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研究生:張嘉哲
研究生(外文):CHANG, CHIA-CHE
論文名稱:開發金屬及金屬化合物奈米材料於儲能及光/電催化之應用
論文名稱(外文):The Development of Metal and Metal Compound Nanomaterials for Energy Storage and Photo/Electrochemical Catalytic Application
指導教授:王迪彥
指導教授(外文):WANG, DI-YAN
口試委員:賴英煌張源杰包志文李紹先郭聰榮
口試委員(外文):LAI, YING-HUANGCHANG, YUAN-JAYPAO, CHIH-WENLI, SHAO-SIANKUO, TSUNG-RONG
口試日期:2023-07-20
學位類別:博士
校院名稱:東海大學
系所名稱:化學系
學門:自然科學學門
學類:化學學類
論文種類:學術論文
論文出版年:2023
畢業學年度:111
語文別:英文
論文頁數:118
中文關鍵詞:電池氮氣還原反應硝酸根還原反應
外文關鍵詞:BatteryNRRNtRR
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工業的發展帶給人們便利生活的同時,不僅大量的消耗環境的資源,例如:石油、稀有礦物…等,也造成了一些迫切需要面對的問題,例如:全球暖化、資源耗竭、糧食短缺…等。隨著環境不斷的惡化,這些都是不遠的將來必須解決的問題。在再生能源快速發展的優勢下,將能源有效的儲存,或是轉換成其他可用資源,成為了很重要的議題之一。另一方面,隨著全球人口的增長,對糧食的需求也相應增加。從生產的角度來看,肥料是提高單位面積生產量最有效的方法之一。氨是氮肥工業中最重要的起始原料,在現代農業中為了追求高產量氮肥是不可或缺的。而目前都是透過哈伯法進行製造。過程中由於高溫高壓必須要耗費相當多的能量並排放出大量的溫室氣體。因此,尋找合適的替代方案進行氨的製造是科學研究相當重要的項目之一。在這篇論文中,我的研究分為三個項目:鋅銀鋅空氣混合電池的開發、二硫化鐵應用於電催化氮氣還原反應、氧化銅奈米團簇修飾於二氧化鈦上進行光催化硝酸根還原反應。
首先,在論文中的第二個章節試圖開發一個具有高電容量及高電位的電池。鋅銀電池本身就具有一些優勢,其資源在地球上較為豐富,成本也隨之降低,鋅銀電池擁有高的電位差,及不錯的理論電容量。透過鋅銀電池及鋅空氣電池的結合,產生一個具有高電位、高電容量的混合電池。這個混合電池在放電過程中產生了兩個平台,分別為1.5伏特和1.1伏特,其中較高的平台是由於Ag2O還原為Ag,而較低的平台則是由於Ag輔助的氧還原反應。循環性能測試顯示,在經過1700個循環後,庫倫效率仍保持在85%以上。並使其在彎曲的情況下,仍可以正常地進行充放電之行為,而能有更多的應用。
在論文的第三章節試圖發展高活性的二硫化鐵奈米材料在一般大氣環境下進行電催化氮還原反應產氨。在-0.6 V 的電位下,二硫化鐵在氮氣飽和的0.25 M過氯酸鋰水溶液中,展現出14.14%的高法拉第效率及每分鐘0.096 微克的高產率。透過近紅外光的雷射產生光電效應,些微的增加其產率至每分鐘0.1微克及14.57%的法拉第效率。
最後,為了解決在水中由工業或是農業產生過多的硝酸根離子並轉換成實用的氨,以助於氮的循環。由水熱法合成的CuOx-TiO2 奈米粒子進行光催化硝酸根還原反應。藉由CuOx的奈米團簇修飾在TiO2上,在0.1 M KNO3表現出153.09 μg gcat-1 h-1 的產率。藉由臨場的X光吸收光譜,觀察催化劑在反應過程中產生的變化,試圖了解其光催化的機制。透過銅的輔助下,其展現比TiO2高三倍的產率。

The rapid development of industry has brought convenience to people's lives, but it has also consumed a significant amount of environmental resources such as oil and rare minerals. This has resulted in urgent problems that to be solved, such as global warming, and resource depletion. With the continuous deterioration of the environment, these are issues that must be resolved shortly. With the rapid development of renewable energy, efficient energy storage or conversion into other usable resources has become an important issue. On the other hand, with the growing global population, there is a corresponding increase in the demand for food. From the view of production, fertilizer is one of the most effective to increase productivity per unit area. Ammonia is a crucial starting material in the nitrogen fertilizer industry, and it is indispensable for achieving high yields in modern agriculture. Currently, ammonia production is mainly carried out through the Haber process, which requires high temperatures and pressures, consuming a significant amount of energy and releasing a large amount of greenhouse gases. Therefore, finding suitable alternative methods for ammonia production is also a significant research project. In this thesis, my research is divided into three projects: the development of zinc-silver/air hybrid battery, the electrocatalytic nitrogen reduction reaction with iron pyrite, and the photocatalytic nitrate reduction reaction with subnanoclusters copper oxide decorated on titanium dioxide.
Firstly, in the second chapter of the paper, an attempt was made to develop a battery with high capacity and high voltage. Zinc-silver batteries have some advantages. The resources required for these batteries are relatively abundant on Earth, and their cost has also decreased. Zinc-silver batteries have a high potential difference and a decent theoretical capacity. By combining zinc-silver batteries with zinc-air batteries, a hybrid battery with high voltage and high capacity is created. This hybrid battery generates two plateaus during discharge, at 1.5 V and 1.1 V, with the higher plateau attributed to the reduction of Ag2O to Ag and the lower one resulting from an Ag-assisted oxygen reduction reaction. Cyclability tests have shown that the Coulombic efficiency remains above 85% after 1700 cycles. Furthermore, the battery can still perform charging and discharging behavior even when bent, allowing for more applications.
In the third chapter of the paper, efforts were made to develop highly active iron disulfide (FeS2) nanomaterials for electrocatalytic nitrogen reduction reaction to produce ammonia under ambient atmospheric conditions. At a potential of -0.6 V, iron disulfide exhibited a high Faradaic efficiency of 14.14% and a high production rate of 0.096 μg min-1 in a nitrogen-saturated 0.25 M lithium hypochlorite solution. By generating photoelectrochemical effects using near-infrared laser, the production rate increased slightly to 0.1 μg min-1 with a Faradaic efficiency of 14.57%.
Finally, to address the excessive nitrate ions generated in water by industrial or agricultural activities and convert them into useful ammonia to aid nitrogen circulation, CuOx-TiO2 nanoparticles synthesized by the hydrothermal method were employed for photocatalytic nitrate reduction. The CuOx-TiO2 nanoparticles decorated on TiO2 exhibited a production rate of 153.09 μg gcat-1 h-1 in a 0.1 M KNO3 solution. The photocatalytic mechanism was explored by conducting in-situ X-ray absorption spectroscopy to observe the catalyst's changes during the reaction. With the assistance of copper, the catalyst demonstrated a threefold higher production rate compared to TiO2.

Acknowledgment I
Publication List II
摘要 V
Abstract VII
Contents IX
Chapter 1 Introduction 1
1.1 The Energy Storage System—Alkaline Zinc Battery 1
1.1.1 Alkaline zinc batteries 1
1.1.2 Zn-Ag batteries 2
1.1.3 Zn-air batteries 3
1.2 Catalytic transformations to ammonia 4
1.2.1 Electrocatalysis of ammonia from nitrogen 4
1.2.2 Photocatalysis of ammonia from nitrate 5
1.3 Reference 7
Chapter 2 Instrumentation and Software 9
2.1 Scanning Electron Microscopy (SEM) with Energy Dispersive X-ray Analysis 9
2.2 Transmission electron Microscopy 10
2.3 X-ray diffractometer 11
2.4 Raman spectroscopy 14
2.5 X-ray absorption 15
2.5.1 XANES 17
2.5.2 EXAFS 18
2.6 Ultraviolet-Visible Spectroscopy (UV-vis) 19
2.7 Linear sweep voltammetry 20
2.8 Chronoamperometry (IT) 21
2.9 Reference 23
Chapter 3 Flexible Hybrid Zn-Ag/air Battery with Long Cycle Life 24
3.1 Abstract 25
3.2 Introduction 26
3.3 Experimental Section 28
3.3.1 Materials 28
3.3.2 Pretreatment of stainless steel wire screen 28
3.3.3 Electrochemical deposition of Ag nanoparticles on the stainless steel wire screen 28
3.3.4 The electrochemical measurement of Zinc/Ag and air hybrid battery 29
3.3.5 Polymer solid electrolyte preparation 29
3.3.6 The assembly of Zinc Ag/air hybrid pouch battery 30
3.3.7 Characterizations of silver electrode 30
3.4 Result and Discussion 31
3.5 Conclusion 40
3.6 Reference 41
Chapter 4 Photoactive Earth-abundant Iron pyrite catalysts for Electrocatalytic Nitrogen Reduction Reaction 47
4.1 Abstract 48
4.2 Introduction 49
4.3 Experimental Section 53
4.3.1 Materials: 53
4.3.2 Acid treatment of carbon fiber paper (CFP) 53
4.3.3 The fabrication of FeS2 grown on carbon fiber paper. 53
4.3.4 Electrochemical measurement of the nitrogen reduction reaction 54
4.3.5 Determination of NH3 generation amount 54
4.3.6 Determination of Faraday Efficiency (FE). 55
4.3.7 Characterization 56
4.4 Result and Discussion 57
4.5 Conclusion 68
4.6 Reference 69
Chapter 5 Reaction Mechanism of Photocatalytic Nitrate Reduction with Reduced Copper Photoproduced from Subnanoclusters Copper(II) Oxide Decorated on Titanium Oxide 74
5.1 Abstract 74
5.2 Introduction 75
5.3 Experimental Section 77
5.3.1 Materials 77
5.3.2 Synthesis of Copper oxide subnanoclusters decorated on Titanium oxide (CuOx-TiO2) 77
5.3.3 Synthesis of different transition metal oxide nanoclusters decorated on Titanium oxide. 78
5.3.4 Photochemical efficiency of nitrate reduction reaction 78
5.3.5 Characterization of oxidized CuOx-TiO2 nanoparticle 78
5.3.6 Determination of NH3 generation amount from nitrate reduction 78
5.4 Result and Discussion 80
5.5 Conclusion 97
5.6 Reference 98
Chapter 6 Summary and Perspective 101
6.1 Summary 101
6.2 Prospective 102

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