本研究的目的在於探討利用兩種鍍膜系統鍍氮化鋯薄膜於不鏽鋼上經真空熱處理後的氧化行為與防蝕性質。首先利用中空陰極放電離子覆膜系統及非平衡磁控濺鍍系統將氮化鋯薄膜鍍著於AISI 304 不鏽鋼基材上，之後將兩種試片同時於1000 °C、真空(4×10-6 Torr)的環境下，進行1到4小時的熱處理。由X光繞射圖顯示，試片即使經過長達4小時的熱處理，氮化鋯仍為主要相。此外，利用非平衡磁控濺鍍系統所鍍之氮化鋯薄膜其晶粒較利用中空陰極放電離子覆膜系統所鍍之薄膜大，使得兩者氧化後之薄膜表面晶粒大小也有相似結果，而晶粒大小也會影響熱處理後氧化相之生成。氧化後薄膜表面及膜與基材的界面附近分別形成外、內氧化層，推測是由於氧氣同時由薄膜表面及膜與基材介面的邊緣擴散進膜內而形成。動態極化掃描的結果顯示經氮化鋯覆膜之不鏽鋼氧化後展現極佳的抗蝕性，且試片腐蝕電流密度至多可下降至1000倍。經過500小時的鹽霧測試後，熱處理後之試片表面腐蝕面積均在6.7 %以下，且非平衡磁控濺鍍系統所鍍之薄膜抗蝕性更佳。另外，利用非平衡磁控濺鍍系統所鍍之氮化鋯薄膜經熱處理所得之全氧化試片，經過動態極化掃描與500小時鹽霧測試後展現極佳抗蝕性且薄膜也不會有脫落的現象，推測是經過熱處理後在膜與基材界面處產生的交互擴散層提高膜對基材的附著性。本研究結果顯示利用非平衡磁控濺鍍與中空陰極放電離子覆膜系統所鍍之氮化鋯薄膜均可藉由真空熱處理來成長氧化層，因此，非平衡磁控濺鍍可以取代中空陰極放電離子覆膜系統鍍製氮化鋯薄膜於不鏽鋼上來生產抗蝕性極佳之氧化層。

The purpose of this study was to investigate the oxidation behavior and corrosion resistance of the vacuum annealed ZrN-coated stainless steel (SS) deposited by two deposition methods. ZrN thin films were deposited on AISI 304SS by hollow cathode discharge ion-plating (HCD-IP) and unbalanced magnetron sputtering (UBMS). Afterwards, the specimens were annealed at 1000°C in vacuum (4×10-6 Torr) for a duration ranging from 1 to 4 hr. The XRD results indicated that ZrN remained as the major phase in the oxidized thin films even after heat treating at 1000 °C for 4 hr in vacuum. Since the grain size of the as-deposited ZrN films by UBMS was larger than that by HCD-IP, the surface grain size of the oxidized film showed the similar results, which also affected the phase formation after vacuum annealing. The oxidized ZrN thin film on 304SS formed two oxide layers, the outer layer on the film surface and the inner layer nearby the film/substrate interface, which could be attributed to the simultaneous diffusion of oxygen from film surface and the edge of film/substrate interface, respectively. The results of potentiodynamic polarization scan showed that the corrosion resistance of the oxidized ZrN-coated SS was excellent and increased by about 1000 times relative to that of bare 304SS. The corrosion area after 500-hr salt spray test was less than 6.7 % for the oxidized ZrN-coated SS, and the oxidized ZrN films deposited by UBMS had better durability in salt spray test. The fully oxidized ZrN thin film deposited by UBMS showed great corrosion resistance and remained intact on 304SS substrate after potentiodynamic polarization scan and 500-hr salt spray test, which was associated with the enhanced adhesion by the interdiffusion layer from heat treatment. The results indicated that ZrN thin films deposited by both UBMS and HCD-IP could be used for the growth of oxidized layer by vacuum annealing. Therefore, UBMS could replace HCD-IP to deposit ZrN thin films on 304SS to produce an oxidized ZrN layer with excellent corrosion resistance.

Content
致謝 i
摘要 iv
Abstract v
Content vi
List of Figures ix
List of Tables xiii
Chapter 1 Introduction 1
Chapter 2 Literature Review 3
2.1 Coating Methods 3
2.1.1 Hollow Cathode Discharge Ion-Plating (HCD-IP) 3
2.1.2 Unbalanced Magnetron Sputtering (UBMS) 4
2.2 The Characteristics of ZrN and ZrO2 5
2.2.1 ZrN 5
2.2.2 ZrO2 7
2.3 Heat Treatment and the Oxidation Behavior of ZrN Thin Films 12
2.4 The Corrosion Resistance of ZrO2 Thin Film 14
Chapter 3 Experimental Details 17
3.1 Substrate Preparation and Coating Process 18
3.2 Vacuum Heat Treatment 23
3.3 Characterization Methods 24
3.3.1 X-ray Diffraction (XRD) 24
3.3.1.1 θ/2θ scan 24
3.3.1.2 Grazing Incident X-ray Diffraction (GIXRD) 24
3.3.2 Field Emission Scanning Electron Microscopy (FEG-SEM) 25
3.3.3 Atomic Force Microscopy (AFM) 26
3.3.4 X-ray Photoelectron Spectroscopy (XPS) 26
3.3.5 Auger Electron Spectroscopy (AES) 27
3.3.6 Dual-Beam Focused Ion Beam Microscopy (FIB) 28
3.4 Properties Measurements 28
3.4.1 Residual Stress 28
3.4.2 Hardness and Young’s Modulus 29
3.4.3 Coloration 29
3.4.4 Corrosion Resistance 31
3.4.4.1 Potentiodynamic Polarization Scan 31
3.4.4.2 Salt Spray Test 33
Chapter 4 Results 34
4.1 Structure 39
4.1.1 XRD and GIXRD 39
4.1.2 OM and SEM Observations 44
4.2 Compositions 51
4.2.1 XPS and AES 51
4.3 Properties 56
4.3.1 Hardness 56
4.3.2 Residual Stress 57
4.3.3 Corrosion Resistance 59
4.3.3.1 Potentiodynamic Polarization Scan 59
4.3.3.2 Salt Spray Test 66
Chapter 5 Discussion 68
5.1 The Comparison of Structure of the Oxidized ZrN Thin Films Deposited by HCD-IP and UBMS 68
5.2 The Oxidation Behavior of ZrN Thin Films Annealed in Vacuum 73
5.3 The Corrosion Resistance of Oxidized ZrN Coated Stainless Steel 80
5.4 The Adhesion of ZrO2 on 304SS Substrate 82
Chapter 6 Conclusions 88
References 89
Appendix A 95
Surface Morphology After 500 hr Salt Spray Test 95
Appendix B 98
The Cross-Sectional Morphology of Specimens 98
Appendix C 100
The Compositional Depth Profiles of the Oxidized ZrN 100
Appendix D 102
The Phase Identification of the Specimens Before and After Potentiodynamic Polarization Scan 102
Appendix E 104
Deconvolution XPS Spectra of the Specimens 104
Appendix F 115
Results of AFM 115
Appendix G 120
The Distribution of Surface Grain Size 120

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