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姓名	王俊堯(Chun-Yao Wang)  查詢紙本館藏	畢業系所	機械工程學系
論文名稱	在焦磷酸鍍液中製備銅-鋅薄膜之平板電鍍法與製備合金微柱之微陽極導引電鍍法之比較 (A comparison between the planar electrodeposition of Cu-Zn thin films and the micro anode-guided electroplating (MAGE) of Cu-Zn micropillars in the pyrophosphate)
相關論文	★ 銅導線上鍍鎳或錫對遷移性之影響及鍍金之鎳/銅銲墊與Sn-3.5Ag BGA銲料迴銲之金脆研究 ★ 單軸步進運動陽極在瓦茲鍍浴中進行微電析鎳過程之監測與解析 ★ 光電化學蝕刻n-型（100）單晶矽獲得矩陣排列之巨孔洞研究 ★ 銅箔基板在H2O2/H2SO4溶液中之微蝕行為 ★ 助銲劑對迴銲後Sn-3Ag-0.5Cu電化學遷移之影響 ★ 塗佈奈米銀p型矽(100)在NH4F/H2O2 水溶液中之電化學蝕刻行為 ★ 高效能Ni80Fe15Mo5電磁式微致動器之設計與製作 ★ 銅導線上鍍金或鎳/金對遷移性之影響及鍍金層對Sn-0.7Cu與In-48Sn BGA銲料迴銲後之接點強度影響 ★ 含氮、硫雜環有機物對鍋爐鹼洗之腐蝕抑制行為研究 ★ 銦、錫金屬、合金與其氧化物的陽極拋光行為探討 ★ n-型(100)矽單晶巨孔洞之電化學研究 ★ 鋁在酸性溶液中孔蝕行為研究 ★ 微陽極引導電鍍與監測 ★ 鍍金層對Bi-43Sn與Sn-9Zn BGA銲料迴銲後之接點強度影響及二元銲錫在不同溶液之電解質遷移行為 ★ 人體血清白蛋白構形改變之電化學及表面電漿共振分析研究 ★ 光電化學蝕刻製作n-型(100)矽質微米巨孔 陣列及連續壁結構
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摘要(中)	本研究在焦磷酸鹽鍍液中，分別以傳統之平板電鍍法(planar electrodeposition, PE)製備銅-鋅薄膜(thin films, TFs)；以即時影像監控之微陽極導引法(micro anode-guided electroplating, MAGE)之局部電鍍法(localized electrodeposition, LE)，製備銅-鋅合金微柱 (micropillars, MPs)。首先分別在平板電鍍法(PE)與局部電鍍法(LE)中，藉由解析產物在表面形貌、化學成分、晶體結構、機械性質、和抗腐蝕性能上與其實驗參數之關聯性。隨後，比較平板電鍍(PE)所得薄膜(TFs)與微電鍍(LE)所得微柱(MPs)在電化學 液中陰極極化曲線(cathodic polarization curve, CPC)和電化學阻抗頻譜(electrochemical impedance spectroscopy, EIS)的行為，有助於理解其反應過程之機制與差異。 在[Zn2+]/[Cu2+]比值為8/1的鍍液中，陰極極化曲線掃描分別解釋一般平板電鍍和微電鍍的電沉積機制，電化學交流阻抗驗證了電沉積機制，薄膜的鋅含量分布較廣(13.3~57.9 at.%)且有不同的銅鋅合金相(α、β和β′相)，而微柱鋅含量較低(3.3~8.1 at.%)且只有單一銅鋅合金α相。微柱α相的硬度大於薄膜(1.7~3.0 GPa > 1.0~1.5 GPa)。經COMSOL 5.2軟體模擬得知薄膜和微柱的電場分佈與電力線密度明顯的不同。薄膜抗腐蝕優於微柱。 改變鍍液中銅離子濃度實驗中，藉由陰極極化曲線觀察微陽極導引局部電鍍的電化學還原機制。在特定的電位下進行電化學交流阻抗分析可以解析電鍍的機制。微柱的鋅含量從8.05 at.% (α 相)增加到54.60 at.% (β和β′相)。微柱由不同尺寸的奈米晶粒組成；含40.51 at.% Zn (β相)的微柱表現出最大硬度(5.30 GPa)和最高楊氏模數(113.64 GPa)；電場模擬顯示，隨著鍍液中[Zn2+]/[Cu2+]比值的增加，集中在微柱頂端的最高場強僅略有增加(從152.2增加到152.5 kV/m)。 當[Zn2+]/[Cu2+]比值為64/1的鍍液中實驗改變電鍍電位，初始間距為30 μm微柱會有不同的結晶晶相(α、β和β + β′)，其中鋅含量範圍為37.12~68.94 at.%；然後使用數據來描述電場強度對晶相、成分、生長速率和微柱直徑的相關性。
摘要(英)	Cu–Zn alloys consisting of thin films (TFs) were prepared through ordinary planar electrodeposition (PE), and those of micropillars (MPs) were fabricated through localized electrodeposition (LE). Energy-dispersive spectroscopy and X-ray diffractometry analyses indicated that the TFs contained a wider range of Zn content (13.3–57.9 at.%) with different crystal phases (α-, β-, and β′-phases) than that in MPs (i.e., Zn content ranging from 3.3 to 8.1 at.%, confined to only α-phase). The results of the nano-indentation test indicate that the hardness of the α-phases in MPs was greater (1.7–3.0 GPa) than that in TFs (1.0–1.5 GPa). Simulations using the commercial software COMSOL 5.2 revealed that the distribution of the electric field in PE and LE was distinct. Through potentiodynamic cathodic polarization, we distinguished between the mechanisms of the PE and LE processes. Electrochemical impedance spectroscopy results confirm these mechanisms. The corrosion resistance in 3.5 wt% NaCl is lower for the MPs than for the TFs. Cu–Zn alloy micropillars were fabricated using microanode-guided electroplating (MAGE) at a constant potntical under an initial inter-electrode gap of 30 μm in pyrophosphate baths. Energy-dispersive spectroscopy and X-ray diffractometry analysis revealed that the micropillar alloys exhibit an increase in the Zn content from 8.05 at.% (in α phase) to 54.60 at.% (in β, and β′ phases) with an increase in the ratio of [Zn2+]/[Cu2+] in the bath from 8/1 to 128/1. Transmission electron microscopy revealed that the Cu–Zn alloy micropillars were composed of nano-grains with different sizes depending on the bath employed. Nano-indentation test indicated that the micropillar containing 40.51 at.% Zn (in presence of β-phase) exhibits the maximum hardness (at 5.30 GPa) and highest Young′s modulus (at 113.64 GPa). Simulation of the electric field using the commercial software COMSOL 5.2 revealed that the highest field strength centralized at the cylindrical top displayed only a slight increase (from 152.2 to 152.5 kV/m) with an increase in the ratio of [Zn2+]/[Cu2+] in the bath. Potentiodynamic cathodic polarization is useful for understanding the mechanism of microanode-guided electroplating. This process was carried out via micro-anode-guided electroplating in a pyrophosphate bath at a constant negative potential in the range -1.85 to -2.05 V. Thus, at an initial gap of 40 μm, the process afforded micropillars with a single α-brass crystal phase and at.% Zn contents in the range 17.20–32.01%. A reduction in the initial gap to 30 μm resulted in varied micropillar crystal phases (α, β, and β+ β′) with at.% Zn contents in the range 37.12–68.94. The simulation commercial software COMSOL 5.2 was employed to correlate the asymmetric distribution of the electric field to the experimental parameters and pillar characteristics. The resultant data was then used to delineate the dependence of the field strength on the crystal phase, composition, growth rate, and micropillar diameters. Finally, a potentiodynamic cathodic polarization study was employed to elucidate the mechanism for the fabrication of the Cu-Zn alloy micropillars via potentiostatic LECD.
關鍵字(中)	★ 焦磷酸鹽 ★ 銅鋅合金 ★ 平板電鍍 ★ 微電鍍 ★ 陰極極化曲線 ★ 交流阻抗	關鍵字(英)	★ Cu–Zn alloy ★ Planar electrodeposition ★ Localized electrodeposition ★ Micro-anode-guided electroplating ★ Potentiodynamic cathodic polarization ★ Electrochemical impedance spectroscopy
論文目次	摘要 i Abstract iii 致謝 v 目錄 vi 表目錄 xii 圖目錄 xiv 符號表 xviii 縮寫 xx 第一章、前言 1 1-1 研究背景 1 1-2 研究動機 2 1-3 研究目的 3 第二章、原理與文獻回顧 5 2-1 電鍍與合金電鍍原理 5 2-2 微電鍍製程之發展 8 2-3 塊材銅鋅合金之文獻 12 2-4 電鍍銅鋅合金之發展 14 第三章、實驗方法 17 3-1 實驗流程 17 3-2 陰陽極的製作 18 3-3 即時影像導引微電鍍平台 19 3-4 實驗方法 21 3-4-1 鍍液調配 21 3-4-2 電化學陰極極化掃描 22 3-4-3 EIS量測分析 24 3-4-4 銅鋅合金製備 24 3-4-5 SEM表面形貌分析 25 3-4-6 EDS定性分析 26 3-4-7 ICP定量分析 26 3-4-8 XRD晶體結構分析 26 3-4-9 TEM繞射結構分析 26 3-4-10 維氏硬度與奈米壓痕測試 27 3-4-11 電場模擬 29 3-4-12 抗腐蝕行為量測 29 第四章、結果 31 4-1 平板電鍍銅鋅合金 31 4-1-1 陰極極化曲線掃描 31 4-1-2 定電位電鍍與電流密度之結果 32 4-1-3 EIS分析結果 32 4-1-4 SEM表面形貌觀察 33 4-1-5 EDS定性之結果 33 4-1-6 XRD結晶結構之結果 33 4-1-7 維氏硬度分析之結果 34 4-1-8 電場模擬之結果 34 4-1-9 腐蝕量測之結果 34 4-2 微電鍍製做銅鋅合金微柱析鍍參數探討 35 4-2-1 改變兩極間距 35 4-2-1-1 電場模擬之結果 35 4-2-1-2 SEM表面形貌之結果 36 4-2-2 改變鍍液中銅離子濃度 36 4-2-2-1 陰極極化曲線掃描 36 4-2-2-2 定電位電鍍與電流之結果 38 4-2-2-3 EIS分析結果 39 4-2-2-4 SEM表面形貌觀察 39 4-2-2-5 EDS、ICP微柱分析結果 40 4-2-2-6 XRD結晶結構之結果 40 4-2-2-7 TEM繞射結構之結果 42 4-2-2-8 奈米壓痕之結果 44 4-2-2-9 電場模擬之結果 45 4-2-2-10 腐蝕量測之結果 45 4-2-3 改變電鍍電位 46 4-2-3-1 定電位電鍍與電流密度之結果 46 4-2-3-2 EIS分析結果 46 4-2-3-3 SEM表面形貌觀察 47 4-2-3-4 EDS定性之結果 47 4-2-3-5 XRD結晶結構之結果 47 4-2-3-6 奈米壓痕之結果 48 4-2-3-7 電場模擬之結果 48 4-2-3-8 腐蝕量測之結果 48 第五章、討論 49 5-1 平板電鍍和微電鍍銅鋅合金之比較 49 5-1-1 析鍍電位對表面形貌之影響 49 5-1-2 析鍍電位對晶體結構之影響 50 5-1-3 析鍍電位對成分含量之影響 51 5-1-4 析鍍電位對硬度之影響 51 5-1-5 析鍍電位對電場分佈之影響 52 5-1-6 析鍍電位對電流密度之影響 53 5-1-7 析鍍電位對陰極極化曲線之影響 54 5-1-8 析鍍電位對EIS之影響 57 5-1-9 析鍍電位對腐蝕之影響 58 5-2 微柱製程鍍液參數(兩極間距)之影響 58 5-2-1 兩極間距對微柱表面形貌之影響 59 5-2-2 兩極間距對微柱鋅含量之影響 59 5-2-3 兩極間距對微柱晶體結構之影響 60 5-2-4 兩極間距對微柱電場大小和沉積速率之影響 60 5-3 微柱製程鍍液參數(銅離子含量)之影響 61 5-3-1 鍍液參數對微柱表面形貌之影響 62 5-3-2 鍍液參數對微柱晶體結構之影響 62 5-3-3 鍍液參數對微柱成分含量之影響 62 5-3-4 鍍液參數對微柱TEM之影響 62 5-3-5 鍍液參數對微柱硬度之影響 63 5-3-6 鍍液參數對微柱電場分佈之影響 63 5-3-7 鍍液參數對微柱陰極極化曲線之影響 64 5-3-8 鍍液參數對微柱EIS之影響 66 5-4 微柱製程電位參數(固定鍍液)之影響 69 5-4-1 電位參數對微柱表面形貌之影響 70 5-4-2 電位參數對微柱晶體結構之影響 70 5-4-3 電位參數對微柱成分含量之影響 70 5-4-4 電位參數對微柱硬度之影響 70 5-4-5 電位參數對微柱電場分佈之影響 71 5-4-6 電位參數對微柱EIS之影響 71 5-4-7 電位參數對微柱腐蝕性能之影響 71 第六章、結論與展望 72 參考文獻 74 個人簡歷 133 著作列表 134
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指導教授	林景崎(Jing-Chie Lin)	審核日期	2022-12-27
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