為未來提供清潔氫氣所制定之鹼性水電解無機奈米結構催化劑

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研究生：	SAKTHIPRIYA BALU SAKTHIPRIYA BALU
論文名稱：	為未來提供清潔氫氣所制定之鹼性水電解無機奈米結構催化劑 Tailoring Inorganic Nanostructured Catalysts for Alkaline Water Electrolysis to Fuel the Future with Clean Hydrogen
指導教授：	黃崧任 Song-Jeng Huang
口試委員:	丘群 Raman Sankar 汪俊延王丞浩 Lena Yadgarov 林景崎李泉黃崧任
學位類別：	博士 Doctor
系所名稱：	工程學院 - 機械工程系 Department of Mechanical Engineering
論文出版年：	2023
畢業學年度：	112
語文別：	英文
論文頁數：	161
中文關鍵詞：	無機奈米結構催化劑、水電解槽、陽極端的產氧反應（OER）、陰極端的產氫反應（HER）、三金屬層狀雙氫氧化物、CoZnFe LDH 、原位摻雜、FeCo(MoO4)3 、混合奈米複合材料、rGO/Ni3Se2/NF
外文關鍵詞：	Inorganic nanostructured catalysts, water electrolyzers, oxygen evolution reaction (OER), hydrogen evolution reaction (HER), trimetallic layered double hydroxides, CoZnFe LDH, in-situ doping, FeCo(MoO4)3, hybrid nanocomposite, rGO/Ni3Se2/NF
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應對氣候變化需要採用清潔能源解決方案。氫氣因其高能量密度和零二氧化碳排放的特性而具有巨大潛力。然而，氫的廣泛應用取決於高效且經濟實惠的生產方法。水電解是一條前景廣闊的途徑，但其慢速的氧氣和氫氣進化反應（分別為 OER 和 HER）需要活性催化劑。
本研究聚焦於新型無機納米結構催化劑的設計和優化，以提升水的分裂效能。我們主要採用了三種策略來提高催化性能：
(i) 三金屬（CoZnFe）層狀雙氫氧化物納米片：我們合成了 Co1-xZnFex LDH 成分，以優化 OER 活性。透過精確的成分調整，我們成功獲得了一種 OER 催化劑，其過電位接近基準 RuO2，這歸功於活性位點密度的提高和電子特性的改善。(ii) 原位摻鈷的鉬酸鐵納米顆粒：摻鈷使顆粒尺寸減小，表面積增大，進而提高了催化活性，比未摻鈷的顆粒高出 1.5 倍。鈷離子在活性位點中也發揮了關鍵作用，促進了高效的電子轉移。(iii) rGO/Ni3Se2/NF 納米覆合材料：這種混合結構與導電泡沫鎳和邊缘修飾的石墨烯相結合，為 HER 和 OER 提供豐富的活性位點，使這兩種催化反應都表現出顯著的過電位。

先進的表徵技術揭示了這些催化劑卓越催化活性背後的結構和形態現象，包括 X 射線衍射、X 射線光電子能譜、場發射掃描電子顯微鏡、拉曼光譜儀、高分辨率過渡電子顯微鏡和電化學活性分析。這些結果提供了對內擴式高效催化劑的制備和表征的清晰而深刻描述，有助於從根本上理解HER和OER催化劑及其改進。我們的工作為實現經濟高效的水電解鋪平了道路，推動氫氣在未來可持續能源中扮演關鍵角色。

The fight against climate change demands clean energy solutions. Hydrogen, with its high energy density and zero carbon dioxide emissions, holds immense potential. However, its widespread adoption hinges on efficient and affordable production methods. Water electrolysis offers a promising path, but sluggish oxygen and hydrogen evolution reactions (OER and HER) require active catalysts.
This study explores the design and optimization of novel inorganic nanostructured catalysts for enhanced water splitting, focusing on three strategies to improve catalytic performance. Thus, trimetallic (CoZnFe) layered double hydroxides nanosheets (i): Co1-xZnFex LDH compositions were synthesized to optimize OER activity. Through precise composition tuning, an OER catalyst with low overpotential close to benchmark RuO2 was achieved, attributed to enhanced active site density and improved electronic properties. In-situ cobalt-doped ferric molybdate nanoparticles (ii): cobalt doping resulted in reduced particle size and increased surface area, thus boosting catalytic activity by 1.5 times, compared to undoped counterparts. Co ions also acted as major role in active sites and promoted efficient electron transfer. rGO/Ni3Se2/NF Nanocomposite (iii): this hybrid structure combines with conductive nickel foam and rGO provides abundant active sites for both HER and OER, achieving remarkable overpotentials for both the catalytic reactions.
Advanced characterization techniques revealed the structural and morphological phenomena underlying the exceptional catalytic activity of these catalysts including x-ray diffraction, x-ray photoelectron spectroscopy, field emission scanning electron microscopy, raman spectrometer, high resolution transition electron microscopy, and electrochemical activity analysis. The results that are displayed significantly contributed to the fundamental understanding of HER and OER catalysts and their improvement, by offering a clear and an insightful description of the preparation and characterization of affordable and effective catalysts. This work paves the way for cost-effective and efficient water electrolysis, propelling hydrogen towards a key role in the sustainable energy future.

ABSTRACT	I
摘要	III
ACKNOWLEDGEMENT	IV
AUTHOR’S DECLARATION	V
LIST OF PUBLICATIONS	VI
OTHER PUBLICATIONS	VII
LIST OF ACRONYMS	VIII
TABLE OF CONTENTS	IX
LIST OF FIGURES	XIV
LIST OF TABLES	XX
CHAPTER 1:	INTRODUCTION	1
1	Motivation: Environmental Concerns and Energy Crisis	1
1.1	Environmental Concerns	3
1.2	Energy Crisis	4
2	Clean Energy: Fueling the Future	6
3	Electrochemical Water Splitting	7
CHAPTER 2:	FUNDAMENTALS AND PRINCIPLES OF WATER SPLITTING	10
1	Fundamentals of Water Splitting	10
2	Principles of Electrocatalytic Water Splitting	12
3	Reaction mechanisms for electrocatalytic WS	14
3.1	Hydrogen Evolution Reaction	15
3.2	Oxygen Evolution Reaction	17
4	Kinetic Parameters of Electrocatalytic WS	19
4.1	Activation Energy	19
4.2	Polarized Potential	19
4.3	Tafel Plots/Slope Analysis	21
4.4	Cyclic Voltammetry	22
4.4.1	Double Layer Capacitance (Cdl)	23
4.4.2	Electrochemically Active Surface Area	24
4.5	Electrochemical Impedance Spectroscopy	24
4.5.1	iR drop	25
4.6	Chronometry Analysis	26
CHAPTER 3:	ELECTROCATALYSTS AND ITS EARLY INVESTIGATIONS	28
1	Selection Criteria for Electrocatalysts	28
2	Importance of Electrocatalysts	29
3	Design Strategies to Improve Catalysts Performances	30
4	Literature survey on electrocatalysts	32
4.1	Early Investigations on Layered Double Hydroxides	32
4.2	Early Investigations on Monoclinic Ferric Molybdates	35
4.3	Early Investigations on Nickel Selenide	36
5	Scope of the thesis	38
CHAPTER 4:	EXPERIMENTAL METHODS AND CHARACTERIZATIONS	42
1	Criteria for selecting material for the synthesis	42
1.1	Materials	42
2	Material synthesis	43
2.1	Trimetallic Layered Double Hydroxide (CoZnFe LDH) Nanosheets Synthesis:	44
2.2	In-situ Co-doped Ferric Molybdates Nanoparticles Synthesis:	44
2.3	rGO/Ni3Se2/NF Nanocomposite Synthesis	45
3	Methods of characterizations	47
3.1	Composition and Structural Assessment	47
3.1.1	X-ray diffraction	47
3.1.2	Field emission scanning electron microscopy, Energy-dispersive x-ray spectroscopy and Elemental mapping	48
3.1.3	Transmission electron microscopy	49
3.1.4	Raman spectroscopy	49
3.1.5	X-ray photoelectron spectroscopy	50
3.2	Electrochemical characterizations	51
3.2.1	Cell setup	51
3.2.2	Electrolyte Preparation	51
CHAPTER 5:	RESULTS AND DISCUSSIONS	54
1	Trimetallic (CoZnFe) Layered Double Hydroxide Nanosheets	54
1.1	Compositions and Structural Analysis of CoZnFe LDH	55
1.1.1	XRD analysis	55
1.1.2	TEM analysis	57
1.1.3	FESEM analysis	57
1.1.4	EDX analysis	58
1.1.5	XPS analysis	60
1.2	Electrocatalytic Activity of CoZnFe LDH	61
1.2.1	OER performance	61
1.3	Summary	70
2	In-situ Cobalt-doped Ferric Molybdate as a Water Oxidation Catalysts	72
2.1	Compositions and Structural Analysis of Fe2(MoO4)3	72
2.1.1	In-situ formation of Fe2(MoO4)3	72
2.2	Electrocatalytic performance of Fe2-xCox(MoO4)3	79
2.2.1	OER performance	79
2.3	Summary	82
3	Nickel Selenide-based Nanocomposite as Bi-functional Catalyst (rGO/Ni3Se2/NF)	83
3.1	Composition and Structural Analysis of rGO/Ni3Se2/NF	84
3.1.1	Crystal structure and XRD analysis	84
3.1.2	FESEM, EDX and elemental mapping analysis	85
3.1.3	XPS analysis	87
3.2	Electrocatalytic Activity of rGO/Ni3Se2/NF	88
3.2.1	OER performance	88
3.2.2	HER performance	91
3.2.3	Surface Analysis after Catalytic Performance	93
3.3	Summary	95
CHAPTER 6:	CONCLUSIONS AND FUTURE PERSPECTIVES	97
1	Conclusions	97
2	Future perspectives	100
APPENDICES	101
REFERENCES	115
                                

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