在控制氣氛及真空中藉由熱處理氮化鋯薄膜成長氧化鋯

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研究生：	謝志威
論文名稱：	在控制氣氛及真空中藉由熱處理氮化鋯薄膜成長氧化鋯 Growth of ZrO2 by Heat Treating ZrN Thin Film under Controlled Atmosphere
指導教授：	黃嘉宏喻冀平
口試委員:	駱榮富李志偉
學位類別：	碩士 Master
系所名稱：	原子科學院 - 工程與系統科學系 Department of Engineering and System Science
論文出版年：	2012
畢業學年度：	100
語文別：	英文
論文頁數：	109
中文關鍵詞：	氧化鋯、氧化、潤濕性、熱處理、抗腐蝕性
外文關鍵詞：	ZrO2, oxidation, wettability, heat treatment, corrosion resistance
相關次數：	點閱：2 下載：0
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本研究的目的在於藉由熱處理的方式於氮化鋯薄膜上成長二氧化鋯，希望可以解決二氧化鋯在304不鏽鋼上的潤濕性問題，另一方面也將研究氮化鋯的氧化機制。首先利用中空陰極放電離子覆膜系統將氮化鋯薄膜鍍著於Si基材及AISI 304不鏽鋼基材，之後將試片在不同的熱處理環境中進行700°C到1000°C、持溫1到4小時的熱處理。選用的熱處理環境為真空(510-6 Torr)以及氮氫混和氣體(N2/H2=9)，希望藉由減少環境中的含氧量來避免劇烈的氧化。在氮氫環境中，當熱處理溫度高於800°C且經過1小時的持溫便會完全氧化，然而在真空環境中即使溫度高達1000°C、持溫時間長達4小時，氮化鋯仍為試片的主要相。此外在兩種環境下熱處理後的試片其表面形貌、微結構和成分亦有明顯不同，推測在不同的環境中表面有著不同的結構因而導致了氧化行為的差異。在氮氫環境中表面氧化層不具保護性，所以氧可以很容易地與氮化鋯反應，而氧化所產生的體積膨脹則會導致表面空泡及裂縫產生，一旦表面有了破裂，則系統中的氧便可以再繼續與未氧化的氮化鋯反應，加速了氧化速率；相較之下表面氧化層在真空中則具有保護性，可以有效的抑止氧向試片內部擴散，因此氧化速度慢且表面仍可以維持完好。以不鏽鋼為基材的試片即使經過800°C持溫4小時的真空熱處理後表面依然可以看到殘餘的ZrN。經過500小時的鹽霧測試後，所有在真空熱處理中氧化的ZrN試片表面腐蝕面積均在0.2%以下，並且不會有脫落的現象，這表示所有試片均有著相當良好的抗腐蝕性，同時也證實了利用熱處理方法於不鏽鋼基材上成長氧化鋯的可行性。另外，當試片在1000°C進行持溫一小時的真空熱處理後，應力可以有效的被釋放，試片亦不會有明顯性質改變。

The purpose of this study is to solve the wettability issue by growing ZrO2 from heat treatment of the ZrN thin films on stainless steel substrate and investigate the oxidation mechanism of ZrN films in different atmospheres. ZrN thin films were deposited on Si and 304 stainless steel substrates using hollow cathode discharge ion-plating (HCD-IP), and were annealing at temperatures ranging from 700 to 1000°C and over durations ranging from 1 to 4 hours. Vacuum (510-6 Torr) and forming gas (N2/H2=9) environment were selected to prevent sever oxidation. As the annealing temperature was higher than 800°C, the specimens were totally oxidized in the forming gas within one hour. However, ZrN still remained as the major phase in the films even annealing at 1000°C for 4hr in vacuum. The microstructure and composition also revealed different behaviors in two annealing atmosphere. The difference may be derived from the surface structure in different annealing environments. The surface oxide was non-protective in the forming gas so that the oxygen in the system can easily reacted with ZrN, and the volume expansion during oxidation would lead to the formation of blisters and cracks on the sample surface. Once cracks appeared on the surface, oxygen could penetrate through the oxide layer and react with ZrN and accelerate the oxidation rate; on the other hand, since the surface oxide was protective in vacuum, the diffusion of oxygen was hindered and remained an intact surface. Retained ZrN could be observed on the surface layer in stainless steel-based specimens even annealed at 800°C for 4hr after vacuum annealing. The ratios of corrosion area for all the oxidized ZrN films were less than 0.2% after 500hr salt spray test indicating an excellent corrosion resistance. Thus, by selecting a proper environment, ZrO2 can be grown from ZrN without peeling and crack formation, which may provide good corrosion protection. Moreover, the stress could be relieved without significant change in properties as the specimens were annealed at 1000°C for 1hr in vacuum.

摘要    i
Abstract    ii
致謝    iii
Content    v
List of Figures    viii
List of Tables    xi
Chapter 1 Introduction    1
Chapter 2 Literature Review    3
2.1 Deposition Method: Hollow Cathode Discharge Ion-Plating (HCD-IP)    3
2.2 The Characteristics of ZrN and ZrO2    6
2.2.1 ZrN    6
2.2.2 ZrO2    8
2.3 Heat Treatment    12
2.4 The Oxidation Behavior of ZrN under Different Heat-Treating Environment    13
2.5 The corrosion resistance of zirconium oxynitride    15
Chapter 3 Experimental Details    17
3.1 Sample Preparation and Coating Process    17
3.2 Heat treatment    19
3.3 Characterization Methods    22
3.3.1 Rutherford Backscattering Spectroscopy (RBS)    22
3.3.2 Auger Electron Spectroscopy (AES)    23
3.3.3 X-ray Diffraction (XRD)    23
3.3.3.1 θ/2θ Scan    23
3.3.3.2 Glancing Incident X-ray Diffraction (GIXRD)    24
3.3.4 Field Emission Gun Scanning Electron Microscopy (FEG-SEM)    25
3.3.5 Atomic Force Microscopy (AFM)    25
3.4 Properties Measurements    25
3.4.1 Residual Stress    25
3.4.1.1 Laser Curvature Method    26
3.4.1.2 XRD cos2αsin2ψ method    26
3.4.2 Corrosion Resistance    29
3.4.2.1 Potentiodynamic Polarization Scan    29
3.4.2.2 Salt Spray Test    32
3.4.3 Coloration    34
Chapter 4 Results    36
4.1 Chemical Compositions    41
4.1.1 AES    41
4.2 Structure    47
4.2.1 XRD and GIXRD    47
4.2.2 SEM    55
4.3.2 Coloration and Reflectance    65
4.3.3 Corrosion Resistance    70
Chapter 5 Discussion    71
5.1 The corrosion resistance of the oxidized ZrN films    71
5.2 Oxidation Behavior of ZrN thin Films in Forming Gas and Vacuum    71
5.2.1 The Surface Conditions in Forming Gas and Vacuum during Annealing    72
5.2.2 Low Oxidation Rate during Vacuum Annealing    74
5.3 Retained ZrN on Surface in Vacuum Annealing    77
5.4 The Stress Relief of ZrN after Vacuum Annealing    79
Chapter 6 Conclusions    80
References    81
Appendix A    91
Results of SEM in low magnification
Appendix B    92
Results of AFM
Appendix C    95
Surface Morphologies after 500 hrs Salt Spray Test
Appendix D    97
The Effect of Flow Rate on the Measured PO2 using Oxygen Sensor
Appendix E    100
Fluid Mechanics Calculation in the Forming Gas Environment
Appendix F    103
The Window of PO2 for ZrN Oxidation
Appendix G    105
Results of Resistivity
Appendix H    106
Residual stress measured by XRD cos2αsin2ψ method
Appendix I    108
Results of RBS

                                

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