自焦磷酸浴中以微陽極導引電鍍製備鎳-鎢合金微柱、微螺旋及其在1.0 M KOH 中電解產氫特性研究

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謝東佑(Tung-Yu Hsieh) 查詢紙本館藏

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材料科學與工程研究所

論文名稱

自焦磷酸浴中以微陽極導引電鍍製備鎳-鎢合金微柱、微螺旋及其在1.0 M KOH 中電解產氫特性研究
(Fabrication of Ni-W alloying micro-pillars & micro-helices by MAGE in pyrophosphate and their HER in 1.0 M KOH solution)

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摘要(中)

本研究中使用微陽極導引電鍍法(Microanode-guided electroplating, MAGE)來製作鎳鎢合金三維微結構。使用線徑125 μm之白金線作為陽極，以線徑為0.643 mm之銅導線作為陰極，於焦磷酸浴中改變析鍍偏壓(5.6 V~6.2 V)與間距(50 μm~80 μm)等條件進行電鍍，希望製作出含鎳、鎢兩金屬元素之微柱與微螺旋結構。再透過SEM觀察表面形貌、EDS分析化學組成、XRD分析晶體結構及COMSOL模擬電場分布，尋求最佳的鎳鎢合金微柱之電鍍條件。再進一步使用循環伏安法、計時電位法、線性極化分析法來探討鎳鎢微柱在鹼性水溶液中的產氫表現。
結果顯示: 析鍍偏壓為6.0 V和間距為60 μm的情況下進行鎳鎢合金之電鍍時，最大的電場強度為118233 V/m，有最高的鎢含量42.3±0.8 at.%。在1.0 M KOH溶液中，也具有最佳的產氫效能，陰極峰值電流密度會有最大的-593.63 mA/cm2，且有最低的產氫起始過電位-0.2 V，在-300 mA/cm2下有最小的電位-0.25 V，最小的Tafel slope為75 mV/dec，最大的交換電流密度值為0.803 mA/cm2。

摘要(英)

Micro-anode guided electrodeposition (MAGE) process was used to fabricate three-dimensional microstructures of Ni-W alloys in this study.Use platinum wire with a wire diameter of 125 μm as the anode, and a copper wire with a wire diameter of 0.643 mm as the cathode. Change the bias voltage (5.6 V~6.2 V) and spacing (50 μm~80 μm) in a pyrophosphate bath. The goal is to produce micro-pillars and micro-helical structures containing two metal elements of nickel and tungsten. Then observe the surface morphology through SEM, EDS analysis of chemical composition, XRD analysis of crystal structure and COMSOL simulated electric field distribution to find the best nickel-tungsten alloy micro-pillar plating conditions. Furthermore, cyclic voltammetry, chronopotentiometry, and linear polarization analysis were used to explore the hydrogen production performance of nickel-tungsten micro-columns in alkaline solutions.
The results show that when nickel-tungsten alloy electroplating is performed with a bias voltage of 6.0 V and a spacing of 60 μm, the maximum electric field strength is 118233 V/m, and the highest tungsten content is 42.3±0.8 at.%. In 1.0 M KOH solution, it also has the best hydrogen production efficiency. The peak current density of the cathode will have the largest -593.63 mA/cm2, and the lowest hydrogen production initial overpotential -0.2 V, at -300 mA/cm2 There is the smallest potential -0.25 V, the smallest Tafel slope is 75 mV/dec, and the largest exchange current density is 0.803 mA/cm2.

關鍵字(中)

★ 微電鍍
★ 微螺旋
★ 焦磷酸
★ 鎳鎢合金
★ 產氫

關鍵字(英)

★ Micro-anode guided electroplating
★ Micro-helix
★ Pyrophosphate
★ Nickle-Tungsten alloy
★ Hydroden Evolution Recation

論文目次

目錄
摘要 i
Abstract vi
目錄 viii
表目錄 xv
圖目錄 xix
第一章、前言 1
1-1 研究背景 1
1-2 研究目的與動機 2
第二章、文獻回顧與基礎理論 4
2-1 微電鍍之原理與技術發展 4
2-1-1 電鍍原理 4
2-1-2 電鍍法拉第效率 5
2-1-3 合金電鍍 6
2-1-4 局部電化學電鍍製程之發展 8
2-1-5 奈微米材料實驗室微電鍍製程之發展 9
2-1-6 COMSOL電場模擬軟體之有限元素分析 11
2-1-7 奈米壓痕測試材料之硬度與楊氏模數 12
2-1-8 微米柱壓縮測試 13
2-2 產氫技術之發展概況 14
2-2-1 電解水產氫機制 16
2-2-2 非貴金屬陰極材料之開發關鍵 18
2-2-3 鎳基合金用於水電解產氫陰極之相關研究 20
2-2-3 (A) Ni-Zn合金 20
2-2-3 (B) Ni-S合金 21
2-2-3 (C) Ni-Co合金 23
2-2-3 (D) Ni-Mo合金 24
2-2-3 (E) Ni-W合金 26
第三章、實驗方法 28
3-1 實驗流程 28
3-2 實驗設備 29
3-3 陰陽極製作 30
3-4 鍍液組成 30
3-5 微陽極導引電鍍法 31
3-5-1 單軸式 31
3-5-2 四軸式 31
3-6 掃瞄式電子顯微鏡/能量色散X射線譜 32
3-7 X光繞射儀 32
3-8 機械性質量測 33
3-9 電場模擬 33
3-10 電化學測試 34
3-10-1 析鍍極化曲線 34
3-10-2 循環伏安法 34
3-10-3 計時電位法 35
3-10-4 產氫極化曲線 35
3-10-5 定電壓收集氫氣法 36
3-10-6 電化學阻抗分析圖譜 36
第四章、結果 37
4-1 鎳鎢合金微柱析鍍參數之影響 37
4-1-1 鎳鎢合金微柱之表面形貌分析 37
4-1-2 鎳鎢合金微柱之COMSOL模擬分析 39
4-1-3 鎳鎢合金微柱之析鍍電流 40
4-1-4 鎳鎢合金微柱之電鍍極化曲線 41
4-1-5 鎳鎢合金微柱之電化學阻抗圖譜分析 41
4-1-6 鎳鎢合金微柱之析鍍速率 42
4-1-7 鎳鎢合金微柱之化學組成分析 43
4-1-8 鎳鎢合金微柱之晶體結構分析 44
4-1-9 鎳鎢合金微柱之法拉第效率分析 45
4-1-10 鎳鎢合金微柱之機械性質分析 46
4-2 鎳鎢合金微螺旋析鍍參數之影響 48
4-2-1 鎳鎢合金微螺旋析鍍之螺旋直徑 48
4-2-2 鎳鎢合金微螺旋析鍍之螺旋間距 48
4-2-3 鎳鎢合金微螺旋析鍍之線徑 49
4-2-4 鎳鎢合金微螺旋結構之析氫效能 51
4-3 鎳鎢合金微柱之析氫反應 51
4-3-1 循環伏安法 52
4-3-2 計時電位法 53
4-3-3 產氫極化曲線 55
4-3-4 定電壓收集氫氣法 56
第五章、討論 58
5-1 析鍍參數對析鍍鎳鎢微柱之探討 58
5-1-1 析鍍參數對COMSOL電場模擬之探討 58
5-1-2 析鍍參數對表面形貌之探討 58
5-1-3 析鍍參數對析鍍電流之探討 61
5-1-4 析鍍參數對電鍍極化之探討 61
5-1-5 析鍍參數對電化學阻抗圖譜之分析探討 63
5-1-6 析鍍參數對析鍍速率之探討 63
5-1-7 析鍍參數對微柱成分之探討 65
5-1-8 析鍍參數對晶體結構之探討 66
5-1-9 析鍍參數對析鍍法拉第效率之探討 67
5-1-10 析鍍參數對微柱機械性質之探討 68
5-2 鎳鎢合金微螺旋結構探討 68
5-2-1 析鍍參數對鎳鎢合金微螺旋直徑之探討 69
5-2-2 析鍍參數對鎳鎢合金微螺旋螺距之探討 69
5-2-3 析鍍參數對鎳鎢合金微螺旋線徑之探討 70
5-2-4 析鍍參數對鎳鎢合金微螺旋結構析氫效能之探討 71
5-3 鎳鎢微柱析氫反應之探討 72
5-3-1 循環伏安法之探討 73
5-3-2 計時電位法之探討 74
5-3-3 產氫極化之探討 75
5-3-4 定電壓排水集氣法之探討 77
第六章、結論與未來展望 79
參考文獻 81

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指導教授

林景崎(Jing-Chie Lin)

審核日期

2022-3-9

推文