輕量化富鈦高熵合金設計及機械性質探討｜國立中央大學博碩士論文系統

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研究生：	彭柏森 Bo-Sen Peng
論文名稱：	輕量化富鈦高熵合金設計及機械性質探討 Alloy design and mechanical properties study of titanium-rich light-weight high-entropy alloy
指導教授：	鄭憲清
口試委員:
學位類別：	碩士 Master
系所名稱：	工學院 - 材料科學與工程研究所 Graduate Institute of Materials Science & Engineering
論文出版年：	2019
畢業學年度：	107
語文別：	中文
論文頁數：	119
中文關鍵詞：	輕量化、非等比例、高熵合金
外文關鍵詞：	light-weight, non-equiatomic, high-entropy alloy
相關次數：	點閱：17 下載：0
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高熵合金之於傳統合金擁有獨特的顯微結構以及優越的機械性質，在應用中引起極大的研究關注。過去十幾年，大部分的研究主要在多元等量的成分上。而本研究將探討非等量高熵合金之成分設計，欲設計出密度在5 g/cm3且具有高強度以及高延展性的高熵合金。
首先由低密度金屬元素Ti、Al開始進行成分設計並配合高熵合金相關參數，由四元合金Ti50系列(Ti50Al25V25-xCrx、Ti50Al25Nb25-xCrx、Ti50Al45-xNbxCr5)逐步至五元Ti60合金系列(Ti60Al40-x(NbVCr)X)，找出適當的合金成分進行微結構分析、機械性質分析、氧化分析以及電化學分析。根據XRD結果顯示，無論是Ti50或Ti60合金系統其微結構皆為單一BCC相；由密度分析結果顯示，五元合金較四元合金系統由更多原子種類結合，導致晶格扭曲效應更加明顯而造成體積膨脹現象；從硬度結果來看，在Ti50Al45-xNbxCr5系列合金中將Al含量由30%降至20%其硬度值從480Hv大幅下降至365Hv，顯示Ti、Al元素之間含量比對合金整體硬度有著非常大的影響力；以SEM觀察合金試片拉伸後之破斷面，可以在Ti60Al10(NbVCr)30中發現類似葉脈狀紋路的塑性行為，此合金成分在本研究中也具有最佳機械性質，其降伏強度1009MPa、抗拉強度1223MPa、塑性更高達27.1%；其磨耗性質也與商用合金Ti6Al4V相當。
在確定Ti60Al10(NbVCr)30合金具有優越的延展性之基本性質條件下，相信藉由冷軋變形使晶粒結構改變調整其機械性質，勢必能夠獲得具有更高強度且保有延展性之高熵合金。

High-entropy alloys (HEA) attract great attention in past few decades. Most HEA researches mainly concentrate on the heavier multi-principal elements with equiatomic or near-equiatomic alloys. In this study, we focus on the light-weight and non-equiatomic medium-entropy alloys (MEA) system with low density (below 5g/cm3). Series of non-equiatomic quaternary alloy system, Ti-Al-Cr-Nb、Ti-Al-Cr-V were firstly designed by using calculating parameter (∆S、∆H、δr), then further modified into quinary Ti-Al-Cr-Nb-V alloy system. All samples were prepared by vacuum arc melting and rapidly cooling process. The XRD results of Ti-Al-Cr-Nb 、Ti-Al-Cr-V and Ti-Al-Cr-Nb-V MEA reveal the single BCC structure. The hardness value of Ti60-Al-Cr-Nb reduced from 480Hv to 365Hv with decreasing the Al content which implies that the ratio of Ti/ Al elements plays an important role on the alloy hardness. The optimum mechanical performance occurs at Ti60-Al-Cr-Nb-V MEA with tensile yield strength of 1009 MPa, fracture strength of 1223 MPa, and plastic strain of 27.1%. In summary. the Ti60-Al-Cr-Nb-V MEA not only possesses higher mechanical properties than the commercial Ti6Al4V alloy, but also has similar density, wear resistance, and oxidation behavior to commercial Ti alloys. Therefore, it is believed that the Ti60-Al-Cr-Nb-V MEA can be a promising light-weight structure material for the applications of transportation vehicles and sport equipment.

總目錄
摘要    i
Abstract    ii
總目錄    vi
表目錄    xi
圖目錄    xiii
第一章 緒論    1
1-1前言    1
1-2研究目的    1
第二章 文獻回顧    3
2-1高熵合金之發展    3
2-1-1高熵合金定義    3
2-2 高熵合金之固溶體形成條件    4
2-3 高熵合金四大效應[13]    6
2-3-1高熵效應    6
2-3-2晶格應變效應    8
2-3-3延遲擴散效應    8
2-3-4雞尾酒效應    9
2-4 高熵合金之特性    9
2-5 機械行為之影響因素    11
2-5-1晶體結構    11
2-5-2固溶強化    11
2-6 高熵合金之成分設計    12
2-6-1低密度高熵合金    12
2-6-2非等量成分設計    14
第三章 實驗方法與步驟    21
3-1 合金設計之相關參數計算    21
3-2 高熵合金試片製備    21
3-2-1 合金成分配製    22
3-2-2 合金熔煉    22
3-2-3 高熵合金板材製作-墜落式鑄造    22
3-3 合金密度量測    23
3-4 高熵合金微觀組織分析    23
3-4-1 X光繞射儀(XRD)    23
3-4-2光學顯微鏡(Optical Microscopy)    24
3-4-3 掃描式電子顯微鏡(SEM)    24
3-4-4 能量散射光譜儀(EDS)    24
3-4-5 穿透式電子顯微鏡(TEM)    25
3-5 熱性質分析    25
3-5-1熱示差掃描熱量分析(DSC)    25
3-5-2均質化熱處理    26
3-5-3氧化測試    26
3-6 機械性質分析    26
3-6-1試片製作    26
以3-6-2維氏硬度分析    27
3-6-3壓縮測試分析    27
3-6-4拉伸測試分析    28
3-6-5耐磨耗測試    29
3-7電化學分析    29
第四章 結果與討論    46
4-1 合金成份設計-四元合金系列    46
4-1-1固溶體之相關參數計算    46
4-1-2 X-ray繞射分析    48
4-1-3 機械性質分析    48
4-2 合金成份設計-五元合金系列    49
4-2-1固溶體之相關參數計算    50
4-2-2 X-ray繞射分析    50
4-2-3 硬度分析    51
4-3 晶格常數    51
4-4 合金密度    52
4-5 CALPHAD之相圖模擬計算    52
4-6 均質化熱處理溫度之選擇    53
4-7微觀組織分析    53
4-7-1合金試片之表面形貌觀察    53
4-7-2成分分析    54
4-8 X-ray繞射分析    54
4-9 機械性質分析    54
4-9-1硬度分析    54
4-9-2壓縮測試分析    55
4-9-3拉伸測試分析    55
4-9-4磨耗分析    56
4-10 OM微觀結構分析    57
4-11 TEM分析    57
4-12 電化學分析    57
4-13 氧化測試分析    58
第五章 結論    88
第六章 參考文獻    89
表目錄
表3-1 相關元素之混合焓 (J/mol)    31
表3-2所選取元素之基本性質    31
表3-3 Ti50合金元素系列表    32
表4-1合金設計之固溶體形成相關參數表    60
表4-2 Ti50合金系列之硬度值    61
表4-3 Ti50Al25Nb25-xCrx合金之壓縮性質測試    61
表4-4 Ti60合金元素系列表    62
表4-5合金設計之固溶體形成相關參數表    62
表4-6 Ti60合金系列之硬度值    62
表4-7不同合金系列之晶格常數    63
表4-8合金密度量測結果    64
表4-9熱性質分析結果    65
表4-10 Ti60Al10(NbVCr)30合金之EDS成分分析    65
表4-11 Ti60Al16(NbVCr)24合金之EDS成分分析    65
表4-12 Ti60Al10(NbVCr)30及Ti60Al16(NbVCr)24合金熱處理前後硬度值    65
表4-13 Ti60Al10(NbVCr)30及Ti60Al16(NbVCr)24合金熱處理前後壓縮性質    66
表4-14 Ti60Al10(NbVCr)30及Ti60Al16(NbVCr)24合金熱處理前後拉伸性質    66
表4-15 磨耗測試結果    67
表4-16電化學測試結果    67
表4-17 不同時間於600℃持溫之氧化測試結果    67
圖目錄
圖2-1合金成分配置示意圖    15
圖2-2 二元至七元Cu-Ni-Al-Co-Cr-Fe-Si合金之X光繞射分析    15
圖2-3不同合金數目與混合熵值對照圖    16
圖2-4 (左)單一元素之簡單固溶結構；(右)高熵合金之複雜固溶結構    16
圖2-5 (a)單一元素之X光繞射；(b)高熵合金之X繞射    17
圖2-6 AlCoCrCuFeNi 合金鑄造態下的TEM微結構影像    17
圖2-7 Fe、Co、Ni、Cr、Mn在不同基地下的活化能比較    18
圖2-8 AlxCoCrCuFeNi合金隨Al含量變化之硬度曲線圖    19
圖2-9 BCC結構之CrMnFiCoNi合金於不同溫度下之機械性質    19
圖2-10 Nb25Mo25Ta25W25及V20Nb20Mo20Ta20W20於不同退火溫度下之壓縮性質    20
圖3-1合金試片製作及實驗分析流程圖    33
圖3-2 電弧融煉爐(大arc)    34
圖3-3 電弧融煉爐使用之氬焊機(大arc)    34
圖3-4 電弧融煉    35
圖3-5 合金鑄錠樣貌    35
圖3-6 噴砂機    36
圖3-7 墜落式鑄造電弧融煉爐(小arc)    36
圖3-8 電弧融煉爐使用之氬焊機(小arc)    37
圖3-9合金板材    37
圖3-10 X-ray繞射分析儀(XRD)    38
圖3-11 光學顯微鏡(OM)    38
圖3-12超高解析冷場發射掃描式電子顯微鏡(SEM)    39
圖3-13 能量分散質譜儀(EDS)    39
圖3-14 穿透式電子顯微鏡(TEM, JEOL, JEM-2100)    40
圖3-15 聚焦離子束(FIB, FEI, Versa3D)    40
圖3-16 高溫熱卡掃描分析儀(DSC)    41
圖3-17 真空管狀加熱爐    41
圖3-18 維式硬度機    42
圖3-19 壓縮試片    42
圖3-20 萬能試驗機(MTS)    43
圖3-21 拉伸試片    43
圖3-22 磨耗測試儀    44
圖3-23 腐蝕測試之襄埋試片    44
圖3-24 恆電位儀(Autolab PGStat 302)    45
圖4-1 Ti50Al25V25-XCrX系列之X光繞射結果    68
圖4-2 Ti50Al25Nb25-XCrX系列之X光繞射結果    68
圖4-3 Ti50Al45-XNbXCr5系列之X光繞射結果    69
圖4-4 Ti50Al25Nb25-XCrX與Ti50Al25V25-XCrX系列之硬度測試結果    69
圖4-5 Ti50Al25Nb25-XCrX合金壓縮測試結果    70
圖4-6 Ti50Al45-XNbXCr5系列之硬度測試結果    70
圖4-7 Ti60Al40-X(NbVCr)X系列之X光繞射結果    71
圖4-8 Ti60Al40-X(NbVCr)X系列之硬度測試結果    71
圖4-9 Ti60Al40-X(NbVCr)X合金成分之CALPHAD相圖模擬結果    72
圖4-10 Ti60Al10(NbVCr)30合金之DSC曲線    73
圖4-11 Ti60Al16(NbVCr)24合金之DSC曲線    73
圖4-12 Ti60Al10(NbVCr)30合金之鑑定區域及mapping鑑定結果    74
圖4-13 Ti60Al16(NbVCr)24合金之鑑定區域及mapping鑑定結果    75
圖4-14 Ti60Al10(NbVCr)30的X光繞射結果    76
圖4-15 Ti60Al16(NbVCr)24的X光繞射結果    76
圖4-16不同合金熱處理前後硬度值    77
圖4-17合金試片壓縮前後對照圖，(左)壓縮前；(右)壓縮後    77
圖4-18 Ti60Al10(NbVCr)30合金熱處理前後壓縮測試結果    78
圖4-19 Ti60Al16(NbVCr)24合金熱處理前後壓縮測試結果    78
圖4-20合金試片拉伸前後對照圖，(左)拉伸前；(右)拉伸後    79
圖4-21 Ti60Al10(NbVCr)30及Ti60Al16(NbVCr)24合金熱處理前後拉伸結果    79
圖4-22 Ti60Al40-X(NbVCr)X合金拉伸測試結果    80
圖4-23 Ti60Al10(NbVCr)30合金之破斷面: (a)100倍，(b)1000倍    81
圖4-24 Ti60Al10(NbVCr)30合金之破斷側面: (a)100倍，(b)500倍    81
圖4-25 Ti60Al16(NbVCr)24合金之破斷面: (a)100倍，(b)1000倍    82
圖4-26 Ti60Al16(NbVCr)24合金之破斷側面: (a)200倍，(b)500倍    82
圖4-27 Ti60Al10(NbVCr)30、Ti60Al16(NbVCr)24以及Ti6Al4V磨耗結果    83
圖4-28 Ti60Al10(NbVCr)30合金經腐蝕後之表面: (a)50倍，(b)100倍    84
圖4-29 Ti60Al16(NbVCr)24合金經腐蝕後之表面: (a)50倍，(b)100倍    84
圖4-30 Ti60Al10(NbVCr)30合金之TEM影像圖    85
圖4-31 Ti60Al10(NbVCr)30合金zone axis [133]之diffraction pattern    85
圖4-32 Ti60Al10(NbVCr)30合金之(a)明視野(b)暗視野    86
圖4-33 不同材料在3.5wt%氯化鈉水溶液之動態極化曲線    87
圖4-34 不同材料在600˚C下持溫12小時的重量變化曲線圖    87


                                

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