氮化鋯薄膜經真空熱處理之氧化行為與防蝕性之研究

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研究生：	周孫安 Chou, Sun-An
論文名稱：	氮化鋯薄膜經真空熱處理之氧化行為與防蝕性之研究 The Oxidation Behavior and Corrosion Resistance of ZrN Thin Films Heat Treated in Vacuum
指導教授：	黃嘉宏 Huang, Jia-Hong 喻冀平 Yu, Ge-Ping
口試委員:	黃嘉宏喻冀平李志偉林郁洧
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：	2014
畢業學年度：	102
語文別：	英文
論文頁數：	104
中文關鍵詞：	二氧化鋯、氮化鋯、熱處理、非平衡磁控濺鍍、相變化
外文關鍵詞：	zirconium oxide, zirconium nitride, heat treatment, unbalanced magnetron sputtering, phase transformation
相關次數：	點閱：1 下載：0
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本研究的目的在於探討氮化鋯薄膜經熱處理過後的氧化行為以及防蝕性質。首先利用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，之後在1000C、真空(4 × 10-6 Torr)的環境下進行1到4小時的熱處理。X光繞射圖顯示，熱處理氮化鋯的相組成為氮化鋯、單斜晶氧化鋯和正方晶氧化鋯。而在4小時的熱處理之後，氮化鋯依然是薄膜中的主要相。另外，在縱深分佈中發現薄膜表面以及薄膜和基材界面處都有一層氧化鋯。相變化後殘餘的氮化鋯則在薄膜中間的部分，使整個薄膜的結構像是多層層狀結構。薄膜和基材界面處的氧化鋯的成因可能是由於高溫下基材的應力釋放。在1小時的熱處理後，正方晶氧化鋯層形成於界面處。單斜晶氧化鋯層則形成於表面處以及鄰接正方晶氧化鋯層和單斜晶氧化鋯層的氮氧化鋯層中，而單斜晶氧化鋯層和氮氧化鋯層中氮化鋯轉變成單斜晶氧化鋯的相變化也導致薄膜增加50%的厚度。隨著熱處理時間加長，薄膜的厚度依然維持定值，指出後續的氧化主要是氮化鋯和氮氧化鋯轉變成正方晶氧化鋯，相變化所造成體積上的變化也由於大的壓應力而被限制住。薄膜的抗蝕性由動態極化掃描、500小時鹽霧實驗以及電化學阻抗來測定。結果顯示熱處理氮化鋯擁有很好的抗蝕性，特別是在重量百分濃度5%的鹽水中。薄膜的腐蝕電流密度隨著熱處理時間的增長而下降，並在熱處理2小時後下降至1000倍。而在500小時鹽霧實驗後，經過熱處理氧化的氮化鋯的腐蝕面積也隨著熱處理時間的增加而減少，並在熱處理4小時後減少至3%。

The purpose of this study was to investigate the oxidation behavior and corrosion resistance of heat-treated ZrN thin films. ZrN thin films were deposited on the 304 stainless steel by unbalanced magnetron sputtering system (UBMS), and then heat treated to grow ZrO2 at 1000C in vacuum (4 × 10-6 Torr) over the duration ranging from 1 to 4 hours. The results of XRD showed that the phase constituents of the heat-treated ZrN were ZrN, m-ZrO2 and t-ZrO2, where ZrN was still the major phase in the thin film even after 4-hr heat treatment. Furthermore, the compositional depth profiles indicated that there were two layers of ZrO2 on the film surface and at film/substrate interface, respectively. The retained ZrN was in the middle part of thin film and the entire thin film displayed a multilayer structure. The ZrO2 layer at film/substrate interface may result from the stress relief of substrate at high temperature. In the 1-hr duration, t-ZrO2 layer was formed at interface, while m-ZrO2 layer was formed on the film surface and Zr(N,O) layers containing m-ZrO2 formed next to t-ZrO2 and m-ZrO2 layers, where the transformation from ZrN to m-ZrO2 led to about 50% of film thickening. The film thickness remained constant with further increase of annealing duration, indicating that the oxidation mainly progressed by the formation of t-ZrO2 at the expense of ZrN or Zr(N,O), where the volume change of phase transformation is restricted by the large compressive stress. The corrosion behavior was determined by potentiodynamic polarization scan, 500-hr salt spray test and electrochemical impedance spectroscopy. The results show that the heat-treated ZrN exhibited excellent corrosion resistance, especially in 5 wt. % NaCl solution. The corrosion current density decreased with increasing annealing duration and reached up to 1000 times after annealing in vacuum for 2 hours. The corrosion area of the oxidized ZrN after 500-hr salt spray test also decreased with the increasing heat treatment duration and downs to 3% after 4-hr heat treatment.

Content
摘要    i
Abstract    ii
致謝    iii
Content    v
List of Figures    ix
List of Tables    xiv
Chapter 1  Introduction    1
Chapter 2  Literature Review    1
2.1 Deposition method    1
2.2 The characteristics of ZrO2 and ZrN    3
2.2.1 ZrO2    3
2.2.2 ZrN    6
2.3 Heat treatment    8
2.4 The oxidation behavior of ZrN thin film under different atmosphere    8
2.5 The corrosion resistance of ZrO2    9
Chapter 3  Experimental Details    11
3.1 Substrate Preparation    11
3.2 Deposition Process    11
3.3 Heat Treatment    13
3.4 Characterization Methods    15
3.4.1 X-ray Diffraction (XRD)    15
3.4.1.1 θ/2θ Scan    15
3.4.1.2 Grazing Incident X-ray Diffraction (GIXRD)    15
3.4.2 Field Emission Scanning Electron Microscopy (FEG-SEM)    16
3.4.3 Atomic Force Microscopy (AFM)    17
3.4.4 X-Ray Photoelectron Spectroscopy (XPS)    17
3.4.5 Focus Ion Beam / Scanning Electron Microscopy (FIB/SEM)    18
3.4.6 Auger Electron Spectroscopy (AES)    18
3.5 Properties Measurements    19
3.5.1 Hardness and Young’s Modulus    19
3.5.2 Residual Stress    19
3.5.3 Corrosion Resistance    20
3.5.3.1 Potentiodynamic Polarization Scan    20
3.5.3.2 Salt Spray Test    23
3.5.3.3 Electrochemical Impedance Spectroscopy (EIS)    24
Chapter 4  Results    25
4.1 Chemical Compositions    29
4.1.1 AES and XPS    29
4.2 Structure    34
4.2.1 XRD and GIXRD    34
4.2.2 Surface morphology    38
4.2.3 Roughness    43
4.3 Properties    44
4.3.1 Residual stress    44
4.3.2 Hardness    46
4.3.3 Corrosion Behaviors    47
4.3.3.1 Potentiodynamic Polarization Scan    47
A. 1N H2SO4 + 0.05M KSCN    47
B. 5 wt. % NaCl    50
4.3.3.2 Salt Spray Test    54
4.3.3.3 EIS    57
Chapter 5   Discussion    59
5.1 The comparison between oxidized ZrN by vacuum annealing and ZrO2 deposited by HCD-IP    59
5.2 The adhesion of vacuum heat-treated ZrN thin film    59
5.3 The oxidation behavior of vacuum heat-treated ZrN    61
5.3.1 The variation of oxide layer thickness with heat treatment duration    63
5.3.2 Further analysis of the oxidation behavior    64
5.4 The corrosion resistance of vacuum heat-treated ZrN    70
5.5 The α-Fe diffraction peak in XRD patterns of stainless steel substrate    71
5.6 The effect of thermal stress    72
Chapter 6  Conclusions    75
References    76
Appendix A    86
Deconvolution XPS spectra of specimens    86
Appendix B    95
The GIXRD diffraction pattern of specimens    95
Appendix C    99
The results of AFM    99
Appendix D    103
The film thickness of specimens    103

                                

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