800 到 950°C下空氣中的鎳基超合金Haynes 282之氧化動力學與氧化層表面殘餘應力分析

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研究生：	陳廷秝 Chen, Ting-Li
論文名稱：	800 到 950°C下空氣中的鎳基超合金Haynes 282之氧化動力學與氧化層表面殘餘應力分析 Oxidation Kinetics and Residual Stress of Scales of a Ni-based Superalloy Haynes 282 in Dry Air at 800-950°C
指導教授：	藍貫哲 Lan, Kuan-Che 黃嘉宏 Huang, Jia-Hong
口試委員:	開物 Kai, Wu 朱鵬維 Chu, Peng-Wei
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：	2021
畢業學年度：	109
語文別：	英文
論文頁數：	96
中文關鍵詞：	鎳基超合金、Haynes 282 、高溫氧化、氧化層厚度、殘餘應力
外文關鍵詞：	Nickel-based superalloy, Haynes 282, High temperature oxidation, Thickness of oxide layer, Residual stress
相關次數：	點閱：2 下載：0
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鎳基超合金Haynes 282為先進超超臨界(A-USC)燃煤發電系統的候選結構材料。本研究利用熱重分析儀(TGA)對Haynes 282進行800、850、900 和950℃下24小時的增重行為分析，並利用箱型爐在相同溫度區間內的空氣中進行12至720小時之氧化，探討該溫度下的短期與長期之氧化動力學，其增重結果與外氧化層厚度增厚之速率皆符合拋物線曲線。此外，利用XRD、帶有EDS的FEG-SEM、FIB-SEM與EPMA對其氧化層進行表面微結構與橫截面微結構觀察、結構判定與成份分析後，得知該合金的氧化層為多層結構，其主要組成相為Rhombohedral-Cr2O3與Spinel-MnCr2O4，Rutile-TiO2與Perovskite-type CoTiO3則形成於外氧化層的表面。內氧化層的主要結構為Rhombohedral-Al2O3與Rutile-TiO2。由白金標記試驗得知，282合金在高溫下氧氣向合金內的擴散通量遠高於金屬離子向外的擴散通量。利用雷射共軛焦光學顯微鏡得知Haynes 282的表面粗糙度隨時間與溫度增加而提高，且在950℃下720小時的氧化後出現外氧化層的剝落與揮發。藉由azimuthal cos^2⁡α sin^2⁡ψ方法量測在800與950℃下12至720小時之氧化後形成之Rhombohedral-Cr2O3表面殘餘應力，扣除冷卻時產生之熱應力後，可以發現其在800℃下氧化時之內應力隨時間增加而由拉應力轉為壓應力，但其在950℃下之內應力皆為拉應力，且其值隨氧化時間增長而提高。期望本研究能提供Haynes 282在未來A-USC系統設計，運轉安全，以及面對意外事故的關鍵參數。

Nickel-based superalloy Haynes 282 is a candidate structural material for advanced ultra-supercritical (A-USC) coal-fired power generation systems. In this study, the thermogravimetric analyzer (TGA) was used to analyze the mass gain behavior of Haynes 282 at 800, 850, 900, and 950℃ for the exposure time of 24 hours, and a box furnace was used to perform the air oxidation test of Haynes 282 in the same temperature ranging from 12 to 720 hours. The studies of oxidation kinetics revealed that both results of mass gain behavior correspond with the parabolic curve. The increase of the thickness of the external oxide layer with time also conformed to a parabolic curve. By using XRD, FEG-SEM with EDS, FIB-SEM and EPMA respectively to observe the surface and cross-section microstructure of the oxide layer, structure characterization and chemical composition analysis, it was known that the oxide layer of the alloy was multilayer structure. The major oxide phases of the external oxide layer formed on Haynes 282 were rhombohedral-Cr2O3 and spinel-type MnCr2O4. rutile-TiO2 and perovskite-type CoTiO3 were the dominant phases on the surface of the oxide layer. The phases of internal oxide layer were rhombohedral-Al2O3 and Rutile-TiO2. From the result of platinum marker experiment, the diffusion flux of oxygen inward to the substrate of 282 alloy was much higher than that of metallic cation. By using the 3D-measuring laser confocal microscope, it was found that the surface roughness of Haynes 282 increased with time and temperature, and the low-lying region of the external oxide layer was observed in the specimen oxidized for 720 hours at 950°C. The surface residual stress of rhombohedral-Cr2O3 formed at 800 and 950℃ for 12 to 720 hours was measured by the average X-ray strain method. After subtracting the thermal stress generated during cooling, it could be found that the intrinsic stress of Cr2O3 at 800℃ changed from tensile stress to compressive stress as time increased, but that at 950°C was all tensile stress, and its value increased with the increase of oxidation time. It is hoped that the results of this study can provide key parameters for using Haynes 282 in the design of A-USC system such that the safety margin in operation can be enhanced in facing accidents.

致謝    i
摘要    iii
Abstract    iv
Contents    v
Lists of Tables    vii
Lists of Figures    viii
Chapter 1    Introduction    1
Chapter 2    Literature Review    3
2.1    Advanced power generation systems    3
2.1.1    Advanced ultra-supercritical (A-USC) coal-fired power generation systems    3
2.1.2    Generation IV nuclear energy systems    3
2.2    Nickel base superalloy    4
2.2.1    γ’ strengthened superalloy    4
2.2.2    Haynes 282    5
2.3    High temperature oxidation    5
2.3.1    Introduction to the oxidation of metal    5
2.3.2    Thermodynamic and the stability of the oxide forming on Ni-based alloys    6
2.3.3    Oxidation kinetics of alloys    7
2.3.4    Oxidation of Haynes 282    8
2.4    The stress influence and distribution in the oxide layer of metal alloy    9
Chapter 3    Experimental Details    16
3.1    Material    16
3.2    Sample Preparation    17
3.3    High temperature oxidation    17
3.3.1    Incipient oxidation    17
3.3.2    Long-term oxidation experiment    18
3.4    Structure analysis    19
3.4.1    X-ray diffraction (XRD) θ-2θ analysis    19
3.4.2    Surface macroscope analysis    20
3.4.3    Surface microstructure analysis    20
3.4.4    Cross-section analysis of oxidized-Haynes 282 specimens    21
3.4.5    Marker experiment of the oxidation of Haynes 282    22
3.5    Residual stress measurement    23
Chapter 4    Experimental Results    25
4.1    Still air oxidation kinetics of Haynes 282    25
4.1.1    Incipient oxidation    25
4.1.2    Long term oxidation kinetics    27
4.1.3    Marker experiment of oxidized Haynes 282    30
4.2    Microstructure analysis of pre-/post- Haynes 282 for high temperature oxidation    31
4.2.1    Crystal structure of pre-/post oxidized Haynes 282    31
4.2.2    Surface morphology and chemical composition analysis of oxidized-Haynes 282    36
4.2.2.1    Surface morphology    36
4.2.2.2    Surface roughness of the oxide layer    38
4.2.2.3    Chemical composition    43
4.2.3    Cross sectional observation and the compositional depth-profile of the
oxidized-Haynes 282    46
4.2.3.1    Cross sectional observation    46
4.2.3.2    Compositional depth-profile    51
4.3    Residual stress in the external layer of Haynes 282    56
Chapter 5    Discussion    57
5.1    Evolution of crystal structures of external oxide    57
5.2    Evolution of microstructures of external oxide    60
5.3    Evolution of internal oxide    62
5.4    Oxidation kinetics and model of oxidation mechanism    65
5.5    Generation and relaxation of intrinsic stress of the oxide layer on Haynes 282    75
Chapter 6    Conclusion    81
References    82
Appendix A    Macroscope images of Haynes 282 oxidized at 800 and 950°C    86
Appendix B  SEM images of special shaped oxides which were non equiaxial of Haynes
282 oxidized at 800°C    88
Appendix C    The raw data of the composition of the oxide layer on Haynes 282 formed
at 800°C and 950°C analyzed by EPMA technique    89
Appendix D    Azimuthal cos^2⁡α  sin^2⁡ψ    92
Appendix E    Texture and crystallography    95


                                

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