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以作者查詢圖書館館藏 、以作者查詢臺灣博碩士 、以作者查詢全國書目 、勘誤回報 、線上人數：44 、訪客IP：3.135.198.49
姓名 黃俊強(Chun-chiang Huang) 查詢紙本館藏 畢業系所 機械工程學系 論文名稱 微電鍍法之製程參數對其製備鎳鐵合金微柱之形貌、機械性質與防蝕特性之影響
(The influence of process parameters on micro electrodeposition Ni-Fe alloy column morphology, mechanical property and corrosion resistance)相關論文 檔案 [Endnote RIS 格式]
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摘要(中) 本論文在探討微陽極導引電鍍法製備單軸鎳鐵合金微柱，於電鍍製程中，改變實驗參數如製程偏壓(4.0V~4.4V)、鍍浴溫度(40℃~55℃)與析鍍間距(10μm~40μm)等條件，對於所得鎳鐵合金微柱表面形貌、機械性質與防蝕特性等之影響。此鎳鐵合金微柱之表面形貌，經由掃描式電子顯微鏡進行觀察比較；其機械性質則藉由微應力拉伸試驗機來測量；至於防蝕特性則將鎳鐵合金微柱浸泡於3.5wt% NaCl水溶液中，藉由電化學試驗比較其腐蝕行為。
結果顯示：較低鍍浴溫度(40℃)與製程偏壓下(4.0V)，和較大的析鍍間距(40μm)製備所得鎳鐵合金微柱之組織均勻細緻、形貌平滑；此鎳鐵合金微柱之機械性質最佳(楊氏係數達162.12GPa)，其對應之直流電極化阻抗測量值最大(2.28×105Ω)，具有最佳之抗蝕性。若鍍液之溫度提高至55℃，或製程偏壓上升至4.4V，微柱之組織均勻度逐漸變差、形貌粗糙化；就機械性質而言，其楊氏係數隨之下降(楊氏係數為23.62GPa)；在NaCl水溶液中之極化阻抗值也隨之下降(8.91×104Ω)，抗蝕性較差。依據析鍍電流量測顯示：在低鍍浴溫度、低製程偏壓下進行微電鍍，其析鍍電流較低且平穩(平均電流為0.875±0.079mA)，析鍍形貌較為平滑(析鍍所得之結構細緻、平滑)，內部結構缺陷較少，因此其機械性質和抗腐蝕性較高。
關鍵字：鎳鐵合金、微陽極導引電鍍、楊氏係數
摘要(英) The effect of operational parameters (including voltage employed, composition of the bath and bath temperature in the micro anode guided electroplating) on the morphology, mechanical property and corrosion behavior of Ni-Fe alloy micro columns was of interest. The surface morphology was examined by scanning electron microscope. The mechanical property was tested by using a micro&nano-scale mechanical testing system to estimate the elastic modulus (Young’s modulus) and the corrosion behavior was evaluated by polarization resistance technique in 3.5 wt% NaCl solution. The results revealed that the micro columns have the smooth surface composed of tiny particles as the deposited from the bath with lower temperature (40℃) under lower voltage employed (4.0V). Their mechanical property was found to be better (with elastic modulus at 162.12GPa) than those (in the range from 106.32GPa to 23.62GPa) fabricated in a bath with higher temperature (i.e. in the range from 40 to 55℃) under higher voltage (in the range from 4.0V to 4.4V). In addition, the corrosion resistance for the micro columns deposited at lower temperature (40℃) and lower voltage (4.0V) is much better (with polarization resistance at 2.28×105Ω) than those (in the range from 1.82×105Ω to to 8.91×104Ω) obtained at higher temperatures (i.e. in the range from 40 to 50℃) and higher voltages (in the range from 4.0V to 4.4V). The variation of the morphology, mechanical property of the micro columns deposited depends upon the voltage, electrode separation and bath temperature those determined by distribution of electric field strength. The micro column appears in smooth surface consisting of tiny particles and dense internal structure. The columns with smooth surface and dense internal were arisen from a uniform, stable and weaker strength of electric field as the deposition taken place in a bath with lower temperature and lower voltage chosen in the electroplating. The micro columns with rough morphology containing, many imperfections in the crystal structure were ascribe to be electrodeposited under non-uniform, less stable and stronger strength of the electric field determined by the deposition conducted in a bath with higher temperature and higher voltages selected. According to the measurement of electroplating current density. When the current density is stable and uniform to maintain at 0.875±0.079mA (electrodeposition at 40℃ and 4.0V), Therefore, a micro columns with smooth morphology and dense internal (containing less imperfections) could be fabricated. Those micro columns revealed better mechanical property and corrosion resistance.
Key words：Ni-Fe alloy, micro-anode guide electrodeposition, Young’s modulus
關鍵字(中) ★ 鎳鐵合金
★ 楊氏係數
★ 微陽極導引電鍍關鍵字(英) ★ NiFe alloy
★ Young's modulus
★ micro anode guide electrodeposition論文目次 目錄
摘要 ……….................................................................................................. i
Abstract .................................................................................................. ii
致謝 .......................................................................................................... iv
目錄 ........................................................................................................... v
表目錄 ...................................................................................................... ix
圖目錄 ....................................................................................................... x
一、前言 .................................................................................................... 1
1-1 研究背景 ........................................................................................ 1
1-2 研究動機與目的 ............................................................................ 1
二、文獻回顧與原理學說 ....................................................................... 3
2-1 文獻回顧 ........................................................................................ 3
2-1-1 微電鍍概說 ................................................................................. 3
2-1-2 微電鍍製程之國外發展 ............................................................. 3
2-1-3 微電鍍製程之國內發展 ............................................................. 6
2-2 電鍍原理 ........................................................................................ 7
2-2-1 直流電電鍍 ................................................................................. 7
2-2-2 物質移動之途徑 ......................................................................... 8
2-3 拉伸試驗應力分析 ........................................................................ 9
2-4 材料的磁特性 ................................................................................ 10
2-4-1 鎳鐵磁性的起因 ......................................................................... 10
2-4-2 鐵磁性材料之磁區結構 ............................................................. 11
2-4-3 磁性材料的評估依據 ................................................................. 12
2-4-4 微量元素添加對合金特性影響的相關研究 .............................. 13
三、研究方法 ............................................................................................ 14
3-1 實驗流程 ......................................................................................... 14
3-2 微陽極與陰極製作........................................................................... 14
3-3 實驗儀器 ......................................................................................... 15
3-3-1 實驗設備 ..................................................................................... 15
3-3-2 檢測儀器 ..................................................................................... 16
3-4 實驗流程 ........................................................................................ 17
3-4-1 電鍍液調配 ................................................................................. 17
3-4-2 微陽極導引電鍍法 ..................................................................... 18
3-5-3 微應力拉伸試驗 ......................................................................... 18
3-5-4 電化學實驗 ................................................................................. 19
3-5-4 磁特性實驗 ................................................................................. 20
四、研究結果 ............................................................................................ 21
4-1 間歇式微電鍍鎳鐵合金微柱 ......................................................... 21
4-1-1 製程偏壓對於間歇式微電鍍鎳鐵合金微柱之結果 .................. 21
4-1-2 鍍浴溫度對於間歇式微電鍍鎳鐵合金微柱之結果 .................. 21
4-1-3 析鍍間距對於間歇式微電鍍鎳鐵合金微柱之結果 .................. 22
4-2 微應力拉伸試驗結果 ..................................................................... 23
4-3 電化學實驗結果 ............................................................................. 24
4-3-1 開路電位量測 .............................................................................. 24
4-3-2 線性極化量測 .............................................................................. 25
4-4 連續式微電鍍 ................................................................................. 25
4-5 EDS定性分析 ................................................................................. 26
4-5-1 改變鎳鐵合金成分比例 .............................................................. 26
4-5-2 鎳鐵鉬合金成分比例 .................................................................. 26
4-6 磁特性分析 ..................................................................................... 26
4-6-1 不同鎳鐵合金成分比例之磁場特性量測結果 .......................... 26
4-6-2 鎳、鎳鐵與鎳鐵鉬之磁場特性量測結果 .................................. 27
五、研究討論 ............................................................................................ 29
5-1 間歇式微電鍍鎳鐵合金微柱之製程參數影響 ............................. 29
5-1-1 製程偏壓之影響 ......................................................................... 29
5-1-2 鍍浴溫度之影響 ......................................................................... 29
5-1-3 析鍍間距之影響 ......................................................................... 29
5-2 微柱形貌對於微應力拉伸試驗之影響 ......................................... 30
5-3 微柱形貌對於電化學實驗之影響 ................................................. 30
5-4 磁場特性討論 ................................................................................. 30
5-4-1 不同鎳鐵合金成分比例之磁場特性之影響 .............................. 30
5-4-2 鎳、鎳鐵與鎳鐵鉬之磁場特性之比較 ...................................... 31
六、結論 .................................................................................................... 32
參考文獻 .................................................................................................... 34
表目錄
表1-1 MEMS之微製造技術分類 ............................................................ 37
表1-2 各種微製造技術相較表 ................................................................ 38
表3-1 鍍液成分 ........................................................................................ 39
表3-2 微應力拉伸機(Nano UTM儀器規格) ........................................ 40
表4-1 鎳鐵EDS能譜分析表 ................................................................... 41
表4-2 鎳鐵鉬EDS能譜分析表 ............................................................... 41
圖目錄
圖2-1 電子自旋與軌道運動示意圖 ........................................................ 42
圖2-2 材料內部Bloch wall示意圖 ......................................................... 42
圖2-3 磁滯曲線示意圖 ............................................................................ 43
圖3-1 實驗流程圖 .................................................................................... 44
圖3-2 微陽極製作流程 ............................................................................ 45
圖3-3 陰極製作流程 ................................................................................ 46
圖3-4 微電鍍實驗裝置 ............................................................................ 47
圖3-5 間歇式微電鍍示意圖(a)給定初始間距並開始微電鍍(b)沉積物接觸微陽極造成系統短路 (c)微陽極向上移動並繼續微電鍍 (d)沉積物在次接觸微陽極 .............................................................................. 48
圖3-6 連續式微電鍍控制介面示意圖 .................................................... 49
圖3-7 微應力拉伸試驗示意圖 ................................................................ 49
圖3-8 電化學檢測試片製作流程圖 ........................................................ 50
圖3-9 電化學實驗裝置 ............................................................................ 50
圖3-10 震動樣品磁度儀 .......................................................................... 51
圖4-1 製程偏壓4.0V~4.4V進行間歇式微電鍍鎳鐵合金微柱之單步時間─析鍍電流圖.................................................................................... 52
圖4-2 製程偏壓4.0V~4.4V進行間歇式微電鍍鎳鐵合金微柱之平均時間─平均電流圖.................................................................................... 52
圖4-3 製程偏壓4.0V~4.4V進行間歇式微電鍍鎳鐵合金微柱之SEM照 片(a) 4.0V (b) 4.1V (c) 4.2V (d) 4.3V (e) 4.4V ............................. 53
圖4-4 鍍浴溫度40℃~55℃與導電度關係圖........................................... 54
圖4-5 鍍浴溫度40℃~55℃進行間歇式微電鍍鎳鐵合金微柱之單步時間─析鍍電流圖.................................................................................... 55
圖4-6 鍍浴溫度40℃~55℃進行間歇式微電鍍鎳鐵合金微柱之平均時間─平均電流圖.................................................................................... 55
圖4-7 鍍浴溫度40℃~55℃進行間歇式微電鍍鎳鐵合金微柱之SEM照片 (a) 40℃ (b) 45℃ (c) 50℃ (d) 55℃ .......................................... 56
圖4-8 析鍍間距10μm~40μm進行間歇式微電鍍鎳鐵合金微柱之單步時間─析鍍電流圖................................................................................ 57
圖4-9 析鍍間距10μm~40μm進行間歇式微電鍍鎳鐵合金微柱之平均時間─平均電流圖................................................................................ 57
圖4-10 析鍍間距10μm~40μm進行間歇式微電鍍鎳鐵合金微柱SEM照片(a)10μm (b)20μm (c)40μm ....................................................... 58
圖4-11 鎳鐵合金微柱於製程偏壓4.0V~4.4V之應力應變圖 ............... 59
圖4-12 鎳鐵合金微柱於製程偏壓4.0V~4.4V之拉伸樣品與截斷面 ….. 59
圖4-13 製程偏壓4.0V~4.4V之破壞應力、破壞應變關係圖 …….…...... 60
圖4-14 製程偏壓4.0V~4.4V所得楊氏係數關係圖 …………………………... 60
圖4-15 鎳鐵合金微柱於析鍍間距10μm~40μm之應力應變圖 ……... 61
圖4-16 鎳鐵合金微柱於析鍍間距10μm~40μm之拉伸樣品與截斷面 ………………….……………………………………………………………………….. 61
圖4-17 析鍍間距10μm~40μm之破壞應力、破壞應變關係圖 ……... 62
圖4-18 析鍍間距10μm~40μm所得楊氏係數關係圖 …………………….. 62
圖4-19 不同製程參數之鎳鐵合金微柱於3.5wt% NaCl水溶液之開路電位圖 ………………………………………………………………………………….……….. 63
圖4-20 不同製程參數的鎳鐵合金微柱進行開路電位量測的表面形貌 (a) 4.0V, 20μm, 40℃ (b) 4.0V, 10μm, 40℃ (c) 4.0V, 20μm, 50℃ (d) 4.4V, 20μm, 40℃ ……………....…………………………..……..…….…. 63
圖4-21 不同製程條件之鎳鐵合金微柱於3.5wt% NaCl進行線性極化掃描所得RLP阻抗值 ……………………………………………………………………..…. 64
圖4-22 間歇式微電鍍(a)析鍍初始距離，(b)實驗進行時，兩極間距逐漸縮小，(c)陰陽兩間間距趨近於接觸時，與(d)連續式微電鍍之兩極間距進行電場模擬的示意圖 ………………………………………………....…. 65
圖4-23 製程參數4.0V、40μm、40℃下，進行間歇式微電鍍與連續式微電鍍的電流－時間關係圖 .…………………………………….…………………. 66
圖4-24製程參數4.0V、40μm、40℃下，進行間歇式微電鍍與連續式微電鍍鎳鐵合金微柱SEM照片(a)間歇式 (b)連續式.………..……….. 66
圖4-25 鎳鐵合金微柱之EDS能譜分析圖 …………………………………………. 67
圖4-26 鎳鐵合金微柱之Mapping 掃描分析圖 ………………………….......... 67
圖4-27 鎳鐵鉬合金微柱之EDS能譜分析圖 …………………….……………….. 68
圖4-28 鎳鐵鉬合金微柱之Mapping 掃描分析圖 ……………………………... 68
圖4-29 Ni96Fe4之磁滯曲線圖 ………………………………………………….…………… 69
圖4-30 Ni88Fe12之磁滯曲線圖 …………………………………………………........…… 69
圖4-31 Ni82Fe18之磁滯曲線圖 ……………………………………………………………… 70
圖4-32 三種不同鎳鐵合金比例之磁滯曲線局部放大疊圖 ………........… 70
圖4-33 Ni100之磁滯曲線圖 ………………………………………………………………...… 71
圖4-34 Ni77Fe23之磁滯曲線圖 ……………………………………….…………………..… 71
圖4-35 Ni72Fe23Mo5之磁滯曲線圖 ………………………………..……………………… 72
圖4-36 鎳、鎳鐵與鎳鐵鉬之磁滯曲線局部放大疊圖 ……………………….… 72
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指導教授 林景崎(Jing-chie Lin) 審核日期 2010-8-28 推文 plurk
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