近年來，三維奈米孔洞材料備受矚目，因其具有能夠客製化的內部結構，在眾多應用領域都被認為是具有潛力的新興材料。在本文中，將會劃分為兩個部分對鐵/鈷二元金屬有機骨架材料(Iron/cobalt metal-organic framework, Fe/Co-MOFs)進行深入的研究。
首先，第一部分是針對材料的合成參數進行成長機制的分析，再利用混合形狀控制劑的方式改變材料形貌。在這個章節中，本實驗除了通過水熱法成功合成出二元金屬有機骨架材料外，亦進行一系列合成參數控制實驗，包含金屬離子濃度對材料結晶度影響，不同形狀控制劑濃度與其尺寸大小的關係，還有溫度與時間對成核的影響與控制。並利用電子顯微鏡(Scanning electron microscope, SEM)，X射線衍射分析(X-ray diffractometer, XRD)進行材料鑑定，以確認所製備的Fe/Co-MOFs的結構形態。在參數的調整下，鐵/鈷二元金屬有機骨架材料不管是在晶體尺寸上，亦或是結晶度都有很大的差異。此外，本文也提供一種新式的結晶形貌控制策略，透過檸檬酸與硫乙醯胺的相互混合，材料形貌也因此改變。除添加劑(形貌控制劑)選擇外，合成步驟與添加劑混合之體積比例，也在晶體的再結晶過程中扮演很重要的角色。實驗中，將起初合成具有平均尺寸為1,080±235 nm之截頭立方體Fe/Co-MOFs進行混合添加劑實驗後，不僅可以使材料擁有多邊形的外觀，同時也給予晶體重新構築孔洞結構的可能性。
而第二部分則是將上述合成的材料(通過兩步驟之控制劑添加的方式所合成的)進行一系列的電化學分析實驗，探討其催化性能。由於經濟發展和人口增長促使能源需求的大幅增長、全球暖化日益嚴重，為了尋找清潔/可再生能源替代品，在過去的十年中，電化學水分解實驗成為許多科學家爭相研究的主題之一。然而，在實際應用面上目前尚未開發出具有低成本，同時穩定和環境友好的催化材料。為了達到上述目標，本實驗將所獲得之材料組裝碳布上，並將其應用於析氧反應實驗。由高解析電子顯微鏡(High resolution transmission electron microscopy, HRTEM)可以發現，經過混合控制劑的方法，Fe/Co-MOF的衍生物由原本的面心立方(Face-center cubic, FCC)轉變為六方最密堆積(Hexagonal close-packed, HCP)結構。而且比起原先的材料能夠擁有更多的晶面，這使得在催化上能有更多的活性位點的可能性。最終，可以發現六角平面狀的鐵/鈷二元金屬有機骨架材料(Fe/Co-MOF C7 T3)擁有最佳的電化學催化性能。不僅有最小的塔菲爾斜率(Tafel slope: 57.6 mV dec-1)、過電位為0.399 V (Overpotential for 10 mA cm-2)、啟動電位(On-set potential: 0.300 V)與電化學阻抗(Electrochemical impedance: 7.72 Ω)，同時，在不同的循環伏安法掃速下，也都有擁有最大的電容量(Capacitance: 4.28 mF cm-2)。本文所報導之Fe/Co-MOF與其衍生物，由於其優異的催化性能，因此可被視為低成本且環境友善優點之潛力催化材料。
在本文中，進行了一系列的參數調整試驗，不管是濃度、添加體積比、反應溫度、反應時間，抑或是pH值的變化，都會很直接的影響到最終材料的形貌、內部結構，或是應用端性能。在精確的控制下，可以針對應用領域的不同，設計出各種各樣的形貌，同時具備有不同功能性的材料，相信在各個領域中都會有不錯的效能。

In recent years, three-dimensional nano-porous materials have attracted wide attention. Because of their customizable internal structure, they are considered as potential emerging materials in various applications. This article is divided into two parts and conducted in-depth research on iron/cobalt metal-organic framework (Fe/Co-MOFs).
First of all, the first chapter introduced how to synthesize the Fe/Co-MOFs, and analyzed the synthesis parameters of the materials through thermodynamics and kinetics. Then, a novel co-solvent method is used to change the morphology of the material. In addition to successfully synthesizing binary metal organic framework materials by hydrothermal method, this work also conducted a series of parameter control experiments, including the influence of metal ions concentration on the crystallinity of the material, and particle size difference with different solvent concentration. There also investigated the influence of reaction time and temperature on nucleation. Furthermore, using scanning electron microscope (SEM), X-ray diffractometer (XRD) for material identification to confirm the structure of the Fe/Co-MOFs prepared. Under the adjustment of the parameters, the crystal size and crystallinity of Fe/Co-MOFs have changed greatly. Additionally, a series of co-solvent experiments have also been carried out in this research. By adding two different solvents (citric acid and thioacetamide), it can be found that the morphology has become completely different. Not only the choice of solvent, but also the volume ratio of the solvent mixture and the synthesis steps play an important role in the re-grow process. It can be found that the synthesized Fe/Co-MOF can be identified as a truncated cube with an average size of 1,080±235 nm which was subjected to a co-solvent experiment. Through modification, the material not only has a variety of morphologies, but also provides an opportunity for the crystal to rebuild the internal (pore) structure.
The second chapter is a series of electrochemical experiments on the above-mentioned materials (two-step synthesis products), and discusses their catalytic performance. With population growth and economic development, the problem of energy demand and global warming has increased significantly. In order to find available clean and renewable energy alternatives, electrochemical water splitting experiments have become one of the popular research topics in the past few decades. However, in practical applications, low-cost, stable and environmentally friendly catalytic materials have not yet been developed. In order to achieve the above-mentioned purpose, this experiment dropped the obtained material on a carbon cloth (CC) and applied it to the oxygen evolution reaction (OER). Through high-resolution transmission electron microscopy (HRTEM), it can be found that after the co-solvent reaction, the original face-center cubic (FCC) transforms into the hexagonal close-packed (HCP) structure. Moreover, Fe/Co-MOF derivatives have more crystal planes than the original one, so they can have more active sites in the catalytic process. In the final result, it can be found that the hexagonal planar MOF (Fe/Co-MOF C7 T3) has the best electrochemical catalytic performance. Not only exhibit the lowest Tafel slope (57.6 mV dec-1), overpotential of 0.399 V (under 10 mA cm-2), on-set potential (0.300 V) and electrochemical impedance (7.72 Ω), but the largest capacitance (4.28 mF cm-2) versus cyclic voltammetry (CV) scan rates. The Fe/Co-MOF and its derivatives reported in this study can be considered as one of the potential catalytic materials due to their excellent catalytic performance, with the advantages of low cost and environmental friendliness.
In this work, a series of parameter adjustment experiments were carried out. Regardless of the concentration, addition volume ratio, reaction time and temperature, or changes in pH, it will directly affect the morphology, internal structure, or performance of the final material. Under precise control, various shapes can be designed according to different application, and materials with different functions can be provided.

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