鎳基合金與鈦基合金鍍鋁後對高溫氧化及腐蝕性質之研究

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研究生：	Pius Kibet Koech Pius Kibet Koech
論文名稱：	鎳基合金與鈦基合金鍍鋁後對高溫氧化及腐蝕性質之研究 High-Temperature Oxidation and Corrosion Behaviours of Aluminized Nickel-based IN-718 Superalloy and Titanium-based Ti-6Al-4V Alloys
指導教授：	王朝正 Chaur-Jeng Wang
口試委員:	王朝正 Chaur-Jeng Wang 鄭偉鈞 Wei-Chun Cheng 郭俞麟 Yu-Lin Kuo 李志偉 Zhi-Wei Lee 蔡文達 Wen-Da Tsai 開物 Wu Kai
學位類別：	博士 Doctor
系所名稱：	工程學院 - 機械工程系 Department of Mechanical Engineering
論文出版年：	2018
畢業學年度：	107
語文別：	英文
論文頁數：	185
中文關鍵詞：	IN 718 、Ti-6Al-4V 、Hot-dip 、Plasma spray 、Plasma spray 、Cyclic oxidation 、Hot-corrosion
外文關鍵詞：	IN 718, Hot-dip, Plasma spray, Cyclic oxidation, Hot-corrosion
相關次數：	點閱：265 下載：15
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Inconel 718 (IN-718) 和 Ti-6Al-4V (Ti64) 合金具優異耐蝕性及高溫下良好機械性質，常用於航太、核能、化工、生物醫學。然而這些合金在高溫熱循環下造成氧化層破裂及剝落，氧化現象增加導致組件失效。研究指出，高溫循環期間因受到水蒸氣、NaCl、熱循環之影響，進而氧化形成兩種氧化鍍層之形貌。經熱浸鍍鋁及等離子噴塗鍍層之In-718及Ti64合金置於臥式管爐中，分別在乾燥及濕空氣條件下進行650、750℃循環氧化，每循環為加熱10小時再空冷至室溫30分鐘。記錄重量變化後，使用XRD、OM、SEM、EDS分析氧化層組成、顯微結構。
Inconel 718裸材表層在空氣中氧化形成Cr2O3氧化層，但合金表層檢測到Fe、Ni元素。而In-718裸材暴露於NaCl熱循環中，表層形成多孔Fe2O3氧化層，且腐蝕層有剝落嚴重產生。由於Fe2O3的揮發較Cr2O3快，Fe2O3氧化物在Cr2O3氧化物上方形成。Ti64裸材在空氣中氧化，生成TiO2與Al2O3為主要形成之氧化層。熱浸鍍鋁後之鋁塗層能改善In-718及Ti64合金的抗氧化性。然而隨著熱循環次數的增加，Al2O3氧化物及鋁化層中因為Kirkendall effect 形成之空洞數量增加。於熱腐蝕環境中，熱浸塗層改善合金的耐腐蝕性，但也由於裂縫和Kirkendall effect所產生空隙，導致鋁化層的降解，使腐蝕鹽侵蝕至底材造成大量腐蝕。鋁塗層向外擴散形成氧化層，而向內擴散則形成NiAl層。
由單位面積之重量變化量結果顯示，熱浸鍍鋁熱增重變化最小，而等離子噴塗及裸材之熱增重最後因氧化層剝離而略微下降。熱浸塗層與等離子噴塗層形成之氧化層有不同形貌及成長速率。乾空氣與濕空氣中氧化層也有所差異，濕空氣測試中，因水存在而形成氧化鋁（Al2O3）使界面韌性降低，造成高氧化速率及空隙，幾乎無保護性之氧化鋁層。儘管如此，與等離子噴塗相比，水蒸氣似乎不會對熱浸塗層產生大的影響。結果可知，熱浸鍍層較等離子塗層有更好的抗氧化性。

Inconel 718 and Ti-6Al-4V alloys are commonly used in aerospace, nuclear, biomedical and chemical industries due to their excellent corrosion resistance with good mechanical properties at elevated temperatures. However, these alloys among other metallic materials are susceptible to high temperature oxidation due to cracking and spallation of the scales especially under thermal-cycling conditions which resulted in the failure of components.
In the present work, effects of water vapour, NaCl salts, and thermocycling commonly prevailing on the morphology and composition of alumina formed during high-temperature cyclic-oxidation were studied using two types of aluminide coatings. The aluminide hot-dip and plasma spray coatings prepared on inconel 718 and Ti-6Al-4V alloys were cyclically oxidized in horizontal tube furnace at 650 and 750 °C respectively. Test were done both in dry and moist air conditions by passing dry air through hot water bath at a flow rate of 200 cc/min. The exposure period was 10 hours in hot the chamber and 30 minutes at 25 C in room temperature per cycle. After recording mass changes, analyses of the composition, microstructure characterization, and morphology of the scales were conducted. Uncoated materials were also tested for comparisons.
A Cr2O3 layer formed on uncoated inconel 718 alloy oxidized in dry air. Small amounts of Fe and Ni were also detected on the surface. However, porous oxide scale of Fe2O3 formed on the surface of uncoated inconel 718 substrate exposed to thermal-cycle in NaCl salt with extensive corrosive attack and scale spallation. Oxide of Fe2O3 formed on top of Cr2O3 oxide layer due to high volatilization of iron-chloride in respect to chromium-chloride. On the other hand, the scales formed on uncoated Ti-6Al-4V alloy in dry air consisted mainly TiO2 and minor oxide of Al2O3. The hot-dip coating provided a better oxidation resistance of both IN 718 and Ti-6Al-4V. However, spallation of Al2O3 oxide scale and formation of Kirkendall voids in the aluminide layer increased under thermal-cycle exposure. In presence of NaCl salts, the hot-dip coating improved corrosion resistance of the alloy compared to uncoated material. However, degradation of aluminide layer due to formation of cracks and voids allowed NaCl ions to diffuse into the substrate which resulted in an extensive corrosion.
The mass change results show that aluminide hot-dip coating had the lowest value while both the plasma spray coating and uncoated specimens had an increase in mass then slightly decreased probably due to spallation of the oxide layer. The results also show that the oxide scale formed on the surface of the hot-dip coating has an inherently different morphology and growth rate compared to those formed on the plasma spray coating. Such discrepancies were also noted in coatings oxidized in dry air compared to those oxidized in moist air. High oxidation rate, severe spallation, extensive blistering and large voids with little protective alumina scale were observed in wet air. This can be attributed to decreased interfacial toughness of alumina oxide in the presence of water.
Thus, it was concluded that the hot-dip coating has a better oxidation resistance compared to plasma spray coating.

Dedication.….    i
Abstract………    ii
Acknowledgements    v
Table of Contents    vi
List of Tables..    x
List of Figures    xi
Nomenclature..    xvi
Chapter 1: Introduction    1
1    Nickel based superalloy - Inconel 718    2
2    Titanium based alloy - Ti-6Al-4V    4
3    Statement of research problem    5
4    Objectives    5
4.1    Broad objective    5
4.2    Specific objectives    5
Chapter 2: Literature Review    6
1    Background    7
1.1    Nickel based superalloys    7
1.2    Titanium based alloys    9
2    Thermodynamics of oxidation and diffusion    13
2.1    Chemical activities    13
2.2    Kinetics of oxidation    16
2.3    Wagner’s theory of oxidation    18
2.4    Solid - state diffusion and transport mechanism in oxides    19
2.4.1    Lattice diffusion: - Point defects in oxides    19
2.4.2    Short-circuit diffusion: - Linear and planar defects    20
2.5    Kirkendall Effect (Interdiffusion)    21
3    High temperature oxidation of metal alloys    22
3.1    Selective oxidation    22
3.2    Internal oxidation    23
3.2.1    Transition from internal to external oxidation    24
3.2.2    Subsurface void formation    24
3.3    Oxide formation and growth    25
3.4    Oxidation of some commercial alloys    26
3.4.1    Growth of Cr2O3 scales on Ni, Fe and Co-based alloys    26
3.4.2    Growth of Al2O3 scales on Ni, Fe and Co-based alloys    27
3.4.3    Growth of TiO2 scales on titanium-based alloys    29
3.5    Stresses generation in oxide scale     31
3.5.1    Oxide growth stress (Pilling-Bedworth ratio)    31
3.5.2    Thermal stress (Coefficient of Thermal Expansion)    32
3.5.3    External Stresses    33
3.6    Healing of oxide scale cracks    34
3.7    Effect of alloy elements on oxidation behavior of alloys    35
3.8    Formation of intermetallics in commercial alloys    36
3.8.1    Ni-Al based intermetallics    36
3.8.2    Ti-Al-based intermetallics    37
3.8.3    Fe-Al based intermetallics    38
3.9    Effects of water-vapor on the oxidation behavior of alloys    38
4    High temperature corrosion of metal alloys    40
4.1    Corrosion environment    40
4.2    Mechanism of hot corrosion    40
4.3    Types of hot corrosion    41
4.4    Corrosion mechanisms in chlorine gas    43
4.5    Hot corrosion of super alloys (Ni-Cr alloys)    43
5    Protective coatings for high temperature applications    44
5.1    Pack cementation    45
5.2    Chemical vapor deposition (CVD) coatings    45
5.3    Physical vapour deposition (PVD) coatings    46
5.4    Plasma electrolytic oxidation (PEO) coatings    46
5.5    Thermally sprayed coatings    47
5.5.1    High velocity oxy-fuel flame (HVOF)    47
5.5.2    Plasma spray coatings    48
5.5.3    Thermal barrier coatings (TBC)    49
5.6    Hot-dip coatings    51
5.6.1    Factors influencing aluminizing process    51
5.6.2    Growth of intermetallic phases during aluminizing process    53
Chapter 3: Experimental Procedures    54
1    Overview    55
2    Design of experiment    56
3    Experimental methodology    56
3.1    Substrate materials    56
3.2    Specimen preparation    57
3.3    Substrate coating    58
3.4    Cyclic oxidation and corrosion test    59
3.5    Kinetics calculation    61
4    Specimen analysis    61
4.1    Mounting, grinding, polishing and etching procedures    61
4.2    X-ray diffraction (XRD) analysis    62
4.3    Scanning electron microscopy (SEM) for metallographic examination    63
Chapter 4: Results    64
1    Preface    65
2    As-deposited aluminium coating specimens    65
2.1    Microstructure of as-coated IN-718 superalloy specimens    65
2.2    Microstructure of as-coated titanium-based Ti64 alloy    67
3    Kinetics of oxidation    69
3.1    Oxidation kinetics of bare and coated IN-718 superalloy    69
3.2    Oxidation kinetics of bare and coated titanium-based Ti64 alloy    71
4    High temperature cyclic oxidation of bare material    72
4.1    Cyclic oxidation of bare IN-718    72
4.2    Cyclic oxidation of titanium based Ti64 alloy    76
5    Scale constitution and phases of aluminized specimens    78
5.1    Cyclic oxidation of aluminized IN-718 alloys at elevated temperatures    77
5.1.1    Effect of hot-dip coatings on cyclic oxidation of IN-718 superalloys    79
5.1.2    Effect of plasma spray coatings on cyclic oxidation of IN-718 superalloy    87
5.2    Cyclic oxidation of aluminized Ti64 alloy at elevated temperatures    93
5.2.1    Cyclic oxidation of hot-dip aluminized Ti64 alloy    93
5.2.2    Cyclic oxidation of plasma-spray aluminized Ti64 alloy    102
6    NaCl induced hot corrosion on bare and coated materials    107
6.1    Corrosion of bare IN-718 in NaCl at elevated temperatures    107
6.2    Corrosion of hot-dip aluminized IN-718 in NaCl    110
Chapter 5: Discussion    115
1    Outline    116
2    Formation of intermetallic phases on as-coated specimens    116
2.1    Phase formation in aluminized as-coated IN-718 superalloys    116
2.2    Phase formation in as-coated titanium-based Ti64 alloy    119
3    Effect of Temperature with respect to oxidation kinetics    121
4    Oxidation mechanisms of bare specimens    124
4.1    Oxidation mechanisms of bare IN-718 superalloy    124
4.2    Oxidation mechanisms of bare titanium based Ti64 alloy    127
5    Effect of aluminized coating on oxidation mechanism    130
5.1    Oxidation mechanisms of aluminized IN-718 superalloy    130
5.2    Oxidation mechanisms of aluminized titanium based Ti64 alloy    136
6    Analysis of protective scale failures due to NaCl salt    141
6.1    Failures mechanisms of bare IN-718 due to NaCl salt deposits    142
6.2    Failures mechanisms of hot-dip coating due to NaCl deposits    147
Chapter 6: Conclusion and Future Works    149
1    Conclusions    150
2    Future works    152
References….    153
Publications…    165
Short Resume    166

                                

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