硫酸與草酸陽極皮膜的光學性質與抗腐蝕分析

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鄭朝翰(Ch’ao-han Cheng) 查詢紙本館藏

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論文名稱

硫酸與草酸陽極皮膜的光學性質與抗腐蝕分析

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摘要(中)

本研究主要探討不同的陽極處理對皮膜厚度、成分、光學性質及CIE L*a*b*值的影響。使用的材料為純鋁(99.999%)，電解液為稀釋的硫酸及草酸溶液，採用固定電流密度法。分析陽極過程中的電壓與時間(V-t)變化曲線，透過SEM觀察陽極多孔氧化膜的生長行為及利用光電子能譜儀(XPS)分析陽極皮膜的表面層和介面層(氧化膜/基材)組成分，並使用AUTOLAB PGSTAT30分析電化學測試，最後使用色度儀及微型光譜儀分析皮膜的顏色及光學性質。
觀察V-t曲線，草酸陽極在各階段下的工作電壓均比硫酸陽極還要高，這是因為草酸陽極溶液的電阻值較大的關係。使用TEM觀察皮膜，可以發現到會有氣泡殘留在皮膜中。將陽極試片進行XPS分析，我們得知陽極皮膜的組成可能是非晶質氧化鋁、水合氧化物及結晶型氧化鋁。將陽極試片進行腐蝕測試分析，陽極皮膜上的成分會影響陽極皮膜的抗腐蝕能力。

摘要(英)

The purpose of this study is aimed at investigating effects of coating thickness, composition, optical properties and CIE L*a*b* value by different anodizing condition. The alloy used in this experiment was pure aluminum(99.999%), and the electrolyte used was dilute sulfuric acid and oxalic acid, all experiments conducted by using constant current density. Anodize was utilized to explore the voltage-time (V-t) curvature changes in the process of anodizing were recored. After the above manufacturing processes, the effect of the microstructure on the growing behavior of the porous AAO film was observed by using SEM, in addition, the XPS was utilized to analyze the composition of AAO film surface and interface (film/metal). Then, the electrochemical tests were conducted and recorded by AUTOLAB PGSTAT30 potentiostat. The CIE L*a*b* colorimeter and Micro Spectrometer were used to analyzed the AAO film surface colour properties and optical properties.
In respect to the variation of V-t curvature, the oxalic acid at various stages of the anode voltage is even higher than the sulfuric acid anodizing, because the resistance in oxalic solution is much higher than the sulfuric acid. By analyzing the Transmission Electron Microscopy (TEM), we found some bubble survive on the film. The anodized samples were then analyzed by X-ray Photoelectron Spectroscopy (XPS). We found that the constituted phases in the AAO film are composed by amorphous alumina (Al-O-H),hydrated oxide (Al(OH)3) and crystallite oxide (AlOOH) phases. In the corrosion test, the composition of the AAO film can affect the corrosion resistance of the AAO film.

關鍵字(中)

★ 純鋁
★ 陽極處理
★ 色度儀
★ 光電子能譜儀
★ 布拉格方程式
★ 極化曲線

關鍵字(英)

★ pure aluminum
★ anodic treatment
★ CIE L*a*b* colorimeter
★ XPS
★ bragg’s equation
★ polarization

論文目次

目錄
中文摘要 I
英文摘要 II
圖目錄 V
表目錄 VII
一、前言 1
二、文獻回顧 2
2-1 鋁合金的材料特性簡介 2
2-1-1 鋁合金的分類 2
2-1-2 5N純鋁簡介 3
2-1-3 鋁的結晶結構 3
2-2 陽極處理 5
2-2-1 陽極氧化膜種類 6
2-2-2 陽極氧化膜的生長機制 6
2-2-3 陽極氧化膜生長過程之電壓與時間關係 7
2-2-4 陽極處理的前處理-電化學拋光 10
2-2-5 陽極處理的操作溫度與氧化層厚度關係 11
2-3 陽極處理的分類 13
2-3-1 硫酸法 13
2-3-2 草酸法 14
2-3-3 鉻酸法 14
2-4 陽極氧化膜封孔 15
2-4-1 熱水封孔 15
2-4-2 鉻酸鹽封孔 16
2-4-3 醋酸鎳封孔 16
2-4-4 熱水封孔與醋酸鎳封孔差異 16
2-5 腐蝕機制 17
2-5-1 氯離子的角色 18
2-5-2 氯離子腐蝕理論 19
2-6 陽極氧化膜光學性質 19
2-6-1 電磁波譜種類 20
2-6-2 陽極氧化膜光學性質與孔洞關係 21
2-6-3 陽極氧化膜與藍光現象的關係 29
2-6-4 陽極膜光學性質與布拉格方程式關係 32
三、實驗方法與步驟 33
3-1 實驗目的 33
3-2 實驗材料及試片準備 33
3-3 實驗設備 33
3-4 實驗步驟 34
四、結果與討論 39
4-1 一般陽極氧化膜性質分析 39
4-2 硫酸陽極與草酸陽極氧化膜光學分析 62
4-2-1 硫酸陽極與草酸陽極氧化膜對L*、a*、b*的光學影響 62
4-2-2 硫酸陽極與草酸陽極氧化膜對色度、反射率、吸收值、折射值的光
學影響 65
4-2-3 陽極氧化膜之布拉格方程式探討 69
4-3 硫酸與草酸陽極氧化膜之腐蝕分析 70
五、結論 73
參考文獻 79
附錄一 86
附錄二 87
圖目錄
第二章
Fig. 2-1 FCC面心立方結構 .4
Fig. 2-2 理想的多孔陽極氧化鋁膜結構示意圖 6
Fig. 2-3 氧化層中離子移動的反應以及氧化層的生長與溶解反應 7
Fig. 2-4 陽極過程電壓與時間關係圖 8
Fig. 2-5 硫酸-不同陽極時間的陽極膜SEM圖 9
Fig. 2-6 草酸-不同陽極時間的陽極膜SEM圖 9
Fig. 2-7 陽極處理之試片前處理-1 10
Fig. 2-8 陽極處理之試片前處理-2 11
Fig. 2-9 不同溫度下的陽極膜生長型態 12
Fig. 2-10 硫酸陽極處理時間與氧化層表面孔洞尺寸的關係 13
Fig. 2-11 陽極氧化膜熱水封孔示意圖 15
Fig. 2-12 陽極氧化膜SEM橫斷面 17
Fig. 2-13 金屬在氯化鈉溶液裡的腐蝕行為 19
Fig. 2-14 電磁波譜圖 20
Fig. 2-15 Al1050硫酸陽極處理-反射率圖 23
Fig. 2-16 Al1050硫酸陽極處理-反射率圖 24
Fig. 2-17 氧化層金屬表面上干擾示意圖 24
Fig. 2-18 硫酸陽極氧化膜在不同條件下的厚度25
Fig. 2-19草酸陽極氧化膜生長速率 26
Fig. 2-20不同陽極時間及製程與反射率關係 26
Fig. 2-21不同陽極處理溫度對孔洞尺寸的影響 27
Fig. 2-22不同陽極處理溫度對孔與孔間的中心距離的影響 28
Fig. 2-23不同陽極處理溫度對孔洞率的影響 28
Fig. 2-24 AAO膜應用實例-1 29
Fig. 2-25 AAO膜應用實例-2 29
Fig. 2-26不同陽極處理的PL圖 31
Fig. 2-27不同陽極處理的吸收光譜 31
Fig. 2-28 AAO膜光學反射示意圖 32
第三章
Fig. 3-1 實驗流程圖 38
第四章
Fig. 4-1 硫酸與草酸陽極之電壓-時間-微分曲線圖 39
Fig. 4-2 硫酸及草酸陽極氧化膜在封孔處理前後成分差異 45
Fig. 4-3 硫酸陽極-膜厚20nm-表面成分XPS分析圖 46
Fig. 4-4 硫酸陽極-膜厚50nm-表面成分XPS分析圖 47
Fig. 4-5 硫酸陽極-膜厚250nm-表面成分XPS分析圖 48
Fig. 4-6 硫酸陽極-膜厚2500nm-表面成分XPS分析圖 49
Fig. 4-7 草酸陽極-膜厚20nm-表面成分XPS分析圖 50
Fig. 4-8 草酸陽極-膜厚50nm-表面成分XPS分析圖 51
Fig. 4-9 草酸陽極-膜厚250nm-表面成分XPS分析圖 52
Fig. 4-10 草酸陽極-膜厚2500nm-表面成分XPS分析圖 53
Fig. 4-11 硫酸陽極-膜厚20nm-介面成分XPS分析圖 54
Fig. 4-12 硫酸陽極-膜厚50nm-介面成分XPS分析圖 55
Fig. 4-13 硫酸陽極-膜厚250nm-介面成分XPS分析圖 56
Fig. 4-14 硫酸陽極-膜厚2500nm-介面成分XPS分析圖 57
Fig. 4-15 草酸陽極-膜厚20nm-介面成分XPS分析圖 58
Fig. 4-16 草酸陽極-膜厚50nm-表面成分XPS分析圖 59
Fig. 4-17 草酸陽極-膜厚250nm-表面成分XPS分析圖 60
Fig. 4-18 草酸陽極-膜厚2500nm-表面成分XPS分析圖 61
Fig. 4-19 硫酸陽極氧化膜在不同膜厚下的L*值 62
Fig. 4-20 草酸陽極氧化膜在不同膜厚下的L*值 62
Fig. 4-21 不同陽極時間下孔洞的觀察 64
Fig. 4-22 不同孔徑對電場強度的影響 64
Fig. 4-23 草酸陽極氧化膜-介面層-C1s之成分差異 65
Fig. 4-24 陽極氧化膜cross-section TEM圖 66
Fig. 4-25 硫酸陽極氧化膜在不同膜厚下的光學性質 67
Fig. 4-26 草酸陽極氧化膜在不同膜厚下的光學性質 68
Fig. 4-27 m值與陽極氧化膜厚度之關係 69
Fig. 4-28 n值與陽極氧化膜厚度之關係 69
Fig. 4-29 硫酸陽極封孔前與封孔後之極化曲線圖 70
Fig. 4-30 草酸陽極封孔前與封孔後之極化曲線圖 70
Fig. 4-31 腐蝕測試前之成分差異：(a)封孔前 (b)封孔後 73
Fig. 4-32 腐蝕測試後之成分差異：(a)封孔前 (b)封孔後 73
Fig. 4-33 硫酸陽極處理-腐蝕測試前-封孔前/後之成分差異：(a)Al2p (b)O1s 74
Fig. 4-34 硫酸陽極處理-腐蝕測試前-封孔前/後之成分差異：(a)Al2p (b)O1s 74
Fig. 4-35 草酸陽極處理-腐蝕測試前-封孔前/後之成分差異：(a)Al2p (b)O1s 75
Fig. 4-36 草酸陽極處理-腐蝕測試後-封孔前/後之成分差異：(a)Al2p (b)O1s 75
Fig. 4-37 硫酸陽極處理-封孔前-腐蝕前/後之成分差異：(a)Al2p (b)O1s 76
Fig. 4-38 硫酸陽極處理-封孔後-腐蝕前/後之成分差異：(a)Al2p (b)O1s 76
Fig. 4-39 草酸陽極處理-封孔前-腐蝕前/後之成分差異：(a)Al2p (b)O1s 77
Fig. 4-40 草酸陽極處理-封孔後-腐蝕前/後之成分差異：(a)Al2p (b)O1s 77
表目錄
第二章
Table 2-1 形成金屬氧化物之自由能(KJ/mol Oxygen at 500k) 4
Table 2-2 純鋁在室溫下的機械性質 5
Table 2-3 不同冷作條件下5N純鋁的機械強度 5
Table 2-4 硫酸陽極處理時，在不同操作溫度下氧化層厚度、孔洞尺寸與電壓關係 12
Table 2-5 不同金屬在25°C，0.1NaCl溶液的孔蝕電位 18
Table 2-6 陽極氧化模參數表 25
Table 2-7 不同陽極處理對孔洞參數的影響 27
Table 2-8 不同陽極處理對孔洞率的影響 27
Table 2-9 不同量測部位之m值變化 32
第三章
Table 3-1 5N純鋁材料成分表(ppm) 33
Table 3-2 XPS 在Al 2p,O 1s,S 2p分析各種成分鍵結能表 37
第四章
Table 4-1硫酸及草酸陽極在各階段下的電壓、氧化時間與能量消耗表 40
Table 4-2硫酸陽極氧化膜在不同時間下之性質結論表 41
Table 4-3草酸陽極氧化膜在不同時間下之性質結論表 41
Table 4-4硫酸陽極在各階段下的表面層XPS成分分析表原子百分比 42
Table 4-5草酸陽極在各階段下的表面層XPS成分分析表原子百分比 42
Table 4-6硫酸陽極在各階段下的介面層XPS成分分析表原子百分比 43
Table 4-7草酸陽極在各階段下的介面層XPS成分分析表原子百分比 43
Table 4-8硫酸陽極-氧化膜厚度10μm下的表面層成分分析原子百分比 44
Table 4-9草酸陽極-氧化膜厚度10μm下的表面層成分分析原子百分比 44
Table 4-10硫酸陽極在不同時間下的表面粗糙度 63
Table 4-11硫酸陽極在不同時間下的表面粗糙度 63

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指導教授

施登士(Teng-Shih Shih)

審核日期

2013-7-26

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