鎳-鈷/二硫化鉬複合微電極之MAGE製備及其在1.0 M KOH中電解水產氫之陰極效能

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葉瀚翔(Han-Hsiang Yeh) 查詢紙本館藏

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機械工程學系

論文名稱

鎳-鈷/二硫化鉬複合微電極之MAGE製備及其在1.0 M KOH中電解水產氫之陰極效能
(Ni-Co/MoS2 Composite Microelectrodes Prepared by MAGE and Their Cathodic Efficiency of H2-production from Water Electrolysis 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)

本研究採用本實驗室研發之微陽極影像導引電鍍法(Micro-anode guided electroplating, MAGE)首先製備鎳-鈷合金微柱，用於電催化工作電極產製氫氣。以直徑250 m之白金絲作微陽極，銅線(直徑0.5 mm)作為陰極，兩極間維持80 m之間距，偏壓控制在4.0 V進行電鍍。在陰極上析鍍出純鎳(Ni)及一系列鎳-鈷合金(Ni80Co20 Ni70Co30 Ni61Co39 Ni55Co45 Ni53Co47)微柱。其次，於製備Ni55Co45鍍浴中加入含0.00, 0.10, 0.20, 0.30, 0.40 mM之1T-MoS2奈米粉末，進一步製備鎳-鈷/二硫化鉬複合微電極。所有鎳-鈷合金電極及鎳-鈷/二硫化鉬複合微柱，藉由SEM來觀察表面形貌、EDS分析元素組成以及XRD分析晶體結構，再將這些微柱作為工作電極，浸泡至1.0 M KOH中進行產氫效能之評估，測試方法包括線性掃描伏安法、循環伏安法、計時電位法和電化學阻抗頻譜等四種方法。
結果顯示: 自鎳-鈷合金鍍液中電鍍所得之微柱，隨鍍浴中[Co2+]由0增高至0.10 M時，其SEM表面形貌粗糙度增加，表面出現顆粒狀結構，經EDS分析，當合金中鈷含量超過40 at. %時，表面呈現錐狀物。以[Co2+]/[Ni2+] 濃度比= 0.08 M/1.25 M製備所得之Ni55Co45合金微柱之產氫效能最好；至於所得之Ni-Co/MoS2複合微柱，複合電極之SEM表面形貌則呈現花椰菜狀結節顆粒，顆粒均勻且介面清晰可辨，隨鍍浴中MoS2含量由0 (g/L)上升至0.4 (g/L)，所得複合微柱表面之花椰菜顆粒間隙逐漸縮小。添加0.4 (g/L)之1T-MoS2複合電鍍浴(代號NCM04)析鍍所得之微柱，經EDS分析，其化學組成(at. %) 含有45 % Ni、34%Co、8%Mo、14%S之產氫效能最優。比較產氫效能，Ni-Co合金系列微柱中以Ni55Co45產氫效能最好: 產氫的交換電流密度最大(0.616 mA/cm2)，塔弗斜率最低(106 mV/dec)，在電流密度10 mA/cm2下之瞬時氫過電位最低(有159 mV)，在進行1週次的循環伏安分析中呈現出了最低的起始電位(-0.273 V)以及最大的陰極峰值電流密度(-448 mA/cm2)。
代號NCM04復合微柱產氫的交換電流密度最大(1.843 mA/cm2)，塔弗斜率最低(68 mV/dec)，在電流密度10 mA/cm2下之瞬時氫過電位最低(有89 mV)，在進行1週次的循環伏安分析中呈現出了最低的起始電位(-0.102 V)以及最大的陰極峰值電流密度(-866 mA/cm2)。經調整極化掃描速率來計算電雙層電容(Cdl)，並計算電極的電化學活性表面積(ECSA)，顯示複合電極NCM04具有最大的電化學活性高表面積: 783 cm2具備最高之電化學活性。本論文證實添加二硫化鉬至鎳-鈷合金鍍浴，電鍍所得之Ni-Co/MoS2複合電極，能有效改善鹼性電解水產氫之陰極。

摘要(英)

This study employs the micro-anode guided electroplating (MAGE) method developed in our laboratory to first prepare nickel-cobalt alloy micro-columns for use in electrocatalytic working electrodes for hydrogen production. A platinum wire with a diameter of 250 μm is used as the micro-anode, and a copper wire (diameter 0.5 mm) as the cathode, maintaining a distance of 80 μm between the electrodes, with the plating voltage controlled at 4.0 V. Pure nickel (Ni) and a series of nickel-cobalt alloys (Ni80Co20, Ni70Co30, Ni61Co39, Ni55Co45, Ni53Co47) micro-columns are deposited on the cathode. Next, 1T-MoS2 nanopowder is added to the Ni55Co45 plating bath in concentrations of 0.00, 0.10, 0.20, 0.30, and 0.40 mM to further prepare nickel-cobalt/molybdenum disulfide composite micro-electrodes. All nickel-cobalt alloy electrodes and nickel-cobalt/molybdenum disulfide composite micro-columns are observed using SEM to study surface morphology, analyzed for elemental composition using EDS, and examined for crystal structure using XRD. These micro-columns are then used as working electrodes, immersed in 1.0 M KOH to evaluate hydrogen production performance. The testing methods include linear sweep voltammetry, cyclic voltammetry, chronoamperometry, and electrochemical impedance spectroscopy.
Results show that the micro-columns electroplated from the nickel-cobalt alloy bath, with increasing [Co2+] from 0 to 0.10 M, exhibit increased surface roughness and granular structures as observed by SEM. EDS analysis indicates that when the cobalt content in the alloy exceeds 40 at. %, the surface presents conical structures. The Ni55Co45 alloy micro-column prepared with a [Co2+]/[Ni2+] concentration ratio of 0.08 M/1.25 M demonstrates the best hydrogen production performance. As for the Ni-Co/MoS2 composite micro-columns, the SEM surface morphology shows uniform and clearly identifiable cauliflower-like granular nodules. With the increase of MoS2 concentration in the plating bath from 0 to 0.4 mM, the gaps between the cauliflower-like particles on the composite micro-column surface gradually decrease. The micro-columns deposited from a composite electroplating bath with 0.4 g/L 1T-MoS2 (designated as NCM04) exhibit the best hydrogen production performance, with EDS analysis showing a chemical composition (at. %) of 45% Ni, 34% Co, 8% Mo, and 14% S.
Comparing hydrogen production performance, the Ni55Co45 micro-columns in the Ni-Co alloy series exhibit the best performance: highest exchange current density (0.616 mA/cm²), lowest Tafel slope (106 mV/dec), lowest instantaneous hydrogen overpotential at a current density of 10 mA/cm² (159 mV), and the lowest onset potential (-0.273 V) with the highest cathodic peak current density (-448 mA/cm²) during one-week cyclic voltammetry analysis. The composite micro-columns NCM04 show the highest exchange current density (1.843 mA/cm²), lowest Tafel slope (68 mV/dec), lowest instantaneous hydrogen overpotential at a current density of 10 mA/cm² (89 mV), and the lowest onset potential (-0.102 V) with the highest cathodic peak current density (-866 mA/cm²) during one-week cyclic voltammetry analysis. By adjusting the polarization scan rate to calculate the double-layer capacitance (Cdl) and the electrochemical active surface area (ECSA), the composite electrode NCM04 demonstrates the largest electrochemical active surface area of 783 cm², indicating the highest electrochemical activity.

關鍵字(中)

★ 微陽極導引電鍍
★ 鎳-鈷合金
★ 二硫化鉬
★ 析氫反應

關鍵字(英)

★ Micro-anode Guided Electroplating
★ nickel-cobalt alloy
★ molybdenum disulfide
★ hydrogen evolution reaction

論文目次

中文摘要 i
ABSTRACT iii
致謝 v
目錄 vi
表目錄 x
圖目錄 xiii
第一章、前言 1
1-1 全球能源發展趨勢 1
1-2 產氫方法之介紹 1
1-3 電解水產氫使用之陰極材料 2
1-4 研究動機與目的 3
第二章、文獻回顧 4
2-1 電鍍原理 4
2-2 局部電鍍製程發展 5
2-3 奈微米材料實驗室微電鍍製程發展 10
2-4 合金共鍍 11
2-4-1 Ni-Co異常共鍍 13
2-5 複合電鍍 14
2-6 鹼性溶液中的產氫機制 15
2-7 析氫火山圖 16
2-8 鎳基合金電極於鹼性溶液中之析氫反應研究 17
2-8-1 鎳-鈷合金 18
2-9 過渡金屬硫族化物電極之析氫反應研究 19
2-10 1T相二硫化鉬 20
2-11 奈米壓痕測試理論 23
第三章、研究方法與實驗設備 25
3-1 實驗流程 25
3-2 微陽極導引電鍍機台與實驗設備 27
3-3 水熱合成釜之儀器介紹 28
3-4 鍍浴選擇與配置 29
3-5 陰陽極製備 31
3-6 二硫化鉬粉末之製備 31
3-7 二硫化鉬粉末1T相之確認 33
3-8 合金微柱之表面形貌觀察 34
3-9 合金微柱之元素組成成份分析 34
3-10 合金微柱之晶體結構分析 34
3-11 合金微柱之顯微結構分析 34
3-12 合金微柱之奈米壓痕硬度測試 35
3-13 合金微柱在1.0 M KOH溶液中之電化學產氫測試 35
3-13-1 線性掃描伏安法(Linear Sweep Voltammetry, LSV) 37
3-13-2 循環伏安法(Cyclic voltammetry, CV) 39
3-13-3 計時電位法(Chronopotentiometry, CP) 40
3-13-4 電化學阻抗頻譜(Electrochemical impedance spectroscopy, EIS) 41
3-13-5 排水集氣法 42
第四章、結果與討論 45
4-1 改變鎳-鈷鍍浴中硫酸鈷濃度之特性分析 45
4-1-1 鎳-鈷合金微柱之元素組成分析 45
4-1-2 鎳-鈷合金微柱之表面形貌 47
4-1-3 鎳-鈷合金微柱之晶體結構分析 49
4-1-4 鎳-鈷合金微柱之顯微結構分析 51
4-2 鎳-鈷合金微柱於1 M KOH溶液中之電化學析氫反應 53
4-2-1 鎳-鈷合金微柱於析氫反應下之線性掃描伏安法 53
4-2-2 鎳-鈷合金微柱於析氫反應下之循環伏安法 57
4-2-3 鎳-鈷合金微柱於析氫反應下之計時電位法 64
4-2-4 鎳-鈷合金微柱於析氫反應下之電化學阻抗圖譜 67
4-3 鎳-鈷合金微柱之產氫效能 69
4-4 二硫化鉬相之判別 72
4-5 1T相二硫化鉬粉末之表面形貌 73
4-6 1T相二硫化鉬粉末之粒徑分析 74
4-7 改變鎳-鈷/二硫化鉬複合電鍍浴中二硫化鉬含量之特性分析 75
4-7-1 鎳-鈷/二硫化鉬複合電極之Zeta potential 75
4-7-2 鎳-鈷/二硫化鉬複合電極之元素組成分析 76
4-7-3 鎳-鈷/二硫化鉬複合電極之表面形貌 78
4-7-4 鎳-鈷/二硫化鉬複合電極之晶體結構分析 80
4-7-5 鎳-鈷/二硫化鉬複合電極之顯微結構分析 81
4-8 鎳-鈷/二硫化鉬複合電極於1.0 M KOH溶液中之電化學析氫反應 82
4-8-1 鎳-鈷/二硫化鉬複合電極於析氫反應下之線性掃描伏安法 82
4-8-2 鎳-鈷/二硫化鉬複合電極於析氫反應下之循環伏安法 86
4-8-3 鎳-鈷/二硫化鉬複合電極之電化學活性表面積 89
4-8-4 鎳-鈷/二硫化鉬複合電極於析氫反應下之計時電位法 94
4-8-5 鎳-鈷/二硫化鉬複合電極於析氫反應下之電化學阻抗圖譜 96
4-9 鎳-鈷、鎳-鈷/二硫化鉬複合電極之元素分佈 98
4-10 鎳-鈷、鎳-鈷/二硫化鉬複合電極之機械性質 100
4-11 與其他文獻之產氫效能比較 102
4-12 鎳-鈷/二硫化鉬複合電極之氫氣蒐集 103
4-13 4×4鎳-鈷/二硫化鉬複合電極陣列之氫氣蒐集 105
第五章、結論與未來展望 107
參考資料 109

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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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