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研究生： 許瑋麟
Hsu, Wei-Lin
論文名稱： NixCo0.6Fe0.2CrySizAlTin 高熵合金披覆式塗層機械性質、熱性質與高溫氧化行為之研究
Study on Mechanical Properties, Thermal Properties and Oxidation Behavior of High-Entropy NixCo0.6Fe0.2CrySizAlTin Overlay Coatings
指導教授： 葉均蔚
Yeh, Jien-Wei
葉安洲
Yeh, An-Chou
口試委員: 洪健龍
Hong, Jian-Long
李勝隆
Lee, Sheng-Long
蔡哲瑋
Tsai, Che-Wei
學位類別： 博士
Doctor
系所名稱： 工學院 - 材料科學工程學系
Materials Science and Engineering
論文出版年： 2018
畢業學年度： 106
語文別： 英文
論文頁數： 160
中文關鍵詞： 高熵合金 、火花電漿燒結 、熱噴塗製程 、高溫氧化阻抗 、熱性質 、機械性質
外文關鍵詞： High-entropy alloy, Spark plasma sintering, Thermal spraying process, High-temperature oxidation resistance, Thermal properties, Mechanical properties
相關次數： 點閱：3  下載：0 
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    • 本研究設計NixCo0.6Fe0.2CrySizAlTin 高熵合金並以火花電漿燒結與熱噴塗製程製備高溫保護塗層。第一部分以火花電漿燒結法製備高熵合金試片，對微結構、高溫硬度、高溫熱傳導與熱膨脹係數、耐氧化性質以及氧化層生成與增厚行為做詳細探討，評估高熵合金作為高溫保護塗層之可行性，並與工業常用之MCrAlY (M = Ni and/or Co) 做比較，以做為工業應用之參考。第二部分則使用熱噴塗方式將高熵合金應用於熱阻絕層系統 [thermal barrier coating (TBC)] 作為黏結層 (bond coat)。首先比較傳統大氣電漿熔射 (APS)，高速火焰熔射 (HVOF) 與溫噴塗 (WS) 製程所製備之塗層的差異，包括機械性質以及抗氧化能力。接著以表現最佳的WS製程將高熵合金粉末噴覆於超合金基板做為與釔安定氧化鋯外層 (YSZ) 間的黏結層，探討在高溫環境下與基板以及陶瓷外層之附著性，用以評估高熵合金作為TBC系統中黏結層之可行性。
    第一部份之實驗結果顯示， HEAC 燒結試片在1100 ℃ 環境形成連續緻密的氧化鋁保護層 (α-Al2O3)，表現出與MCrAlY相似的優異氧化行為。且在1100 °C高溫環境仍保有相穩定與不錯的硬度，其硬度值可維持在230 Hv左右。而MCrAlY已經明顯軟化硬度值只有55 Hv。HEAC除了具有高硬度與優異的耐氧化能力之外，同時展現良好的熱阻抗力，1000 °C高溫熱傳導值比MCrAlY低30 %。經由計算結果證實，以HEAC取代MCrAlY作為保護層能進一步降低工件內部的溫度。此外，HEAC是體心立方 (BCC) 為主的結構，其熱膨脹係數也比面心立方 (FCC) 為主的MCrAlY低。熱膨脹係數對溫度作圖結果顯示，HEAC曲線比MCrAlY更貼近超合金基材曲線，高溫環境下預期能降低熱膨脹失配並減少塗層與基板間之裂痕產生。
    由於HEAC合金中的鈦元素在高溫下容易形成結構鬆散的氧化鈦 (TiO2)，對於釔安定氧化鋯 (YSZ) 之附著性不利。針對本研究第二部分熱阻障層系統之實驗，另外設計無鈦合金 HEACM. HEACM 合金粉末同樣先以火花電漿燒結製備試片以評估上述各項性質，包括硬度、熱傳導係數、熱膨脹係數、氧化增重測試以及氧化層成長機制等。實驗結果顯示SPS-HEACM之熱傳導係數與熱膨脹係數 (TC: 9.6 W/mK at RT, 19.3 W/mK at 1000 °C; average CTE: 13.2 × 10−6/K) 與SPS-HEAC相近 (TC: 9.8 W/mK at RT, 18.6 W/mK at 1000 °C; average CTE: 13.9 × 10−6/K)，硬度則稍低於 SPS-HEAC (HEACM: 980 Hv at RT; HEAC: 1045 at RT)。其氧化增重曲線與MCrAlY曲線相似且氧化實驗過程中沒有氧化鈦與氧化鉻層形成。
    本研究第二部份採用機械性質與氧化阻抗表現最佳之溫噴塗製程分別製備HEAC、HEACM以及MCrAlY黏結層；以大氣電漿熔射製備YSZ 陶瓷外層。1100 °C 循環熱處理實驗結果顯示，含有鈦及較多量鉻之HEAC在熱處理過程中產生大量的鉻鈦氧化物，導致在100週期時YSZ就剝落。而HEACM系統則有明顯改善，直到168周期才發生剝落。與傳統MCrAlY相比，高熵合金塗層具有較佳的硬度與熱阻抗，抗氧化力亦能媲美MCrAlY，在高溫環境下作為工件外部保護層應用極具潛力。但是作為TBC系統中的黏結層，則可能因為塗層厚度不足以及塗層有較多裂縫等問題，尚無法達到MCrAlY的使用壽命。

    This research proposes an overlay coating based on the high-entropy alloys (HEAs) composition NixCo0.6Fe0.2CrySizAlTin by using spark-plasma sintering and thermal spraying processes. In the first part, the microstructure, high-temperature hardness, oxidation kinetics, high-temperature heat conduction and thermal expansion behavior of spark plasma-sintered HEA specimens were investigated to evaluate the high-entropy alloys as a high-temperature protective coating for industrial applications. The conventional MCrAlY (M = Ni and/or Co) specimens were prepared by the same process for comparison. The second part utilized thermal spraying technique to prepare HEA coatings. Firstly, the characteristics of coatings prepared by atmospheric plasma spraying (APS), high speed flame spraying (HVOF) and warm spraying (WS) processes were compared, including mechanical properties and oxidation kinetics. The best-performed WS-HEA coatings were then applied to thermal barrier coating (TBC) systems as a bond coat. The TGOs (thermally ground oxides) growing behavior and the adhesion among YSZ top coat and HEA bond coat were investigated.
    For the first part, experimental results indicates that the spark plasma-sintered HEAC can form protective α-Al2O3 at 1100 °C and exhibits oxidation behavior similar to that of MCrAlY. It also exhibits good thermal stability and very high room-temperature hardness (1045 Hv) and a hot hardness of 230 Hv at 1100 °C whereas the hardness of MCrAlY dropped from 450 Hv to 55 Hv. Moreover, as compared to MCrAlY, the HEAC possesses a thermal conductivity lower than MCrAlY by 30% at 1000 °C. The heat insulation of TBC for turbine material can be improved by replacing MCrAlY to the HEAC. Besides, due to its BCC structure, the CTE of HEAC is smaller than MCrAlY and thus is expected to show more compatibility to the blade alloys or YSZ top coat by reducing the thermal mismatch along the interfaces of YSZ/HEAC and HEAC/substrate, respectively.
    However, the formation of Ti-Cr-Al mixed oxides above HEAC surface will be significantly detrimental to the adhesion to YSZ top coat when the HEAC bond coat is utilized to the TBC system. Therefore, a new alloy composition Ti-free with decreased Cr was designed (HEACM). This alloy was also prepared by SPS with the same sintering parameters as those used for HEAC for comparison. The experimental results show that the thermal conductivity and thermal expansion coefficient of SPS-HEACM (TC: 9.6 W/mK at RT, 19.3 W/mK at 1000 °C; average CTE: 13.2 × 10−6/K) are similar to those of SPS-HEAC (TC: 9.8 W/mK at RT, 18.6 W/mK at 1000 °C; average CTE: 13.9 × 10−6/K), and the hardness is just slightly lower than SPS-HEAC (HEACM: 980 Hv at RT, 213 Hv at 1100 °C; HEAC: 1045 at RT, 230 at 1100 °C). The oxidation weight-gain curve of HEACM is similar to the MCrAlY curve and no oxidation of titanium oxide and chromium oxide is formed during the cyclic oxidation experiment.
    For the second part, the warm-sprayed HEAC and HEACM coatings, which show the best performance in mechanical properties and oxidation resistance, were utilized to TBC system as a bond coat (with YSZ ceramic top coat and superalloy substrate). The results of 1100 ° C cyclic heat treatment show that the Ti-contained HEAC presented large amount of Ti-Cr-Al oxides at bond-coat/top-coat interface during heat treatment, resulting in earlier delamination of YSZ layer at 100th cycle. Meanwhile, the HEACM system did not exhibit Ti-Cr-Al oxides during heat treatment and its life had prolonged to 168th cycle. As compared to conventional MCrAlY coatings, the HEA coatings have higher hardness, better thermal resistance and comparable oxidation resistance, which show great potential as an external protective layer in high temperature environment. However, as a bond coat in the TBC system, the service life of HEA coatings has not reached MCrAlY level so far, which might be due to the insufficient thickness of bond coating and the insufficient soundness of HEA layer with more internal cracks.

    摘要 i Abstract iv Contents viii List of Figures xii List of Tables xviii Chapter 1 Introduction 1 Chapter 2 Background 4 2.1 Thermal Barrier Coating Systems 4 2.1.1 Yttria-Stabilized Zirconia 7 2.1.2 Metallic Bond Coat 9 2.1.3 Failure Mode of TBC System 12 2.2 Thermal Spraying Processes 16 2.2.1 Atmospheric Plasma Spraying Process 18 2.2.2 Detonation Spraying 21 2.2.3 High Velocity Oxy-fuel Spraying Process 23 2.2.4 Warm Spraying Process 25 2.2.5 Cold Spraying Process 27 2.3 Spark Plasma Sintering and Electron Beam Physical Vapor Deposition 30 2.3.1 Spark Plasma Sintering (SPS) 30 2.3.2 Electron Beam Physical Vapor Deposition (EB-PVD) 32 2.4 Review of Thermal-Sprayed High-Entropy Alloy Coatings 34 2.4.1 High-Entropy Alloy 34 2.4.2 Definition and Core Effects 36 2.4.3 Thermal-Sprayed High-Entropy Alloy Coatings 39 2.5 Purpose of This Study 45 Chapter 3 Experimental Procedure 47 3.1 Powder Preparation 49 3.2 Spark Plasma Sintering 52 3.3 Thermal Spraying Processes 54 3.4 Coating Characterization 56 3.4.1 Microstructures and Chemical Composition 56 3.4.2 Mechanical Properties 56 3.4.3 Thermal Conductivity 57 3.4.4 Coefficient of Thermal Expansion 57 3.4.5 Oxidation Kinetics 58 Chapter 4 Spark plasma-sintered HEA coatings 60 4.1 Effect of Sintering Temperature on the Properties of Spark Plasma-Sintered Ni0.2Co0.6Fe0.2CrSi0.2AlTi0.2 (HEAB) and NiCo0.6Fe0.2Cr1.5SiAlTi0.2 (HEAC) 60 4.1.1 Cross-sectional Microstructure, Mechanical and Thermal Properties 60 4.1.2 Oxidation Kinetics 65 4.2 Comparison of 900 °C-Sintered NiCo0.6Fe0.2Cr1.5SiAlTi0.2 and MCrAlY Coatings 68 4.2.1 Cross-sectional Microstructure, Chemical Composition and XRD Analysis 68 4.2.2 Hardness Test 73 4.3 Oxidation Kinetics 74 4.3.1 Cyclic Oxidation Weight-gain Test 74 4.3.2 Analysis of Surface Oxides (thermally grown oxides) 76 4.3.3 Growing Mechanism of Thermally Grown Oxide Layer 81 4.3.4 Elemental Inter-diffusion 86 4.4 Thermal Properties 89 4.4.1 High Temperature Thermal Conductivity 89 4.4.2 Coefficient of Thermal Expansion 95 4.5 Ti-free NiCo0.6Fe0.2Cr1.3SiAl Alloy (HEACM) 97 4.5.1 Microstructure, Mechanical and Thermal Properties 97 4.5.2 Oxidation Kinetic of HEACM 101 4.6 Summary 106 Chapter 5 Thermal-Sprayed HEA Coatings 109 5.1 Comparison of HEA Coatings Sprayed by APS, HVOF and WS Process 109 5.1.1 Microstructure and Mechanical Properties 109 5.1.2 Oxidation Kinetics 122 5.2 TBC Systems with HEA Bond Coat 126 5.2.1 Characteristics 126 5.2.2 1100 °C Cyclic Heat Treatment 131 5.3 Summary 136 Chapter 6 Conclusions 138 Contributions 143 Future Topics 144 References 145 Vita and Publication List 159

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