.3.2	AZO Sol-Gel Preparation	62
4.4 	GIXRD Residual Stress Measurement Process 64
        4.4.1	Stress Measurement Process	64
        4.4.2 	Measurement Devices	65
	4.4.3	Measurement Planning	65
CHAPTER V RESULTS AND DISCUSSION	67
5.1 Nanoindentation of AZO Thin Films 67
5.2 Scanning Electron Microscopy (SEM) of AZO Thin Film    	73
5.3 The Electrical and Optical Properties of AZO Thin Film 75
	5.3.1 	Description of Experimental Parameters 	75
	5.3.2 	The Transmittance of ZnO Thin Film For Different RTA Temperature 	75
	5.3.3	The Thickness of AZO Thin Films	76
	5.3.4	Sheet Resistance of AZO Thin Films at Different RTA Temperatures 	77
5.4 The Residual Stress of AZO Thin Films. 78
	5.4.1  Thin Film Plane Stres Measured by XRD 78
        5.4.2  The Principal Stress And Maximum Shear Stress by Mohr's Circle 91
	5.4.3  Stress Gradient Analysis via GIXRD	95
CHAPTER VI CONCLUSIONS AND FUTURE WORKS	102
5.1 Conclusions 102
5.2 Future Works105
REFERENCES	106
APPENDIX A 	109
APPENDIX B      116
                                    

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