以微電鍍法製備鎳鈷鐵、鎳鈷鐵鉻合金及其在鹼性環境中之產氧反應行為研究

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楊政諭(Cheng-Yu Yang) 查詢紙本館藏

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材料科學與工程研究所

論文名稱

以微電鍍法製備鎳鈷鐵、鎳鈷鐵鉻合金及其在鹼性環境中之產氧反應行為研究
(Fabrication of Ni-Co-Fe and Ni-Co-Fe-Cr Alloy by Micro-anode Guided Electroplating and Behaviors of Oxygen Evolution Reaction in Alkaline Media)

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摘要(中)

目前電解水產氫為最具潛力的再生能源之一，但整體水分解效率受限於陽極產氧反應之動力學障礙。當今產氧效能較佳的材料為IrO2和RuO2，由於其價格昂貴且含量稀少，使得難以大規模生產。為解決上述問題，本研究以微陽極導引電鍍法(Micro-anode guided electroplating, MAGE)製備鎳鈷鐵三元、鎳鈷鐵鉻四元合金微柱作為陽極之催化電極，並探討其在鹼性環境(1.0 M KOH)中之產氧性能。本製程固定析鍍參數為電壓4.0 V與間距100 μm，並分別改變鍍浴中亞鐵離子濃度(0.03 M~0.06 M)及鉻離子濃度(0.0 mM~2.5 mM)進行析鍍。將所得之合金微柱以SEM觀察表面形貌、EDS分析化學組成、XRD分析晶體結構。接著進行線性掃描伏安法、循環伏安法、計時電位法與電化學阻抗頻譜之電化學測試，探討合金微柱之產氧效能。結果顯示鎳鈷鐵鉻合金比鎳鈷鐵合金有更佳產氧效能，其中具有最佳產氧效能的為Ni21Co33Fe34Cr12 (NCFR20)，塔弗斜率60.7 mV/dec為最低，產氧起始電位1.41 V為最低，循環伏安法最大電流密度為1525 mA/cm2，電荷轉移電阻僅51.09 Ω·cm2，且僅需1.50 V就可以維持電流密度在100 mA/cm2。本研究也證實添加鉻元素有利於電荷轉移使催化電極具更佳之產氧效能。

摘要(英)

At present, hydrogen production by water electrolysis is one of the most potential renewable energy sources, but the overall water splitting efficiency is limited by the kinetic barrier of oxygen evolution reaction at the anode. IrO2 and RuO2 have better oxygen evolution efficiency nowadays, which are difficult to produce on a large scale due to their high price and scarcity. In this study, Micro-anode guided electroplating (MAGE) was used to prepare nickel-cobalt-iron ternary and nickel-cobalt-iron-chromium quaternary alloy microcolumns as anode catalytic electrodes, and to discuss their performance for oxygen generation in alkaline media (1.0 M KOH). In this process, the bias voltage is fixed at 4.0 V and the gap is 100 μm, and the concentration of ferrous ions (0.03 M~0.06 M) and chromium ions (0.0 mM~2.5 mM) in the electroplating bath are respectively changed for fabrication. The surface morphology of the microcolumns was observed by SEM, the chemical composition was analyzed by EDS, and the crystal structure was analyzed by XRD. Subsequently, different alloy microcolumns were immersed in 1.0 M KOH for electrochemical tests such as linear sweep voltammetry, cyclic voltammetry, chronopotentiometry, and electrochemical impedance spectroscopy to observe oxygen evolution efficiency of alloy microcolumns. The results show that nickel-cobalt-iron-chromium alloy has better oxygen evolution efficiency than nickel-cobalt-iron alloy, and Ni21Co33Fe34Cr12 (NCFR20) has the best oxygen evolution performance, with the lowest Tafel slope of 60.7 mV/dec, and the lowest onset potential of oxygen evolution is 1.41 V, the maximum current density of cyclic voltammetry is 1525 mA/cm2, the charge transfer resistance is only 51.09 Ω·cm2, and only 1.50 V is needed to maintain the current density at 100 mA/cm2. This study also confirmed that the addition of chromium is beneficial for the charge transfer, so that the catalytic electrode has a better oxygen evolution efficiency.

關鍵字(中)

★ 微陽極導引電鍍法
★ 鎳鈷鐵合金
★ 鎳鈷鐵鉻合金
★ 產氧反應
★ 非貴金屬電催化劑

關鍵字(英)

★ Micro-anode guided electroplating
★ Nickel-cobalt-iron alloy
★ Nickel-cobalt-iron-chromium alloy
★ Oxygen evolution reaction (OER)
★ Non-precious metal electrocatalyst

論文目次

摘要 vi
Abstract vii
致謝 ix
目錄 x
表目錄 xv
圖目錄 xvii
第一章、前言 1
1-1 研究背景 1
1-2 水電解反應 2
1-3 水電解產氧之電極材料選擇 2
1-4 研究動機與目的 3
第二章、文獻回顧 5
2-1 電鍍原理 5
2-2 合金電鍍 5
2-3 局部電鍍製程之發展 7
2-4 微陽極導引電鍍法之發展 10
2-5 奈米壓痕測試基礎理論 12
2-6 產氧反應機制 14
2-7 3d過渡金屬元素用於產氧反應之相關研究 16
2-7-1 OER電催化劑種類 16
2-7-2 鎳鐵電催化劑 18
2-7-3 鎳鈷鐵電催化劑 18
2-7-4 鎳鐵鉻電催化劑 19
2-7-5 鈷鐵鉻電催化劑 20
2-7-6 鎳鈷鐵鉻電催化劑 20
2-8 X光光電子能譜儀(X-ray Photoelectron Spectroscopy, XPS) 21
第三章、實驗方法 23
3-1 實驗流程 23
3-2 鍍液配置 23
3-3 微陽極導引電鍍法實驗機台 24
3-4 陽極與陰極製備 24
3-5 合金微柱之表面形貌觀察與成分分析 25
3-6 合金微柱之縱剖面元素分析 25
3-7 合金微柱之晶體結構分析 26
3-8 機械性質測試 26
3-9 電化學產氧測試 27
3-9-1 線性掃描伏安法(Linear Sweep Voltammetry, LSV) 27
3-9-2 循環伏安法(Cyclic Voltammetry, CV) 28
3-9-3 計時電位法(Chronopotentiometry, CP) 28
3-9-4 電化學阻抗頻譜(Electrochemical Impedance Spectroscopy, EIS) 29
3-10 合金微柱之表面分析 29
3-11 合金微柱之水電解反應 30
3-11-1 法拉第效率與定電流氧氣蒐集 30
3-11-2 5×4之微柱陣列產氧 31
3-11-3 微柱陣列之水電解反應 31
第四章、結果 32
4-1 改變硫酸亞鐵濃度之鍍浴對鎳鈷鐵合金微柱之影響 32
4-1-1 表面形貌與柱徑 32
4-1-2 鎳鈷鐵合金微柱成分分析 32
4-1-3 鎳鈷鐵合金微柱之晶體結構 33
4-2 改變硫酸鉻濃度之鍍浴對鎳鈷鐵鉻合金微柱之影響 33
4-2-1 表面形貌與柱徑 34
4-2-2 鎳鈷鐵鉻合金微柱成分分析 34
4-2-3 鎳鈷鐵鉻合金微柱之縱剖面元素分布 35
4-2-4 鎳鈷鐵鉻合金微柱之晶體結構 35
4-2-5 機械性質分析 35
4-3 鎳鈷鐵、鎳鈷鐵鉻合金微柱在1.0 M KOH中之析氧反應 36
4-3-1 線性掃描伏安法 36
4-3-2 循環伏安法 38
4-3-3 計時電位法 39
4-3-4 電化學阻抗頻譜 40
4-4 最佳產氧效能合金微柱之表面分析 40
4-5 鎳鈷鐵、鎳鈷鐵鉻合金微柱產氧反應之定電流氧氣蒐集 42
第五章、討論 44
5-1 析鍍參數對於鎳鈷鐵、鎳鈷鐵鉻合金微柱表面形貌影響 44
5-2 析鍍參數對於鎳鈷鐵、鎳鈷鐵鉻合金微柱化學成分影響 45
5-3 鎳鈷鐵、鎳鈷鐵鉻合金微柱之晶體結構 45
5-4 改變硫酸鉻濃度對鎳鈷鐵鉻合金微柱之機械性質探討 46
5-5 析鍍參數對於鎳鈷鐵、鎳鈷鐵鉻合金微柱產氧性能影響 47
5-5-1 線性掃描伏安法 47
5-5-2 循環伏安法 48
5-5-3 計時電位法 48
5-5-4 電化學阻抗頻譜 49
5-6 析鍍參數對於產氧反應活化前後表面狀態影響 50
5-7 鎳鈷鐵、鎳鈷鐵鉻合金微柱之水電解反應 52
5-8 本研究與相關文獻電催化劑之產氧效能比較 53
第六章、結論與未來展望 55
參考資料 57

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指導教授

林景崎(Jing-Chie Lin)

審核日期

2023-7-26

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