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| DC 欄位 | 值 | 語言 |
|---|---|---|
| dc.contributor.advisor | 李岳聯(Yueh-Lien Lee) | |
| dc.contributor.author | Chang-Yang Hsieh | en |
| dc.contributor.author | 謝鎮洋 | zh_TW |
| dc.date.accessioned | 2022-11-25T06:34:23Z | - |
| dc.date.copyright | 2022-02-21 | |
| dc.date.issued | 2022 | |
| dc.date.submitted | 2022-02-14 | |
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| dc.identifier.uri | http://tdr.lib.ntu.edu.tw/jspui/handle/123456789/82251 | - |
| dc.description.abstract | 本研究於不燃型鎂合金Mg-8Al-4Ca 進行表面化成處理與腐蝕，該鎂合金添加金屬元素後析出二次相成為雙相合金，浸泡於水溶液時易產生伽凡尼腐蝕。透過 SKPFM量測表面電位，發現二次相鋁二鈣有較低的表面電位，並可能扮演微陽極加速腐蝕。同時透過 TEM 表面分析，發現在水溶液環境時二次相鋁二鈣確實有較快的腐蝕速率，且當進行硝酸鈰化成反應時，二次相的存在也會影響鎂底材的析氫速率，使 α-Mg 有較快的析氫速率。此外，進行化成處理前，將試片浸泡於去離子水將表面的二次相溶解，會產生氫氧化鋁（〖Al(OH)〗_3）的腐蝕產物，由於該層的存在使得硝酸鈰化成處理無需透過底材溶解，僅透過置換反應便可使化成皮膜沈積於試片表面達到保護試片的作用。同時 〖Al(OH)〗_3 層的存在也使試片得到進一步保護，透過電化學與析氫實驗量測試片的抗蝕能力時，優先浸泡去離子水產生並化成後的試片都有最優異的表現。 | zh_TW |
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| dc.description.tableofcontents | 總目錄 致謝 i 中文摘要 ii Abstract iii 總目錄 iv 圖目錄 vii 表目錄 xi 第1章 前言 1 第2章 文獻回顧 2 2.1不燃型鎂合金與元素添加 3 2.1.1鋁 3 2.1.2鈣 5 2.1.3錳 6 2.2鎂合金的腐蝕 7 2.2.1鎂合金腐蝕產物及微結構 7 2.2.2負差值效應 12 2.3鎂合金化成處理 22 2.3.1鉻酸鹽化成處理 23 2.3.2錳酸鹽化成處理 24 2.3.3鈰酸鹽化成處理 25 第3章 實驗方法 28 3.1鎂合金試片前處理 29 3.1.1試片之命名 29 3.1.2 浸泡去離子水 30 3.1.3化成溶液配置與浸泡 30 3.2微結構分析 31 3.2.1 SEM 表面形貌分析 31 3.2.2 TEM 橫截面結構觀察 31 3.3 EDS 成分分析 33 3.4電化學性質分析 33 3.4.1動電位極化曲線 33 3.4.2析氫實驗 34 3.5 AFM 原子力顯微鏡 35 第4章 實驗結果 36 4.1浸泡水溶液之腐蝕行為 36 4.1.1浸泡前底材之表面形貌 36 4.1.2浸泡氯化鈉溶液 38 4.1.3 Mg_DI之SEM表面影像 39 4.1.4 Mg_DI之TEM橫截面影像 40 4.2短時間化成處理 45 4.2.1浸泡60秒OCP監測 45 4.2.2 Ce初期 SEM 表面形貌 46 4.2.3 Ce初期 TEM 橫截面形貌 49 4.2.4 Ce_DI初期 SEM 表面形貌 52 4.2.5 Ce_DI初期 TEM 橫截面影像 54 4.3長時間化成處理 61 4.3.1 Ce、Ce-DI浸泡 60 秒 SEM 影像 61 4.3.2 Ce浸泡60秒 TEM 橫截面影像 64 4.3.3 Ce-DI 浸泡 60 秒 TEM 橫截面影像 66 4.4 化成皮膜電化學及抗蝕性分析 70 4.4.1開路電位量測 70 4.4.2動電位極化量測 71 4.4.3析氫速率量測 73 第5章 討論 76 5.1 二次相組成 76 5.2 水溶液之腐蝕行為 79 5.3化成反應機制 83 5.4兩相對化成反應之影響 85 5.5試片化成60秒OCP監測 88 5.6二次相對抗蝕性之影響 90 第6章 結論 91 第7章 未來展望 92 參考文獻 93 圖目錄 圖2 1鎂鋁平衡相圖[37] 4 圖2-2高溫中氧化膜之厚度比較[42] 5 圖2 3鎂鈣平衡相圖[37] 6 圖2 4鎂錳平衡相圖[37] 6 圖2 5鎂的 Pourbaix Diagram [48] 7 圖2-6鎂在 0.1M 、 0.01M 硫酸鈉溶液中浸泡 21 小時後對腐蝕產物的電化學交流阻抗分析結果[51] 8 圖2 7 純鎂浸泡於純水 1 分鐘的 XPS 縱深分析圖 O1s 光譜[53] 9 圖2-8 表面氫氧化鎂層與氧化鎂層厚度隨浸泡時間變化關係圖[55] 10 圖 2-9 對腐蝕產物 (a) 外層與 (b) 內層的選區繞射圖 (c) 腐蝕產物與底材界面處擇區繞射影像，圈選氧化鎂多晶環上 (200) 繞射點形成[56]。 11 圖 2-10 純鎂浸泡於純水 48 小時的雙層結構示意圖[53] 11 圖2-11 (a)浸泡24 小時 5 wt.% NaCl溶液 STEM -HAADF 影像， 12 圖2-12 (a) SVET 裝置架設 (b) 鎂在腐蝕發生處、腐蝕產物上與腐蝕前緣等區域陰陽極的分佈與電流大小[66]。 15 圖2-13 (a)鎂腐蝕過程電流分佈示意圖(b)假設一價鎂貢獻之電流分佈示意圖[66] 15 圖2-14 鎂電極在不同陽極電流密度下表面形貌[68] 16 圖2-15 (a) 腐蝕過程中鎂溶解反應的示意圖，(b)Mg 上暗區中間物種與腐蝕產物的混合物示意圖[68] 17 圖2 16惰性金屬沈積後產生陰極活性區之示意圖[56] 18 圖2-17 (a)為腐蝕產物 SEM 表面形貌(b)為試樣橫截面 STEM HAADF 影像[56] 19 圖2 18 陽極溶解 ultra-high purity Mg 與 high purity Mg 析氫活性變化量[72] 19 圖2-19析氫反應的即時攝影圖與示意圖[74] 21 圖2-20 ToF-SIMS 對鎂試樣浸泡於純水 2 分鐘之縱深分析結果[76] 22 圖2 21 AZ31B 鎂合金浸泡於錳酸鹽化成液中 90 秒的 TEM 橫截面微結構圖[88] 25 圖2 22 (a) 未經酸洗前處理AZ31試片浸泡硝酸鈰之 SEM 表面形貌(b) 經過HF酸洗前處理後之鈰酸鹽皮膜之 SEM 表面形貌[92] 27 圖2 23研磨完的 AZ31 浸泡於鈰酸鹽化成溶液中的 TEM 橫截面圖[92] 27 圖2 24 經 HF 酸洗前處理之 AZ31 浸泡鈰酸鹽化成溶液中 TEM 橫截面圖[92] 27 圖3-1實驗流程圖 28 圖3-2 (a) Mg 試片 (b) Mg_DI試片 30 圖3-3 (a) Ce 試片(b) Ce-DI 試片 30 圖3-4 析氫試驗裝置示意圖 34 圖3-5 AFM 儀器圖 35 圖4-1 不燃型鎂合金試片浸泡水溶液前形貌，圖 (a) SEM影像，圖 (b) BSE 影像 37 圖4-2 不燃型鎂合金試片浸泡水溶液前各元素 Mapping 結果。圖 (a) 為 SEM 影像；圖 (b)、(c)、(d)、(e)、(f) 為對應元素分佈。 38 圖4-3 不燃型鎂合金試片浸泡 NaCl 溶液1小時之表面影像，圖 (a) 腐蝕產物之表面形貌；(b) BSE 影像之表面形貌；(c)、(d) 腐蝕產物之高倍率影像。 39 圖4-4 浸泡 1 小時去離子水之 Mg_DI 試片表面影像，圖 (a) 腐蝕產物表面形貌；(b) BSE 影像之表面形貌；(c)、(d) 缺口處之高倍率影像。 40 圖4-5 Mg_DI 試片之橫截面影像組圖 41 圖4-6 Mg_DI 試片二次相與腐蝕產物之橫截面影像組圖 41 圖4-7 Mg_DI 試片元素Mapping結果，(a) 為 BF 影像；(b)、(c)、(d)、(e)、(f)、(g) 為對應元素分佈 42 圖4-8 Mg_DI 二次相腐蝕產物之橫向 line scan 元素分析結果 43 圖4-9 Mg_DI 試片之二次相腐蝕產物縱向line scan 元素分析結果 44 圖4-10 二次相腐蝕產物之diffraction pattern影像 44 圖4-11 Ce、Ce_DI 兩試片化成 60 秒之 OCP 圖 46 圖4-12 (a) Ce 試片化成 10 秒 SEM 影像；(c) 高倍率影像；(b)、(d) BSE影像 47 圖4-13 (a) Ce 試片化成 30 秒 SEM 影像；(c) 高倍率影像；(b)、(d) BSE 影像 48 圖 4-14 Ce 試片化成1秒之橫截面影像組圖 49 圖4-15 Ce 試片化成1秒之元素 Mapping結果，(a) STEM 影像；(b)、(c)、(d)、(e)、(f)、(g)、(h) 為對應元素分佈 50 圖4-16 Ce試片化成 1 秒之point元素分析位置圖 51 圖4-17 (a) Ce_DI 試片化成 5 秒SEM影像；(c) 高倍率影像；(b)、(d)BSE影像 52 圖4-18 (a) Ce_DI試片化成 10 秒 SEM 影像；(c) 高倍率影像；(b)、(d)BSE影像 53 圖4-19 (a) Ce_DI 試片化成 30 秒SEM影像；(c) 高倍率影像；(b)、(d)BSE影像 54 圖4-20 Ce_DI 試片化成 5 秒之橫截面影像組圖 55 圖4-21 Ce_DI 試片化成5秒之元素 Mapping結果，(a) 為STEM 影像；(b)、(c)、(d)、(e)、(f)、(g)、(h) 為對應元素分佈 56 圖4-22 Ce_DI 試片缺口處化成 5 秒之橫截面影像組圖 57 圖4-23 Ce_DI 試片化成 5 秒之缺口處元素Mapping結果，(a) 為 STEM 影像；(b)、(c)、(d)、(e)、(f)、(g)、(h) 為對應元素分佈 58 圖4-24 Ce_DI 試片化成 10 秒之橫截面影像組圖 59 圖4-25 Ce_DI 試片化成 10 秒之元素Mapping結果，(a) 為 STEM 影像；(b)、(c)、(d)、(e)、(f)、(g)、(h) 為對應元素分佈 60 圖4-26 (a) Ce 試片化成60秒 SEM 影像；(b) 為高倍率影像。 62 圖4-27 (a) Ce_DI 試片化成 60 秒 SEM 影像；(b) 為高倍率影像。 63 圖4-28 Ce試片化成 60 秒之橫截面影像組圖 64 圖4-29 (a) α-Mg 之皮膜結構；(b) 二次相之皮膜結構 65 圖4-30 Ce_DI 試片化成 60 秒之橫截面影像組圖 66 圖 4-31 (a) 二次相皮膜結構；(b) α-Mg 皮膜結構 67 圖4-32 Ce_DI 試片化成 60 秒元素Mapping結果，(a) 為 STEM 影像；(b)、(c)、(d)、(e)、(f)、(g)、(h) 為對應元素分佈 68 圖4-33 Ce_DI 試片化成 60 秒之橫向line scan 元素分析結果 69 圖4-34 二次相腐蝕產物之縱向 line scan 元素分析結果 69 圖4-35 Mg、Mg_DI、Ce、Ce_DI 試片之OCP監控 71 圖4-36 Mg、Mg_DI、Ce、Ce_DI 試片之極化曲線 72 圖4-37 Mg、Mg_DI、Ce、Ce_DI試片析氫體積圖 (a) 5 小時(b) 1 小時 74 圖4-38 Mg、Mg_DI、Ce、Ce_DI 試片之腐蝕速率比較圖 75 圖 5-1 使用 EPMA 內的 SEM 得到表面的影像 77 圖5-2不燃型鎂合金二次相之TEM繞射影像 78 圖5-3 不燃型鎂合金試片之 BSE 影像 80 圖 5-4 不燃型鎂合金試片之 SKPFM 量測結果 (a) 表面粗糙度 (b) Volta-potential 80 圖 5-5 SKPFM 量測 AB 線段上的Volta-potential 值 80 圖 5-6 Mg試片浸泡於水溶液溶解示意圖 82 圖5-7 Ce 表面之化成反應機制示意圖 83 圖5-8 Ce_DI 表面化成反應機制示意圖 84 圖5-9 Ce、Ce_DI 試片於 α-Mg 總膜層厚度 86 圖5-10 Ce、Ce_DI 試片於二次相上 CeO2 皮膜厚度比較 87 圖 5-11 Ce、Ce_DI 試片化成 60 秒開路電位監測圖 89 表目錄 表2 1鎂、鋁及鐵之物理性質[16] 2 表 3 1 不燃型鎂合金成分組成 29 表3-2不燃型鎂合金試片之命名 29 表4-1 Mg_DI 試片腐蝕產物厚度量測表 41 表4-2各位置元素分析結果 51 表4-3 Ce試片化成 60 秒各膜層平均厚度表 65 表4-4 Ce_DI 試片化成 60 秒後各膜層平均厚度表 67 表4-5 各試片之腐蝕速率數值表 75 表5-1對 A、B 兩位置的元素分析結果 77 表5-2Ce、Ce_DI 試片 α-Mg 之總膜層厚度 86 表5-3 Ce、Ce_DI 試片於二次相上 CeO2 皮膜厚度 87 | |
| dc.language.iso | zh-TW | |
| dc.subject | 表面分析 | zh_TW |
| dc.subject | 化成處理 | zh_TW |
| dc.subject | 不燃型鎂合金 | zh_TW |
| dc.subject | 伽凡尼腐蝕 | zh_TW |
| dc.subject | 電化學 | zh_TW |
| dc.subject | Surface analysis | en |
| dc.subject | Mg-Al-Ca-Mn alloys | en |
| dc.subject | Micro-galvanic Corrosion | en |
| dc.subject | Cerium conversion coating | en |
| dc.subject | Electrochemistry | en |
| dc.title | 不燃型鎂合金腐蝕及表面處理性質之研究 | zh_TW |
| dc.title | Corrosion and Surface Treatment Properties of Non-flammable Magnesium Alloys | en |
| dc.date.schoolyear | 110-1 | |
| dc.description.degree | 碩士 | |
| dc.contributor.oralexamcommittee | 林招松(Hui-Lin Lin),楊舜涵(Hsien-Feng Lee),林新智 ,朱鵬維 | |
| dc.subject.keyword | 不燃型鎂合金,表面分析,化成處理,伽凡尼腐蝕,電化學, | zh_TW |
| dc.subject.keyword | Mg-Al-Ca-Mn alloys,Micro-galvanic Corrosion,Cerium conversion coating,Electrochemistry,Surface analysis, | en |
| dc.relation.page | 100 | |
| dc.identifier.doi | 10.6342/NTU202200536 | |
| dc.rights.note | 未授權 | |
| dc.date.accepted | 2022-02-14 | |
| dc.contributor.author-college | 工學院 | zh_TW |
| dc.contributor.author-dept | 工程科學及海洋工程學研究所 | zh_TW |
| dc.date.embargo-lift | 2024-02-28 | - |
| 顯示於系所單位： | 工程科學及海洋工程學系 | |
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