鎂基複合材料Mg-Ca / MgO經等通道轉角擠製對機械性質與耐蝕性之研究

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研究生：	陳易寬 Yi-Kuan Chen
論文名稱：	鎂基複合材料Mg-Ca / MgO經等通道轉角擠製對機械性質與耐蝕性之研究 Effect of Equal Channel Angular Pressing on the mechanical properties and corrosion resistance of Mg-Ca / MgO magnesium matrix composites
指導教授：	黃崧任 Song-Jeng Huang
口試委員:	丘群 Chiu Chun 李天錫 Tien-Hsi Lee 曾有志 Yu-Chin Tzeng
學位類別：	碩士 Master
系所名稱：	工程學院 - 機械工程系 Department of Mechanical Engineering
論文出版年：	2023
畢業學年度：	111
語文別：	中文
論文頁數：	121
中文關鍵詞：	鎂基複合材料、等通道轉角擠製、機械性質、耐蝕性質
外文關鍵詞：	magnesium matrix composites, equal-channel angular pressing, mechanical properties, corrosion resistance
相關次數：	點閱：331 下載：0
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上一筆

鎂合金作為可生物降解之植入物被廣泛研究，但由於鎂合金在人體內的腐蝕速率過快，造成許多不利影響。本實驗利用等徑轉角擠製ECAP及強化相之添加，加以改善可生物降解之鎂合金。以鎂鈣合金(Mg-1Ca)作為實驗基材，用奈米級之MgO顆粒作為添加的強化相，添加量分別為0、1、2 wt. %，使用重力鑄造法製備鎂基複合材料。隨後鑄錠切割成ECAP試棒，再進行450 °C之T4固溶處理，持溫24小時，再以等徑轉角擠製加工（ECAP）之Bc路徑進行擠製，加工道次是分別為1、4道次，研究不同比例之Mg-1Ca / MgO鎂基複合材料及不同道次之微觀結構、機械性質及耐腐蝕性的影響。
實驗結果中發現，添加MgO後因散布強化有效增加極限抗拉強度及降伏強度，但會因強化項為脆性且部分團聚的關係使材料伸長率下降，而鎂基複合材料藉由後續的ECAP擠製加工使晶粒產生動態再結晶而晶粒細化，其機械性質進一步提升，且經過4道次ECAP後，含有強化項的鎂基複合材料延展性比無添加強化項的更加優異。在電化學實驗中，添加過多的MgO會使耐蝕力下降，但透過ECAP加工後能藉由晶粒細化使保護膜更能抵抗腐蝕，提升耐蝕能力。

Magnesium alloys are widely studied as biodegradable implants, but due to the rapid corrosion rate of magnesium alloys in human body, many adverse effects are caused. In this experiment, the magnesium alloys were improved by using equal channel angular pressing and the reinforcement.
Mg-1Ca was used as the experimental substrate, and nano MgO particles were used as the reinforcement with the addition amounts of 0, 1, and 2 wt. %, respectively. After solution treatment, the cast ingots were extruded by equal channel angular pressing process, and the number of passes was 1 and 4 respectively.
The experimental results show that the addition of MgO to the material effectively increases the ultimate tensile strength and yield strength due to the dispersal strengthening, but the elongation decreases due to the agglomeration of the reinforcement. The mechanical properties of the magnesium-based composite material were further improved by the ECAP process, which resulted in dynamic recrystallization and grain refinement.
In electrochemical experiments, the addition of too much MgO will reduce the corrosion resistance, but the ECAP process can make the protective film more resistant to corrosion by grain refinement and improve the corrosion resistance.

摘要    i
Abstract    ii
誌謝    iii
目錄    iv
圖目錄    ix
表目錄    xv
第一章 緒論    1
1.1 前言    1
1.2 文獻回顧    4
1.2.1 鎂鈣合金相關文獻    4
1.2.2 鑄造技術相關文獻    7
1.2.3 機械加工對鎂合金影響相關文獻    8
1.2.4 鎂基複合材料相關文獻    18
1.2.5 MgO之生物相容性相關文獻    25
1.3 文獻回顧整理    26
1.4 研究動機與目的    27
第二章 研究理論基礎    30
2.1 鎂之基本性質    30
2.2 鎂主要優缺點    31
2.3 金屬元素鈣對鎂合金及生物相容性影響    33
2.4 鎂腐蝕概論    35
2.4.1鎂的腐蝕機制    35
2.4.2 不同類型腐蝕的說明    36
2.5 鎂基複合材料強化理論    39
2.5.1 晶粒細化強化    40
2.5.2 熱膨脹係數差異之影響    40
2.5.3 Orowan強化與散佈強化    40
2.5.4 負荷影響    41
2.5.5 析出強化    41
2.6 鎂合金鑄造法    42
2.6.1砂模鑄造法 (Sand Casting)    42
2.6.2重力鑄造法 (Gravity Casting)    42
2.6.3壓力鑄造法    42
2.6.4 真空鑄造法    43
2.7氧化鎂(MgO)之特性    43
2.8鎂合金熱處理    43
2.9等通道轉角擠製（Equal Channel Angular Pressing, ECAP）    44
2.10 腐蝕電化學分析原理    49
2.10.1 腐蝕電化學量測    49
2.10.2 開路電位    49
2.10.3 Tafel 外推法    50
2.10.4 動電位極化法(Potentiodynamic polarization, PDP)    51
第三章 實驗方法與步驟    52
3.1 實驗方式    52
3.2實驗材料    54
3.3實驗設備    55
3.3.1電阻式熔煉爐    55
3.2.2 等徑轉角擠製機 (Equal Channel Angular Pressing)    58
3.3.3高溫熱處理爐    60
3.3.4 濕式研磨／拋光機    61
3.3.5 光學顯微鏡 (Optical Microscope, OM)    61
3.3.6 掃描式電子顯微鏡 (Scanning Electron Microscope, SEM)    62
3.3.7 愛克斯光繞射 (X-ray Diffraction, XRD)    63
3.3.8 拉伸試驗機 (Material Test System, MTS)    64
3.3.9 微型維克氏硬度機(Micro-Vickers Hardness Tester)    66
3.3.10 恆電位儀及電化學三電極系統    67
3.4 實驗規劃    71
3.4.1 鎂基複合材料製備    71
3.4.2 熱處理    73
3.4.3 ECAP擠製加工及試棒規劃    73
3.4.4 拉伸試片規劃    73
3.4.5電化學試片規劃    74
3.4.6 HBSS模擬溶液調配    75
第四章 結果與討論    76
4.1 Mg-1Ca/MgO鎂基複合材料表面微觀結構分析    76
4.1.1 OM微觀結構分析    76
4.1.2 平均晶粒尺寸分析    82
4.2 Mg-1Ca/MgO鎂基複合材料成分分析    85
4.2.1 材料密度分析    85
4.2.2 XRD材料成分分析    86
4.2.3 SEM微觀組織材料分析    88
4.3 Mg-1Ca/MgO鎂基複合材料機械性質分析    92
4.3.1拉伸試驗    92
4.4.2拉伸試片斷面分析    97
4.4.3硬度試驗    103
4.4鎂基複合材料在HBSS中的電化學分析    106
第五章 結論    113
第六章 未來研究方向    115
參考文獻    116




 
圖目錄
圖1-1鎂鈣合金OM圖    4
圖1-2鈣含量對鎂鈣合金硬度值的影響    5
圖1-3鎂鈣合金在 Kokubo 溶液中的極化曲線    5
圖1-4鎂鈣合金之極化電阻    7
圖1-5電阻式熔煉爐式意圖    8
圖1-6鎂鈣合金拉伸性能圖    9
圖1-7 AZ31鎂合金維氏硬度圖    10
圖1-8 AZ31鎂合金析氫量圖    11
圖1-9 AZ31鎂合金經不同道次ECAP的工程應力-應變曲線    12
圖1-10 AZ31鎂合金在SBF中進行SSRT的應力應變圖    12
圖1-11 AZ91之OM圖    14
圖1-12經不同道次ECAP之AZ91的腐蝕重量損失圖    14
圖1-13 ME21鎂合金在空氣、蒸餾水和漢克斯溶液中的SSRT曲線    15
圖1-14未加工及經ECAP後純Mg、Mg-1Ca和Mg-2Sr之SEM圖    17
圖1-15經ECAP後純Mg、Mg-1Ca和Mg-2Sr之拉伸性能    17
圖1-16擠壓態及經ECAP後純Mg、Mg-1Ca和Mg-2Sr之腐蝕後重量損失圖    17
圖1-17不同溫度及下壓率軋製之Mg-1Ca在SBF中的腐蝕率    18
圖1-18不同β-TCP含量之鎂合金機械性能    19
圖1-19 Mg-Zn-Ca /MgO在SBF中的動電位極化曲線    21
圖1-20 Mg-Zn-Ca /β-TCP經ECAE後在37°C下SBF中的極化曲線    22
圖1-21 AZ61/Al2O3/SiC的 (a) 硬度圖和 (b)應力-應變圖    24
圖1-22 AZ61/Al2O3/SiC複合材料的斷裂表面    25
圖1-23 MgO、 ZnO 及MgO/ZnO 在外周血單核細胞中的生物相容性測定    26
圖2-1鎂的六方最密堆積晶體結構    30
圖2-2 Mg-Ca二元相圖    34
圖2-3等通道轉角擠製示意圖    45
圖2-4等通道轉角擠製加工路徑示意圖    46
圖2-5四種不同路徑的旋轉角度及方向    47
圖2-6單次擠製通過模具中的剪切示意圖：X、Y和Z為三個正交的觀測面    48
圖2-7ECAP加工路徑特性    48
圖2-8 Tafel 外推法    50
圖3-1實驗流程圖    53
圖3-2 Pure Mg之外觀圖    54
圖3-3 Mg-30Ca之外觀圖    54
圖3-4奈米級MgO之SEM圖    55
圖3-5電阻式熔煉爐外觀    56
圖3-6電阻式熔煉爐示意圖    57
圖3-7熔煉工具    57
圖3-8喇叭型模具及尺寸圖    58
圖3-9等徑轉角擠製機實體圖    59
圖3-10模角(Φ)120°、外側圓角(Ψ)0°模具內部示意圖    59
圖3-11高溫熱處理爐    60
圖3-12濕式研磨/拋光機外觀圖    61
圖3-13光學顯微鏡    62
圖3-14高解析度場發射掃描式電子顯微鏡 7900F    63
圖3-15 D2 PHASER 粉末X 光繞射儀    64
圖3-16拉伸試驗機    65
圖3-17微型維克氏硬度機    67
圖3-18硬度測試示意圖    67
圖3-19 Solartron SI 1287    69
圖3-20 Solartron SI 1260    69
圖3-21密封五口瓶    69
圖3-22白金片電極    70
圖3-23飽和氯化銀電極    70
圖3-24電化學冷鑲埋試片正、背面圖    70
圖3-25 ECAP棒材規劃圖    72
圖3-26 拉伸試片尺寸規格    74
圖4-1 As-cast Mg-1Ca之OM圖    77
圖4-2 Mg-1Ca經T4固溶處理之OM圖    77
圖4-3 Mg-1Ca經T4固溶處理之OM圖    78
圖4-4 Mg-1Ca/ 1 wt.% MgO經T4固溶處理之OM圖    78
圖4-5 Mg-1Ca/ 2 wt.% MgO經T4固溶處理之OM圖    79
圖4-6 Mg-1Ca經1道次ECAP之OM圖    79
圖4-7 Mg-1Ca/ 1 wt.% MgO經1道次ECAP之OM圖    80
圖4-8 Mg-1Ca/ 2 wt.% MgO經1道次ECAP之OM圖    80
圖4-9 Mg-1Ca經4道次ECAP之OM圖    81
圖4-10 Mg-1Ca/ 1 wt.% MgO經4道次ECAP之OM圖    81
圖4-11 Mg-1Ca/ 2 wt.% MgO經4道次ECAP之OM圖    82
圖4-12平均晶粒尺寸    84
圖4-13 MgO之XRD圖    86
圖4-14 Mg-1Ca經不同ECAP道次擠製之XRD圖    87
圖4-15 Mg-1Ca/1 wt.% MgO經不同ECAP道次擠製之XRD圖    87
圖4-16 Mg-1Ca/2 wt.% MgO經不同ECAP道次擠製之XRD圖    88
圖4-17 Mg1Ca鎂基複合材料之SEM及EDS圖    89
圖4-18 (A) Mg1Ca鎂基複合材料EDS圖中之強化相MgO    90
圖4-19 (B) Mg1Ca鎂基複合材料EDS圖中之β相Mg2Ca    90
圖4-20 (C) Mg1Ca鎂基複合材料EDS圖中之基體Mg    91
圖4-21鎂基複合材料MgO團聚現象之SEM圖    91
圖4-22 鎂基複合材料最大拉伸應力    95
圖4-23 鎂基複合材料降伏強度    95
圖4-24 鎂基複合材料伸長率    96
圖4-25 Mg-1Ca之SEM拉伸斷面圖    99
圖4-26 Mg-1Ca經1道次ECAP之SEM拉伸斷面圖    99
圖4-27 Mg-1Ca經4道次ECAP之SEM拉伸斷面圖    100
圖4-28 Mg-1Ca/1wt.%MgO之SEM拉伸斷面圖    100
圖4-29 Mg-1Ca/1wt.%MgO經1道次ECAP之SEM拉伸斷面圖    101
圖4-30 Mg-1Ca/1wt.%MgO經4道次ECAP之SEM拉伸斷面圖    101
圖4-31 Mg-1Ca/2wt.%MgO之SEM拉伸斷面圖    102
圖4-32 Mg-1Ca/2wt.%MgO經1道次ECAP之SEM拉伸斷面圖    102
圖4-33 Mg-1Ca/2wt.%MgO經4道次ECAP之SEM拉伸斷面圖    103
圖4-34 Mg-1Ca經不同ECAP擠製道次之硬度圖    109
圖4-35 Mg-1Ca添加不同重量百分比之MgO之動電位極化曲線圖    109
圖4-36 Mg-1Ca經不同ECAP加工道次之動電位極化曲線圖    108
圖4-37 Mg-1Ca/ 1 wt.%經不同ECAP加工道次之動電位極化曲線圖    110
圖4-38 Mg-1Ca /2 wt.%經不同ECAP加工道次之動電位極化曲線圖    110
圖4-39 Mg-1Ca鎂基複合材料經不同ECAP加工道次之開路電位圖    111
圖4-40 Mg-1Ca鎂基複合材料經不同ECAP加工道次之腐蝕電流密度圖    112
 
表目錄
表1-1鎂鈣合金與人體皮質骨的彎曲性能    6
表1-2鎂鈣合金的壓縮性能    6
表1-3鎂鈣合金腐蝕速率表    9
表1-4 AZ31鎂合金殘餘應力表    10
表1-5 AZ31鎂合金經不同道次ECAP的腐蝕電位及腐蝕電流密度    12
表1-6未加工與經ECAP加工之鎂合金在不同溶液中的拉伸性能    15
表1-7 β-TCP鎂基複合材料的腐蝕電位及腐蝕電流    19
表1-8 α-TCP鎂基複合材料電化學參數表    20
表1-9 Mg-Zn-Ca /MgO的鑄態和擠壓態的晶粒尺寸    21
表2-1鎂之物理參數表    31
表2-2天然骨與各種植入材料的物理和機械性能比較    32
表3-1 Pure Mg純鎂錠成分表    54
表3-2 Mg-30Ca 鎂鈣合金成分表    55
表3-3 腐蝕液配方    61
表3-4 模擬體液SBF成分表    71
表4-1平均晶粒尺寸下降百分比    85
表4-2鎂基複合材料密度表    85
表4-3鎂基複合材料最大拉伸應力及提升百分比    96
表4-4鎂基複合材料降伏強度及提升百分比    97
表4-5鎂基複合材料伸長率及提升百分比    97
表4-6鎂基複合材料之硬度值及提升百分比    105
表4-7鎂基複合材料經不同ECAP加工道次的各項腐蝕數據    111


                                

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全文公開日期 2025/03/07 (校內網路)
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