含次亞磷酸鈉深共熔溶劑搭配脈衝電沉積製備鐵鈷鎳銅鋅高熵合金/氧化物電觸媒應用於產氫及氨氮廢水處理

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姓名

蕭丞閔(Chen-Min Hsiao) 查詢紙本館藏

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化學工程與材料工程學系

論文名稱

含次亞磷酸鈉深共熔溶劑搭配脈衝電沉積製備鐵鈷鎳銅鋅高熵合金/氧化物電觸媒應用於產氫及氨氮廢水處理
(Pulsed Electrodeposition of FeCoNiCuZn High-Entropy Alloys/Oxides Electrocatalyst in Deep Eutectic Solvents with Sodium Phosphinate for Hydrogen Production and Ammonia-Nitrogen Wastewater Treatment)

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摘要(中)

氫能因其具備零碳排放、高效能及可再生等優點，被視為未來清潔能源的重要支柱。然而，目前主流的水電解制氫技術仍高度依賴貴金屬催化劑，其昂貴成本限制了大規模商業化的推廣。因此，開發高效且低成本的非貴金屬催化材料成為當前研究的關鍵方向。本研究利用脈衝電沉積技術，將鐵、鈷、鎳、銅、鋅五元高熵合金及高熵氧化物沉積於碳氈上，並採用以氯化膽鹼和乙二醇構成的深共熔溶劑作為電沉積介質，輔以次亞磷酸鈉作為添加劑以進一步提升材料性能。
實驗設計分為四個主要部分。首先，對碳纖維氈基底進行高溫熱處理與酸處理，以增強其表面活性及金屬附著能力。其次，製備深共熔溶劑，並通過脈衝電沉積法進行金屬沉積，針對不同頻率與占空比的脈衝參數進行優化比較。隨後，利用多種表徵分析確定材料的組成與表面形貌。最後，將製備的複合材料應用於電解水產氫及氨氮廢水降解，評估其電化學性能。
P-wP 2展現出卓越的電化學性能，在所有樣品中具有最低的析氫過電位，於50和100 mA/cm2 的電流密度下分別達到179 mV和232 mV。此外其Tafel斜率為178 mV/dec，顯示出良好的催化活性。阻抗分析進一步證實了其優異特性，鍍層阻抗僅為0.529 Ω，電荷轉移阻抗亦相對較低，僅7.559 Ω，促進了電子轉移動力學。最後P-wP 2具備出色的耐腐蝕性，並在氨氮廢水產氫方面展現出卓越的性能，突顯其作為高效且耐用電觸煤的潛力。

摘要(英)

Hydrogen energy is known as a critical green energy source due to its no carbon emissions, high efficiency, and renewability. However, the large-scale commercialization of water electrolysis remains constrained by the high cost of noble metal catalysts. To handle this issue, this study developed a novel pulsed electrodeposition technique to fabricate FeCoNiCuZn high-entropy alloys and high-entropy oxides on a carbon felt substrate. The electrodeposition process utilized a deep eutectic solvent composed of choline chloride and ethylene glycol, supplemented with sodium phosphinate as an additive to enhance material performance.
The study involved substrate pretreatment, material synthesis using optimized pulsed parameters, comprehensive material characterization and electrochemical testing for hydrogen production and ammonia-nitrogen wastewater degradation. Results indicated that pulsed electrodeposition with sodium phosphinate significantly improved the uniformity and surface morphology of the materials. Among the synthesized composites, P-wP 2 exhibited the best overall performance.
P-wP 2 exhibited exceptional electrochemical performance, achieving the lowest overpotential (179 mV at 50 mA/cm2, 232 mV at 100 mA/cm2) and a favorable Tafel slope (178 mV/dec) for HER. It also demonstrated the smallest coating resistance (0.529 Ω) and low charge transfer resistance (7.559 Ω), enhancing electron transfer kinetics. Additionally, P-wP 2 showed excellent corrosion resistance and outstanding hydrogen production from ammonia-nitrogen wastewater, confirming its potential as an efficient and durable electrocatalyst.

關鍵字(中)

★ 高熵合金
★ 高熵氧化物
★ 脈衝電沉積
★ 深共熔
★ 產氫
★ 氨氮廢水處理

關鍵字(英)

★ High-Entropy Alloys
★ High-Entropy Oxides
★ Pulsed Electrodeposition
★ Deep Eutectic Solvents
★ Hydrogen Production
★ Ammonia-Nitrogen Wastewater Degradation

論文目次

摘要 I
Abstract II
致謝 III
Figure Contents IX
Table Contents XI
Chapter 1 Introduction 1
1.1 Energy Transformation 1
1.2 Introduction to Green Energy 2
1.3 Overview of Hydrogen Energy 3
1.4 Hydrogen Production Technologies 4
1.5 Overview of Water Electrolysis Catalysts and Fabrication Methods 5
1.6 Deep Eutectic Solvents 6
1.7 High-Entropy Alloys and Oxides 8
1.8 Pulsed Electrodeposition 9
1.9 Ammonia-Nitrogen Wastewater Treatment 10
1.10 Research Motivation 11
Chapter 2 Background 12
2.1 Water Electrolysis for Hydrogen Production 12
2.2 Conventional Hydrogen Evolution Catalysts 14
2.3 Applications of Deep Eutectic Solvents 16
2.4 Effects of Additives in Electrodeposition 17
2.5 Applications of High-Entropy Alloys and Oxides 18
2.6 Applications of Pulsed Electrodeposition 20
Chapter 3 Experiment 21
3.1 Experimental Framework 21
3.2 Experimental Procedures 25
3.2.1 Pretreatment of Carbon Felt Substrate 25
3.2.2 Preparation of Deep Eutectic Solvent 27
3.2.3 Fabrication of High-Entropy Alloy Composite Electrodes 27
3.2.4 Electrochemical Analysis of Electrode Materials 29
3.3 Material Characterization of Composite Electrodes 29
3.3.1 X-ray Diffraction, XRD 30
3.3.2 Field Emission Scanning Electron Microscope, FE-SEM 30
3.3.3 X-ray Photoelectron Spectroscopy, XPS 31
3.4 Electrochemical Analysis of Composite Electrodes 32
3.4.1 Linear Sweep Voltammetry, LSV 33
3.4.2 Tafel Kinetics 34
3.4.3 Electrochemical Impedance Spectroscopy, EIS 35
3.4.4 Double-Layer Capacitance, Cdl 35
3.4.5 Chronopotentiometry Test, CP 36
3.4.6 Corrosion Potential 37
3.4.7 Hydrogen Production Efficiency 38
3.4.8 Gas Chromatography-Mass Spectrometry 38
3.4.9 UV-Vis Spectrophotometer 39
Chapter 4 Results and Discussion 40
4.1 Pre-Treatment Analysis of Carbon Felt Substrate 40
4.2 Double-Layer Mechanism of Pulse Electrodeposition 41
4.3 Comparison Between Potentiostatic Electrodeposition with Sodium Hypophosphite Addition and Pulse Electrodeposition of High-Entropy Alloys in Deep Eutectic Solvent 43
4.3.1 SEM and EDS Analysis of Electrocatalyst Composites Materials 43
4.3.1 Linear Sweep Voltammetry: Analysis of Hydrogen and Oxygen Evolution Overpotential 47
4.3.2 Electrochemical Impedance: Kinetic Analysis of Composite Materials 52
4.3.3 Corrosion Potential: Corrosion Resistance Testing of Composite Materials 57
4.3.4 Interim Conclusion 58
4.4 Material Analysis of High-Entropy Alloy and High-Entropy Oxide Electrocatalyst Composites 59
4.4.1 XRD Analysis of Electrocatalyst Composites 59
4.4.2 SEM and EDS Analysis of Electrocatalyst Composites 62
4.4.3 XPS Analysis of Electrocatalyst Composites 65
4.5 Electrical Analysis of High-Entropy Alloy and High-Entropy Oxide Electrocatalyst Composites 70
4.5.1 Linear Sweep Voltammetry: Analysis of Hydrogen and Oxygen Evolution Overpotential 70
4.5.2 Tafel Kinetics: Kinetic Analysis of Composite Materials 75
4.5.3 Electrochemical Impedance: Kinetic Analysis of Composite Materials 77
4.5.4 Double-Layer Capacitance: Electrochemical Active Surface Area Analysis of Composite Materials 82
4.5.5 Corrosion Potential: Corrosion Resistance Testing of Composite Materials 84
4.5.6 Galvanostatic Testing: Long-Term Stability Analysis of Composite Materials 86
4.5.7 Faraday Efficiency: Analysis of Hydrogen and Oxygen Evolution Performance of Composite Materials 90
4.5.8 Gas Chromatography-Mass Spectrometry: Hydrogen Purity Analysis in Hydrogen Evolution Products 92
4.5.9 Ammonia-Nitrogen Wastewater Treatment Efficiency of Composite Materials 94
4.5.10 Hydrogen Production in Ammonia-Nitrogen Wastewater 97
Chapter 5 Conclusion and Prospect 100
5.1 Conclusion 100
5.1.1 Conclusion for Early Stage 100
5.1.2 Material Characterization of Pulse Electrodeposited High-Entropy Alloy Composites with Sodium Phosphinate Addition 100
5.1.3 Electrochemical Performance of Pulse Electrodeposited High-Entropy Alloy Composites with Sodium Phosphinate Addition 101
5.1.4 Performance in Hydrogen Production and Ammonia-Nitrogen Wastewater Degradation 103
5.2 Prospect 105
References 106
Appendix 1 113
Appendix 2 119

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指導教授

劉奕宏(Yi-Hung Liu)

審核日期

2025-1-21

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