以微電鍍法析鍍鎳鎢合金微結構並研究其在鹼性溶液電解產氫行為

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姓名

李盈家(Lee-Ying-Chia) 查詢紙本館藏

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材料科學與工程研究所

論文名稱

以微電鍍法析鍍鎳鎢合金微結構並研究其在鹼性溶液電解產氫行為
(Ni-(20~40 at. %) W alloyed micro features prepared by MAGE process and their electrolytic behavior of hydrogen production in the alkaline solution)

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摘要(中)

本研究中使用微陽極導引電鍍(Microanode-guided electroplating, MAGE)來製造鎳鎢合金微結構。電鍍製程中改變鍍浴酸鹼值(6.0~7.5)與溫度(60 °C~75 °C)等條件對析鍍鎳鎢合金微結構表面形貌、化學組成、結晶構造、機械性質等之影響。表面形貌以冷場發射掃描式電子顯微鏡觀測，晶體構造以X光繞射儀分析。電鍍過程監測析鍍電流，並對產物秤重，以計算電流效率。結果顯示: 鍍浴pH 在7.5、溫度75 °C時，所產出的鎳鎢合金微結構具較平滑表面，鎢含量可達37 at.%。
若以鎳鎢合金作為鹼性溶液電解產氫的陰極時，由於其氫還原的交換電流密度高、氫過壓低，因而成為當前產氫的熱門陰極材料。本論文以MAGE所製造出來的鎳鎢合金微結構，以循環伏安法、計時電位法、Tafel極化分析法來檢測此合金在鹼性水溶液中的產氫表現。結果顯示:含37 at.% W的鎳鎢合金微結構，具有最大的交換電流密度(6.01  10-1 mA/cm2)，最小的Tafel slope (80 mV/dec)。計時電位法之結果顯示，含38 at.% W的合金微柱在1.0 M KOH溶液中，以定電流-300mA/cm2經過六小時的電解產氫，其電位始終維持在-0.30±0.07 V，並無明顯的漂移，顯示此材料相當穩定，是鹼性水溶液電解產氫及有潛力之候選材料。

摘要(英)

Micro-anode guided electrodeposition (MAGE) process was used to fabricate three-dimensional (3-D) micro features of Ni-W alloys in this work. The effect of pH value (from 6.0 to 7.5) and the bath temperature (60~75 °C) on the surface morphology, chemical composition, crystallographic microstructure and mechanical property was investigated. The surface morphology was observed through SEM and the chemical composition determined by EDS; the crystallographic microstructure phase was examined by XRD. The micro feature was weighed and compared to the overall electrical quantity evaluated by integration of the current with time to calculate the cathodic current efficiency. As a result, the Ni-W micro features containing 37 at.% W in smooth surface was attained in a 75 °C-bath with pH of 7.5.
Nickel-tungsten alloy is known as a good cathode material used to produce hydrogen gas by means of electrolysis in the alkaline water solution because of high exchange current density and low overvoltage of the hydrogen evolution reaction (HER). Micro features of the Ni-W alloys from MAGE were investigated in terms of cyclic voltammetry (CV), chronoamperometry (CP) and Tafel polarization to study their cathodic behavior of water electrolysis. The alloy containing 37 at.% W resulted from the MAGE in the 75 °C-bath with pH of 7.5 revealed the best HER efficiency. It demonstrated the highest exchange current density (6.01 x 10-1 mA/cm2) and lowest Tafel slope (80 mV/dec). The chronopotentiometry of the 37 at.% W alloy conducted at- 300 mA/cm2 in1.0 M KOH displayed a stable potential at -0.30±0.07 V without showing any significant shift within 6 hours. This fact indicates that this material is a stable and excellent cathode candidate for HER in the alkaline electrolysis.

關鍵字(中)

★ 微電鍍
★ 鎳鎢合金
★ 產氫

關鍵字(英)

論文目次

摘要 i
Abstract ii
目錄 iv
圖目錄 xi
表目錄 xx
第一章、前言 1
1-1 全球能源使用近況 1
1-1-1 Power-to-gas 技術 1
1-2 水解產氫的介紹 2
1-3 電解水電極材料發展 2
1-4 研究動機與目的 3
第二章、文獻回顧與基礎理論 5
2-1 鹼性水溶液中的產氫原理 5
2-2 不同鎢含量之鎳鎢合金對於在鹼性水溶液中產氫反應的影響 6
2-3 電鍍原理 7
2-4 合金電鍍 9
2-4-1 規則共鍍 (regular codeposition) 10
2-4-2 誘導共鍍(induced codeposition)之鐵族與鎢金屬共鍍: 10
2-5 在檸檬酸鹽鍍液中加入氨水對於鎳鎢合金成分的影響 14
2-6 鍍浴中無添加氨水時不同酸鹼值下對於析鍍鎳鎢合金之影響 14
2-7 鍍浴中無添加氨水時不同析鍍溫度下對於析鍍鎳鎢合金之影響 15
2-8 法拉第效率 16
2-9 鎳鎢合金之陰極極化曲線 17
2-10 鎳鎢合金之結晶相 18
2-11 局部電化學微製造技術之發展 19
2-12 微奈米實驗室微電鍍之研究歷程 21
第三章、實驗方法 23
3-1 實驗流程 23
3-2 電鍍之實驗設備 23
3-3 陰陽極製備 25
3-4 鍍浴組成 26
3-5 微陽極導引電鍍法 26
3-6 鎳鎢合金之表面形貌觀察與組成分析 27
3-7 晶體結構分析 27
3-8 奈米壓痕試驗 28
3-9 法拉第效率計算 30
3-10 陰極極化曲線測量 30
3-11 Comsol之電場模擬方式與設定 31
3-12 產氫裝置設置 31
3-13 循環伏安法 32
3-14 定電壓收集氫氣法 32
3-15 計時電位法 33
3-16 產氫極化曲線與Tafel參數 33
第四章、結果 35
4-1 不同酸鹼值鍍浴所得之鎳鎢合金差異 35
4-1-1 表面形貌與柱徑 35
4-1-2 成分分析 36
4-1-3 晶體結構 36
4-1-4 微硬度分析 37
4-1-5 析鍍電流與析鍍速率 37
4-1-6 導電度與電場強度 38
4-1-7 極化曲線 38
4-1-8 微柱重量與法拉第效率 39
4-2 不同鍍浴溫度所得之鎳鎢合金差異 39
4-2-1 表面形貌與柱徑 39
4-2-2 成分分析 40
4-2-3 晶體結構 41
4-2-4 析鍍電流與析鍍速率 41
4-2-5 導電度 42
4-2-6 極化曲線 42
4-2-7 微柱重量與法拉第效率 43
4-3 鎳鎢合金之循環伏安法 43
4-3-1 改變酸鹼值之差異 44
4-3-2 改變析鍍溫度之差異 44
4-4 定電壓排水集氫氣法 45
4-4-1 改變酸鹼值之差異 45
4-4-2 改變析鍍溫度之差異 46
4-5 產氫下之極化曲線 47
4-6 計時電位法 48
4-7 產氫後之鎳鎢合金表面形貌 49
4-7-1 改變酸鹼值之差異 49
4-7-2 改變析鍍溫度之差異 49
4-8 產氫前後之鎳鎢成分分析 49
4-8-1 改變析鍍酸鹼值之差異 49
4-8-2 改變析鍍溫度之差異 50
第五章、討論 51
5-1 改變鍍浴酸鹼值對析鍍微柱組成之影響 51
5-2 改變鍍浴酸鹼值對析鍍微柱之XRD晶體結構與微柱外觀之關係 51
5-3 改變鍍浴酸鹼值對硬度之影響 53
5-4 改變鍍浴酸鹼值之導電度、電場強度、平均析鍍電流、析鍍速率與微柱直徑之關係 53
5-5 改變鍍浴酸鹼值之極化曲線解析 54
5-6 改變鍍浴酸鹼值對法拉第效率之影響 55
5-7 改變鍍浴溫度對析鍍微柱組成之影響 56
5-8 變鍍浴溫度對析鍍為柱之XRD晶體結構、微柱外觀與析鍍速率之關係 56
5-9 改變鍍浴溫度對導之導電度、平均析鍍電流、析鍍速率與微柱直徑之關係 57
5-10 改變鍍浴溫度之極化曲線解析 58
5-11 改變鍍浴溫度對法拉第效率的影響 59
5-12 產氫效能分析 60
5-12-1 改變鎢含量的影響 60
5-12-2 改變析鍍溫度的影響 64
5-13 產氫前後外觀與成分差異討論 65
5-14 產氫效能比較 66
第六章、結論與未來展望 67

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指導教授

林景崎

審核日期

2020-8-20

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