以微電鍍法製備鎳-鋅合金與鎳-鋅/1T相二硫化鉬複合微電極並比較它們在1.0 M KOH之電解產氫性能

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林暐翔(Wei-Hsiang Lin) 查詢紙本館藏

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機械工程學系

論文名稱

以微電鍍法製備鎳-鋅合金與鎳-鋅/1T相二硫化鉬複合微電極並比較它們在1.0 M KOH之電解產氫性能
(Fabrication of Ni-Zn alloys and 1T-MoS2/Ni-Zn composite Microelectrodes by MAGE and comparison their hydrogen evolution performance in 1.0 M KOH)

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至系統瀏覽論文 (2026-7-24以後開放)

摘要(中)

本研究以微陽極導引電鍍法製備三維鎳鋅微柱電極，並藉由鋅在鹼性環境下之溶蝕效果藉此增加電極的電化學催化表面積；並利用複合電鍍製備1T相二硫化鉬鑲嵌於鎳鋅合金之中，利用二硫化鉬增加電催化邊緣活性位點以及優化能帶結構等優點，產製1T相二硫化鉬鎳鋅鍍浴之中進行複合電鍍，進而提高電極之產氫活性。
微陽極導引電鍍法中探討不同濃度氯化鎳所析鍍出之鎳鋅合金微柱其成分比例以及電化學產氫效率，並使用水熱合成法製備出金屬相的二硫化鉬，配製成0.16 g/L ~ 0.64 g/L添加至鎳鋅合金鍍液中，在鍍液中固定施加偏壓3.6 V 與間距60 µm進行複合電鍍以獲得最佳產氫效能之二硫化鉬@鎳鋅複合電極。
所製得之微柱由電子顯微鏡觀察表面形貌，以能量散射光譜分析化學組成及以X-ray 結晶繞射測定晶體結構。最終將不同濃度之1T相二硫化鉬鑲嵌於鎳鋅微柱浸泡在1.0 M KOH 溶液中，進行線性掃描伏安法、循環伏安法、有效電化學表面積、計時電位法、交流阻抗頻譜法等電化學測試，探討其產氫性能。上述結果顯示合金複合微柱在二硫化鉬20 at.%、鎳45 at.%、鋅35at.%的情況下其擁有最佳的產氫效率，具有最低之塔弗斜率(Tafel slope = 66 mV/dec)、過電位(η10 = -81 mV)和起始電位(Eonset = -0.66 V vs RHE)，其電荷轉移阻抗為3.28 Ω·cm2，其結果顯示析氫反應時所需能量。綜上結果顯示可證實二硫化鉬與鎳鋅合金共鍍可增加活性位點以及加速電荷轉移，使電催化電極具備更佳產氫效能。

摘要(英)

This study employs microanode guided electroplating to fabricate three-dimensional nickel-zinc microcolumn electrodes. The electrochemical catalytic surface area of the electrodes is increased through the dissolution effect of zinc in an alkaline environment. Additionally, composite electroplating is used to embed 1T phase molybdenum disulfide (MoS₂) into the nickel-zinc alloy. The MoS₂ enhances the electrocatalytic edge active sites and optimizes the energy band structure, thereby improving the hydrogen evolution activity of the electrode.

The study investigates the composition ratio and electrochemical hydrogen evolution efficiency of nickel-zinc alloy microcolumns deposited with different concentrations of nickel chloride. Metal-phase MoS₂ is synthesized using the hydrothermal method, and a specific concentration is added to the nickel-zinc alloy plating solution. Composite electroplating is performed under a fixed bias of 3.6 V and a spacing of 60 µm to achieve the optimal hydrogen evolution performance of the nickel-zinc/MoS₂ composite electrode.

The microcolumns′ surface morphology is observed using electron microscopy, the chemical composition is analyzed by energy-dispersive spectroscopy, and the crystal structure is determined by X-ray diffraction. Finally, microcolumns embedded with different concentrations of 1T phase MoS₂ are immersed in a 1.0 M KOH solution, and electrochemical tests, including linear sweep voltammetry, cyclic voltammetry, electrochemical surface area measurement, chronopotentiometry, and electrochemical impedance spectroscopy, are conducted to evaluate their hydrogen evolution performance. The results indicate that the alloy composite microcolumns with 20 at.% MoS₂, 45 at.% nickel, and 35 at.% zinc exhibit the best hydrogen evolution efficiency, with the lowest Tafel slope (66 mV/dec), overpotential (η10 = -81 mV), and onset potential (Eonset = -0.66 V vs RHE), and a charge transfer resistance of 3.28 Ω·cm². Overall, the findings confirm that co-depositing MoS₂ with nickel-zinc alloy increases active sites and accelerates charge transfer, enhancing the electrocatalytic electrode′s hydrogen evolution performance.

關鍵字(中)

★ 微陽極導引電鍍法
★ 複合電鍍
★ 鎳鋅合金
★ 二硫化鉬
★ 水熱合成法
★ 析氫反應

關鍵字(英)

★ MAGE
★ Composite electroplating
★ Nickel-Zinc alloys
★ Hydrothermal synthesis
★ Hydrogen evolution reaction(HER)
★ Molybdenum disulfide
★ Microcolumns array

論文目次

摘要 i
Abstract iii
致謝 v
表目錄 f
圖目錄 j
第一章、前言 1
1.1研究背景 1
1.1.1能源與工業革命 1
1.1.2第三次能源革命 2
1.2氫能源 2
1.2.1氫能經濟價值 2
1.2.2氫能生產概況 5
1.3研究動機 5
第二章、文獻回顧 8
2.1綠氫 8
2.2電解水產氫原理 9
2.2.1鹼性水電解產氫 9
2.2.2火山圖 10
2.3微陽極導引電鍍法之發展歷程 12
2.4電鍍 16
2.4.1合金電鍍 16
2.4.2 Ni-Zn異常共鍍 17
2.4.3複合電鍍 19
2.5過渡金屬硫化物 21
2.5.1過渡金屬硫化物 21
2.5.2過渡金屬硫化物之產氫應用 23
2.6二硫化鉬 25
2.6.1金屬相二硫化鉬合成方式 25
2.6.2合成方式(插層類) 25
2.6.3合成方式(成長類) 27
第三章、實驗方法 29
3.1實驗流程 29
3.2微陽極與陰極製備 30
3.3微陽極導引電鍍機台與實驗設備 31
3.4水熱合成法 32
3.5鍍液配置 35
3.6金微柱之表面形貌與成分以及晶體結構分析 37
3.6.1 SEM表面形貌觀測 37
3.6.2 EDS成分分析 37
3.6.3 XRD晶體結構分析 37
3.7奈米壓痕機械性質分析 37
3.8析氫效能之電化學測試 39
3.9線性掃描伏安法 41
3.9.1 過電位 41
3.9.2 塔弗斜率 42
3.10循環伏安法 43
3.11計時電位法 44
3.12電化學阻抗圖譜分析 44
3.13排水集氣法 46
3.14 4×4之陣列產氧 47
3.15拉曼光譜分析 48
3.16微柱之XPS表面元素及價態分析 51
第四章、結果與討論 53
4.1探討鍍浴中氯化鎳濃度變化對合金微柱之影響 53
4.1.1鎳鋅微柱之表面形貌 53
4.2.2鎳鋅微柱組成成分分析 57
4.2.3鎳鋅微柱之晶體結構分析 60
4.2二硫化鉬粉末分析 63
4.2.1 XRD晶體結構分析 63
4.2.2二硫化鉬之Raman光譜鑑定 64
4.2.3 SEM表面形貌分析 65
4.2.4二硫化鉬@鎳鋅鍍液之Zeta電位分析 68
4.2.5二硫化鉬@鎳鋅鍍液之二硫化鉬粒徑分析 70
4.3探討二硫化鉬濃度變化對複合微柱之影響 71
4.3.1二硫化鉬@鎳鋅微柱表面形貌 71
4.3.2二硫化鉬@鎳鋅微柱組成成分分析 73
4.3.3二硫化鉬@鎳鋅微柱之晶體結構分析 77
4.3.4二硫化鉬@鎳鋅微柱之顯微結構分析 78
4.3.5二硫化鉬@鎳鋅微柱之機械性質分析 80
4.4二硫化鉬@鎳鋅、鎳鋅微柱之電化學產氫分析 83
4.4.1線性掃描伏安法(鎳鋅微柱) 83
4.4.2線性掃描伏安法(二硫化鉬@鎳鋅微柱) 87
4.4.3循環伏安法(鎳鋅微柱) 91
4.4.4循環伏安法(二硫化鉬@鎳鋅微柱) 95
4.4.5電化學活性表面積 100
4.4.6計時電位法 105
4.4.7電化學阻抗圖譜 109
4.4.8本文獻與其他文獻之產氫效能比較 113
4.5最佳產氫效能微柱之表面分析 115
4.6二硫化鉬@鎳鋅微柱之定電流氫氣蒐集 122
4.7二硫化鉬@鎳鋅微柱之4×4陣列產氫性能 125
第五章、結論與未來展望 126
參考文獻 128

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指導教授

林景崎(Jing-Chie Lin)

審核日期

2024-7-30

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