電鍍製作銅錫合金及Cu6Sn5之三維奈米晶微結構及其特性研究

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姓名

林佳政(Chia-Cheng Lin) 查詢紙本館藏

畢業系所

材料科學與工程研究所

論文名稱

電鍍製作銅錫合金及Cu6Sn5之三維奈米晶微結構及其特性研究
(Three-dimensional micro features of copper-tin alloy with Cu6Sn5 in Nanocrystals prepared by electroplating and their characterization)

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摘要(中)

本研究以即時影像導引微電鍍法來製作銅錫合金及Cu6Sn5三維微結構物。使用白金線作為陽極其線徑125 μm，以銅導線作為陰極其線徑為0.643 mm，陰陽兩極間距為80 μm，在含硫酸銅、硫酸亞錫、檸檬酸鈉與抗壞血酸之鍍液中進行電鍍，期望製作出含銅、錫兩金屬元素之微柱與微螺旋。研究目標，探討施以不同偏壓和在鍍液中添加不同濃度硫酸亞錫對微柱析鍍物表面形貌、化學組成、晶體結構以及還原電位之影響，進而尋找最佳之含銅、錫二元金屬微柱之電鍍條件，再以此條件出發，探討製作微型螺旋之可行性，並研究微螺旋析鍍角度與製程參數對微型螺旋尺寸與線徑均勻度之影響。
結果顯示:當析鍍偏壓越高、鍍液中硫酸亞錫濃度越高微柱錫含量也越高，當兩極間之偏壓設定在3.00 V、硫酸亞錫濃度控制為0.035 M，電鍍所得之含銅、錫二元金屬微柱，經分析其化學組成為含銅、錫(Cu: 88.2 ± 0.6 at. % 與Sn: 11.8± 0.6 at. %) 二元金屬之微柱，晶體結構分析顯示含Cu6Sn5相、Sn相二相，且根據Scherrer equation計算析鍍偏壓越大晶粒尺寸也隨之減少。以奈米壓痕儀測量其機械性質，其硬度為8.10 ± 0.40 GPa，楊氏模數為127.83 ± 5.20 GPa；以電化學分析量測其抗蝕性能，其腐蝕電流(Icorr)為0.27×10-2 mA/cm2，線性極化阻抗(RLP)為1435 ohm。
微螺旋析鍍結果顯示，析鍍角度30 °、製程參數4為銅錫合金及Cu6Sn5微螺旋之最佳析鍍參數，微螺旋線徑最為均勻，其d2/d1線徑比值為112 %，d3/d1線徑比值為129 %。

摘要(英)

In this study, three-dimensional microstructures of copper-tin alloys and its intermetallic compounds were prepared by instant image guided micro-plating.
The electroplating system uses a platinum wire with a wire diameter of 125 μm as an anode, and a copper wire with a diameter of 0.643 mm as a cathode and Cathode and anode distance is 80 μm, which is electroplated in an electroplating bath containing copper sulfate, stannous sulfate, sodium citrate and ascorbic acid
to manufacture three dimensional micro-structure with two metal elements of copper and tin. The goal of this research is to firstly investigate the effect of applying different bias and adding different concentrations of stannous sulfate on the surface morphology, chemical composition, crystal structure and reduction potential of the micro-column in the plating bath, and then seek to find the best electroplating conditions of electroplating micro-columns with two metal elements of copper and tin. Then using these conditions to research the feasibility of making micro-helix, and studying the influence of micro-helix electroplating angle and process parameters on micro-helix size and the variation of wire diameter.
The results showed that When the plating bias is higher and the higher the concentration of stannous sulfate in the electroplating bath, the higher the micro-column tin content. When the bias is set at 3.00 V and the concentration of stannous sulfate is 0.035 M, the copper and tin binary metal micro-column obtained by electroplating have the best surface morphology. After analyzing, its chemical composition is Cu: 88.2 ± 0.6 at.% and Sn: 11.8±0.6 at.%. The crystal structure analysis shows that the crystal structure is Cu6Sn5, Sn coexisting. According to the Scherrer equation, the larger the plating bias, the smaller the grain size.The mechanical properties of the micro-column were measured by a nanoindenter. The hardness was estimated to be 8.10 ± 0.40 GPa and the Young′s modulus was 127.83 ± 5.20 Gpa. The corrosion resistance was measured by electrochemical measurement. The corrosion current (Icorr) was 0.27×10-2 mA/cm2, linear polarization resistance (RLP) is 1435 ohm.
The results of electroplating micro-helix showed that electrochemical deposition angle 30 ° and process parameter 4 is the best electroplating parameter of copper-tin intermetallic compound helix because the diameter of helix wire d1、d2、d3 are the most close, the d2 / d1 ratio is 112 %, the d3 / d1 ratio is 129 %.

關鍵字(中)

★ 微陽極導引電鍍
★ 銅錫微柱
★ 銅錫微螺旋
★ 奈米壓痕
★ 奈米晶

關鍵字(英)

★ Micro-anode guided electroplating
★ Copper-Tin micro-column
★ Copper-Tin micro-helix
★ Nano indentation
★ Nanocrystal

論文目次

目錄
摘要 i
ABSTRACT iii
誌謝 v
表目錄 x
圖目錄 xi
第一章、前言 - 1 -
1-1 研究背景 - 1 -
1-2 研究動機與目的 - 2 -
第二章、基礎理論與文獻回顧 - 3 -
2-1 電鍍原理 - 3 -
2-2 合金電鍍 - 3 -
2-3局部電化學沉積發展之文獻回顧 - 4 -
2-4 局部電化學沉積之本實驗室發展 - 6 -
2-5 銅錫合金電鍍 - 7 -
2-6 奈米壓痕測試估計材料之硬度與楊氏模數 - 8 -
第三章、研究方法 - 10 -
3-1 研究方法流程 - 10 -
3-2 即時影像導引微電鍍系統之架設 - 10 -
3-3 微陽極與陰極製備 - 12 -
3-4 鍍液調配 - 12 -
3-5 實驗步驟 - 12 -
3-5-1微柱析鍍參數探討 - 12 -
3-5-2微螺旋結構之析鍍角度與製程參數之探討 - 13 -
3-6 分析儀器 - 14 -
3-6-1鍍液酸鹼度量測 - 14 -
3-6-2形貌觀察 - 14 -
3-6-3化學組成分析 - 14 -
3-6-4晶體結構分析 - 15 -
3-6-5示差掃描熱分析 - 15 -
3-6-6奈米壓痕測試 - 15 -
3-6-7陰極極化曲線量測 - 16 -
3-6-8抗蝕性能量測 - 16 -
3-6-9電場模擬 - 17 -
第四章、結果 - 18 -
4-1 銅錫合金及Cu6Sn5微柱析鍍參數探討 - 18 -
4-1-1形貌觀察 - 19 -
4-1-2平均析鍍電流與平均析鍍速率之分析 - 19 -
4-1-3化學組成分析 - 20 -
4-1-4陰極極化分析 - 21 -
4-1-5晶體結構分析 - 22 -
4-1-6微柱之析鍍參數探討示差掃描熱分析 - 22 -
4-1-7奈米壓痕測試 - 23 -
4-1-8抗蝕性能量測 - 24 -
4-1-9電場強度模擬 - 25 -
4-2 微螺旋析鍍參數探討 - 25 -
4-2-1 微螺旋直徑與螺距量測 - 26 -
4-2-2 微螺旋線徑量測 - 27 -
4-2-3 微螺旋析鍍之電場強度模擬 - 27 -
第五章、討論 - 29 -
5-1 析鍍參數對析鍍微柱之影響 - 29 -
5-1-1 析鍍偏壓對微柱平均柱徑之影響 - 29 -
5-1-2 析鍍參數對微柱錫含量之影響 - 29 -
5-1-3 析鍍偏壓對微柱晶體尺寸之影響 - 30 -
5-1-4 探討XRD分析和DSC分析結果 - 30 -
5-1-5 析鍍參數對機械性質之影響 - 31 -
5-1-6 析鍍參數對抗蝕性能之影響 - 31 -
5-1-7 最佳析鍍參數之選擇 - 32 -
5-2 析鍍角度與製程參數對析鍍微螺旋之影響 - 33 -
5-2-1 析鍍角度與製程參數對螺旋直徑與螺距之影響 - 33 -
5-2-2 電場強度與螺旋線徑均勻度之關係 - 33 -
第六章、結論與前瞻 - 35 -
參考文獻 - 37 -

表目錄
表3-1電鍍液中硫酸亞錫為0.035 M之成分 - 42 -
表3-2電鍍液中硫酸亞錫為0.040 M之成分 - 42 -
表3-2電鍍液中硫酸亞錫為0.045 M之成分 - 43 -

表4-1 各析鍍參數析鍍微柱之柱徑量測結果 - 43 -
表4-2 各析鍍參數之平均析鍍電流量測結果 - 44 -
表4-3 各析鍍參數之平均析鍍速率量測結果 - 44 -
表4-4 各析鍍參數析鍍的微柱之EDS分析結果 - 45 -
表4-5 各析鍍參數之X光繞射圖之主峰半高寬 - 45 -
表4-6 各析鍍參數之X光繞射圖主峰2θ角度 - 46 -
表4-7 各析鍍參數由Scherrer equation計算之晶粒尺寸大小 - 46 -
表4-8固定硫酸亞錫濃度0.035 M下，不同析鍍偏壓析鍍的微柱之硬度與楊氏模數(單位: GPa) - 47 -
表4-9固定硫酸亞錫濃度0.040 M下，不同析鍍偏壓析鍍的微柱之硬度與楊氏模數(單位: GPa) - 47 -
表4-10固定硫酸亞錫濃度0.045 M下，不同析鍍偏壓析鍍的微柱之硬度與楊氏模數(單位: GPa) - 48 -
表4-11各參數條件析鍍的微柱之腐蝕電流量測結果 - 48 -
表4-12各參數條件析鍍的微柱之線性極化阻抗量測結果 - 49 -
表4-13不同析鍍偏壓下，Comsol模擬電場之中心最大值 - 49 -
表4-14以不同析鍍角度與製程參數析鍍微螺旋之螺旋直徑量測結果 - 50 -
表4-15以不同析鍍角度與製程參數析鍍微螺旋之螺距量測結果 - 50 -
表4-16以析鍍角度30 °於不同製程參數析鍍微螺旋之線徑量測結果 - 51 -
表4-17以析鍍角度50°於不同製程參數析鍍微螺旋之線徑量測結果 - 51 -
表4-18以析鍍角度70°於不同製程參數析鍍微螺旋之線徑量測結果 - 52 -
表4-19以不同析鍍角度與製程參數析鍍微螺旋之平均線徑量測結果 - 52 -
表4-20不同製程參數與析鍍角度於d1、d2、d3之電場大小 - 53 -

圖目錄
圖2-1銅錫合金平衡相圖[49] - 54 -
圖2-2奈米壓痕負載-深度圖[41] - 55 -

圖3-1第一部分實驗流程圖 - 55 -
圖3-2第二部分實驗流程圖 - 56 -
圖3-3微電鍍微柱設備示意圖 - 56 -
圖3-4 微電鍍微螺旋設備示意圖 - 57 -
圖3-5 微陽極製備示意圖 - 57 -
圖3-6 陰極製備示意圖 - 58 -
圖3-7 微螺旋析鍍角度示意圖 - 58 -
圖3-8 微螺旋製程參數示意圖 - 59 -
圖3-9 微螺旋幾何尺寸示意圖 - 59 -
圖3-10 陰極極化曲線量測設備示意圖 - 60 -
圖3-11 腐蝕電化學量測設備示意圖 - 60 -
圖3-12 析鍍微柱之電場強度模擬結果 - 61 -
圖3-13 析鍍微螺旋之電場強度模擬結果 - 62 -

圖 4-1 析鍍參數析鍍的微柱之放大40倍SEM影像，(a)~(d)為固定硫酸亞錫濃度0.035 M時，析鍍偏壓由3.00 V上升至3.45 V；(e)~(h)為定硫酸亞錫濃度0.040 M時，析鍍偏壓由3.00 V上升至3.45 V；(i)~(l)為定硫酸亞錫濃度0.045 M時，析鍍偏壓由3.00 V上升至3.45 V - 63 -
圖4-2 各析鍍參數析鍍的微柱之平均柱徑分析結果 - 64 -
圖4-3 各析鍍參數之平均析鍍電流分析結果 - 64 -
圖4-4 各析鍍參數之平均析鍍速率分析結果 - 65 -
圖4-5 各析鍍參數析鍍微柱之EDS分析結果 - 65 -
圖4-6將鍍液之金屬離子逐一抽離之陰極極化量測結果 - 66 -
圖4-7 將鍍液之金屬離子逐一抽離之陰極極化量測結果 - 66 -
圖4-8 將鍍液之金屬離子逐一抽離之陰極極化量測結果 - 67 -
圖4-9 硫酸亞錫濃度(a)0.035 M、(b) 0.040 M、(c) 0.045 M下不同析鍍偏壓析鍍的微柱之X光繞射圖譜 - 68 -
圖4-10 硫酸亞錫濃度為0.040 M時，各析鍍偏壓之DSC曲線 - 69 -
圖4-11 硫酸亞錫濃度(a)0.035 M、(b) 0.040 M、(c) 0.045 M下，不同析鍍偏壓析鍍的微柱之奈米壓痕負載力-壓痕深度曲線圖 - 71 -
圖4-12 硫酸亞錫濃度(a)0.035 M、(b) 0.040 M、(c) 0.045 M下，不同析鍍偏壓析鍍微柱之塔弗極化量測結果 - 73 -
圖4-13 硫酸亞錫濃度(a)0.035 M、(b) 0.040 M、(c) 0.045 M下，不同析鍍偏壓析鍍微柱之線性極化量測結果 - 75 -
圖4-14 不同析鍍偏壓之電場強度模擬結果 - 76 -
圖4-15 不同析鍍角度與製程參數製得的微螺旋之影像圖，(a)析鍍角度: 30 °、製程參數: 2，(b)析鍍角度: 30 °、製程參數: 3，(c)析鍍角度: 30 °、製程參數: 4，(d)析鍍角度: 50 °、製程參數: 2，(e)析鍍角度: 50 °、製程參數: 3，(f)析鍍角度: 50 °、製程參數: 4，(g)析鍍角度: 70 °、製程參數: 2，(h)析鍍角度: 70 °、製程參數: 3，(i)析鍍角度: 70 °、製程參數: 4。 - 77 -

圖5-1改變析鍍偏壓之電場和微柱柱徑關係圖。 - 78 -
圖5-2電場和微柱柱徑關係圖。 - 78 -
圖5-3 各析鍍參數與微柱硬度之關係圖 - 79 -
圖5-4 各析鍍參數與微柱楊氏模數之關係圖 - 79 -
圖5-5 化學組成與硬度、楊氏模數之關係圖 - 80 -
圖5-6化學組成與腐蝕電流(Icorr)大小之關係圖。 - 80 -
圖5-7化學組成與與線性極化阻抗(RLP)大小之關係圖。 - 81 -
圖5-8 析鍍角度及製程參數與微螺旋直徑之關係圖。 - 81 -
圖5-9 析鍍角度及製程參數與微螺旋間距分析圖。 - 82 -

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指導教授

林景崎(Jing-Chie Lin)

審核日期

2019-8-20

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