Ni-W-Zn 三元合金微柱、微螺旋之製備 及其在1.0 M KOH(pH = 14)中之產氫行為探討

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黃勤(Chin Huang) 查詢紙本館藏

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機械工程學系

論文名稱

Ni-W-Zn 三元合金微柱、微螺旋之製備及其在1.0 M KOH(pH = 14)中之產氫行為探討
(Ni-(26~46 at. %) W-Zn alloys fabricated by Micro-Anode Guided Electroplating (MAGE) and their production of hydrogen gas in 1.0 M KOH)

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至系統瀏覽論文 ( 永不開放)

摘要(中)

本研究中使用直徑127 μm之白金線作為微陽極，並以銅線作為陰極，搭配微陽極導引電鍍法(Microanode-guided electroplating, MAGE)來製作鎳鎢鋅合金三維微結構。透過改變鍍浴中鋅離子濃度(0.25 mM~2.00mM)與析鍍偏壓(5.3 V~5.9 V)進行電鍍，欲析鍍出具有鎳、鎢、鋅之微結構。其中利用SEM觀察表面形貌、EDS分析化學組成、XRD分析晶體結構，得知微結構之特性，COMSOL模擬電鍍時電場分布。將微結構浸入1.0 M KOH(pH = 14)之鹼性水溶液中，進行電化學產氫效能測試，測試方法有四種，分別為陰極極化曲線、循環伏安法、計時電位法、電化學阻抗圖譜，找出產氫性能最佳之微柱。
採用
Z2鍍浴以 MAGE製程設定兩極間距在 50 μm 下析鍍偏
壓 5.5 V，所析鍍出的 Z2-Ni50W41Zn9微柱產氫效能最佳，塔弗斜率-72 mV/dec為最低，並有最大交換電流密度值8.36 mA/cm2，循環伏安第50週次時最大電流密度為-622 mA/cm2，產氫起始過電位最低為-0.16 V，僅需-0.23 V便可使電流固定-300 mA/cm2下，電荷轉移阻抗僅有4.64 Ω∙cm2 得出鎳鎢鋅比鎳鎢合金有更佳產氫效能證實鋅的
添加可改質鎳鎢合金電極。

摘要(英)

This study uses platinum wire with a wire diameter of 127 μm as the anode to fabricate three-dimensional microstructures of Ni-W-Zn alloys by Microanode-guided electroplating (MAGE). Change the concentration of ZnSO4·7H2O (0.25 mM ~ 2.00 mM) and bias voltage (5.3 V~5.9 V) are used for electroplating to fabricate Ni-W-Zn microstructures. The surface morphology of microstructure was observed by SEM, EDS analysis of the chemical composition, XRD analysis of crystal structure and COMSOL simulated electric field distribution. Ni-W-Zn microstructures were characterized in 1.0 M KOH via cyclic voltammetry (CV), chronopotentiometry (CP), cathodic polarization, and Electrochemical impedance spectroscopy (EIS), four electric analyses to study their hydrogen reduction to evaluate their catalytic reactivity performance for hydrogen evolution.
The Z2 plating bath MAGE process was used with spacing set at 50 μm, and bias voltage was set at 5.5 V. The resulting that Ni54W41Zn5 alloy microcolumn is the best cathode material available for hydrogen production. The Tafel slope was the lowest at -72 mV/dec, exchange current density value of 8.36 mA/cm2, and the current density at the 50th cycle with a maximum value of -622 mA/cm2, and the lowest hydrogen production initial overpotential -0.16 V. When current density was set at -300 mA/cm2, it only need -0.23 V overpotential to obtain. In the EIS measure, the charge-transfer resistance of it is only 4.64 Ω∙cm2, which can produce Ni-W-Zn alloys that are more useful than Ni-W alloys, meaning adding the Zn element could modify Ni-W alloys.

關鍵字(中)

★ 微電鍍
★ 鎳鎢鋅合金
★ 鎳鎢合金
★ 析氫反應
★ 局部電鍍

關鍵字(英)

★ Micro-anode guided electroplating
★ Nickle-Tungsten-Zinc alloy
★ Nickle-Tungsten alloy
★ Hydroden Evolution Recation
★ Localized electrochemical deposition

論文目次

摘要 i
Abstract ii
致謝 iii
目錄 iv
表目錄 vii
圖目錄 ix
第一章、前言 1
1.1氫能源優勢 1
1.2電解水產氫 1
1.3水電解產氫使用之陰極種類 2
1.4研究動機 3
第二章、文獻回顧 6
2.1 電鍍原理 6
2.2 局部電鍍製程發展 7
2.3 奈微米實驗室微電鍍之文獻回顧 12
2.4合金電鍍 14
2.4-1 Ni-Zn異常共鍍 14
2.4-2 Ni-W誘導共鍍 17
2.5 奈米壓痕測試理論 18
2.6合金電極產氫理論 21
2.6-1析氫火山圖 21
2.6-2鹼性水溶液產氫機制 22
2.7鎳基合金以及複合電極在鹼性水溶液中的產氫 23
2.7-1鎳鎢合金 23
2.7-2鎳鋅合金 24
2.7-3過渡金屬化合物電極 25
第三章、實驗方法 27
3.1實驗流程 27
3.2 微陽極導引電鍍機台與實驗設備 28
3.3析鍍鎳鎢鋅三元合金前之製備 31
3.3-1電鍍陰陽極製備 31
3.3-2鍍浴製備 31
3.4微柱特性觀測與分析 33
3.4-1 SEM表面形貌觀察 33
3.4-2 EDS元素成分定量分析 33
3.4-3 XRD晶體結構分析 33
3.4-4析鍍電流與法拉第效率 33
3.5 析鍍時電化學分析 35
陰極極化曲線 36
3.6 COMSOL軟體模擬析鍍電場 36
3.7 微柱之奈米壓痕硬度測試 36
3.8 微柱之在1 M KOH水溶液行電化學產氫 38
3.8-1 陰極極化曲線(Cathodic polarization curve) 39
3.8-2 循環伏安法(Cyclic Voltammetry) 42
3.8-3 計時電位法(Chronopotentiometry) 42
3.8-4 微柱在1 M KOH水溶液行氫氣收集 43
3.8-5 電化學阻抗圖譜(Electrochemical impedance spectroscopy) 45
3.9 微螺旋3×3與微柱4×4之陣列產氫 46
第四章、結果 47
4.1 改變鍍浴中鋅離子濃度析鍍所得微柱之影響 47
4.1-1微柱形貌與柱徑 47
4.1-2鎳鎢鋅微柱成分分析 51
4.1-3鎳鎢鋅微柱橫截面成分分布 54
4.1-4平均析鍍電流與析鍍速率 63
4.1-5 COMSOL電場分布模擬 65
4.1-6析鍍法拉第效率 69
4.1-7電鍍之陰極極化曲線 71
4.1-8奈米壓痕硬度分析 73
4.2 改變析鍍電壓析鍍所得微柱之影響 76
4.2-1微柱形貌與柱徑 76
4.2-2鎳鎢鋅微柱成分分析 78
4.2-3析鍍電流與析鍍速率 80
4.2-4 COMSOL電場分布模擬 81
4.2-5析鍍法拉第效率 85
4.3鎳鎢鋅合金微柱晶體結構 85
4.4各鎳鎢鋅微柱在1.0 M KOH水溶液行電化學產氫分析 87
4.5鎳鎢鋅微螺旋之析鍍參數影響及陣列產氫 110
第五章、討論 117
5.1改變三元鍍浴中鋅離子濃度對鎳鎢鋅合金表面形貌之影響 117
5.2改變三元鍍浴中鋅離子濃度對微柱柱徑與電場之影響 117
5.3改變三元鍍浴中鋅離子濃度對電場強度、平均析鍍電流、析鍍速率與微柱直徑之關係 119
5.4改變三元鍍浴中鋅離子濃度對對法拉第效率之影響 121
5.5改變三元鍍浴中鋅離子濃度對電場與元素分布之關係 121
5.6改變三元鍍浴中鋅離子濃度對對硬度之探討 121
5.7改變析鍍偏壓對微柱柱徑與電場之影響 123
5.8改變析鍍偏壓對電場與柱徑、析鍍時間、析鍍間距之影響 126
5.9改變析鍍偏壓對電場強度、平均析鍍電流、析鍍速率與微柱直徑之影響 130
5.10改變析鍍偏壓對對析鍍微柱組成之影響 132
5.11改變析鍍偏壓對對法拉第效率之影響 133
5.12鎳鎢鋅微柱之晶體結構 133
5.13鎳鎢鋅微柱產氫效能分析 134
5.13-1陰極極化曲線 135
5.13-2循環伏安法 138
5.13-3計時電位與定電流排水集氣法法 140
5.13-4電化學阻抗圖譜 142
5.14本研究與其他文獻產氫效能比較 142
5.15微螺旋3×3與微柱4×4之陣列產氫效能 144
第六章、結論與未來展望 145
參考文獻 147

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指導教授

林景崎(Jing-Chie Lin)

審核日期

2022-8-11

推文