本研究目的在於探討鍍著於鋯四合金上之二氧化鋯薄膜的初期氧化行為，並與未鍍膜之鋯四合金比較。利用非平衡磁控濺鍍系統，鍍著正方晶與單斜晶結構之二氧化鋯薄膜於鋯四合金。潤濕性測試顯示，正方晶與單斜晶結構之二氧化鋯與鋯四合金間的接觸角皆小於30°，其交互擴散區間皆大於150 nm。這也代表兩結構之二氧化鋯薄膜在鋯四合金上沒有吸附性不佳的問題。在經過700°C、800°C，以及900°C氬氣環境下之氧化熱重分析，X光繞射結果顯示兩種結構濺鍍之薄膜與表面自然形成之二氧化鋯均呈現單斜晶為主的結構。在700°C之下的氧化增重，有無二氧化鋯覆膜的鋯四合金間並沒有顯著的差異，並且氧化增重與時間符合拋物線關係。當氧化溫度為800°C時，單斜晶二氧化鋯覆膜之鋯四合金具有最少的增重，然而氧化指數n值為0.78。當氧化溫度提升至高於鋯四合金相變化溫度以上之900°C時，正方晶二氧化鋯覆膜之鋯四合金具有較佳的抗氧化能力。然而當溫度高於800°C時，氧化增重曲線不再遵守拋物線關係。在高於700°C的氧化熱重分析中，於鋯四合金上自然形成之二氧化鋯發現到有瘤狀氧化物。由預先濺鍍形成的正方晶與單斜晶結構之二氧化鋯覆膜均可以避免表面瘤狀氧化物的產生。藉由azimuthal cos2(alpha)sin2(psi)方法量測正方晶與單斜晶結構的二氧化鋯的殘留應力分布，可以發現殘留應力隨方位角的不同，並不一定呈現均勻分布。此外，azimuthal cos2(alpha)sin2(psi)方法為一種便利的非破壞性方法，可應用於檢測表面氧化物的分布均勻性，且適用於多種相同時存在的狀況。

The purpose of this study was to investigate the incipient oxidation behavior of ZrO2-coated Zircaloy-4 (Zry-4) and compare with that of uncoated Zry-4. ZrO2 thin films with tetragonal (t) and monoclinic (m) dominant phases were deposited on Zry-4 by unbalanced magnetron sputtering (UBMS). The wettability tests showed that the contact angles of both t-ZrO2 and m-ZrO2 on Zry-4 were less than 30°, and the corresponding widths of interdiffusion zones were larger than 150 nm, indicating that there would be no adhesion problem between ZrO2 film and Zry-4 substrate. Thermogravimetric analysis (TGA) tests were carried out at 700, 800 and 900°C in argon atmosphere. X-ray diffraction (XRD) patterns showed that both naturally formed ZrO2 and the deposited ZrO2 on Zry-4 possessed a m-ZrO2 dominant structure after oxidation. The results of weight gain at 700°C showed that there was no significant difference in oxidation behavior between uncoated and ZrO2-coated Zry-4, and the oxidation kinetics obeyed parabolic law. At 800°C, m-ZrO2-coated Zry-4 possessed the least weight gain, while the oxidation rate deviated from parabolic law with an exponent n value of 0.78. As the oxidation temperature increased to 900°C, above the phase transformation temperature of Zry-4, t-ZrO2-coated Zry-4 displayed a better oxidation resistance. However, the oxidation kinetics of all series of specimens no longer obeyed parabolic law above 800°C. Oxide nodules were observed on the uncoated Zry-4 after TGA oxidation test at 700°C and above. The pre-deposited ZrO2 thin films, both monoclinic or tetragonal phases, can act as a protective layer to prevent the formation of oxide nodules. The azimuthal cos2(alpha)sin2(psi) technique was used to show the distribution of residual stress of t-ZrO2 and m-ZrO2 phases in the specimens. The results indicated that the oxide phases were not always uniformly distributed in the specimens. Moreover, the azimuthal cos2(alpha)sin2(psi) technique can be one of the convenient and nondestructive methods to examine the uniformity of multi-phase oxide layer on the sample surface.

Content
致謝 i
摘要 iv
Abstract v
Content vi
List of Figures ix
List of Tables xiv
Chapter 1 Introduction 1
Chapter 2 Literature Review 3
2.1 Severe Oxidizing Environments in PWR 4
2.2 Improvements of Zirconium-based Alloys 5
2.2.1 Alternative Cladding Materials 5
2.2.2 Compositional Modification of Zirconium-based Alloys 5
2.2.3 Coating Technology 6
2.3 Candidate Protective Coating Material for Zry-4: ZrO2 7
2.3.1 Characteristics of ZrO2 7
2.3.2 Applications of ZrO2 8
2.4 The Stress Distribution of ZrO2 Thin Films 13
2.5 Oxidation of Zirconium-based Alloys at High Temperature 14
Chapter 3 Experimental Details 15
3.1 Substrate Preparation and Deposition Process 15
3.2 Characterization of Composition and Structure 19
3.2.1 Chemical Composition 19
3.2.2 Compositional Depth Profiles 20
3.2.3 Crystal Structure and Preferred Orientation 21
3.2.4 Topography and Cross-sectional Morphology 22
3.2.5 Surface Roughness 24
3.3 Characterization of Thin Films Properties 24
3.3.1 Hardness and Elastic Constant 25
3.3.2 Residual Stress 25
3.3.3 Wettability 26
3.3.4 Oxidation Behavior 28
Chapter 4 Results 31
4.1 Chemical Compositions 34
4.1.1 Surface Compositions and Compositional Depth Profiles for the As-deposited Specimens 34
4.1.2 Surface Compositions after TGA Oxidation Test 36
4.2 Structure 37
4.3 Characterization of Thin Film Properties 58
Chapter 5 Discussion 73
5.1 The Structure of the As-deposited ZrO2 on Zry-4 73
5.2 The Oxidation Behavior of ZrO2-coated Zry-4 73
5.2.1 The Structure of ZrO2 Films 73
5.2.2 Surface Morphology 75
5.2.3 Weight Gain of TGA Oxidation Test 77
5.3 Distribution of Residual Stress: Azimuthal cos2(alpha)sin2(psi) 81
Chapter 6 Conclusions 83
References 84
Appendix A Grinding and Polishing Procedures of Zircaloy-4 93
Appendix B Deconvolution of XPS 95
Appendix C Azimuthal cos2(alpha)sin2(psi) 107
Appendix D Vacuum Annealing of ZrN-coated Zry-4 127
Appendix E Enlarged SEM Images after Oxidation 144

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