臺灣博碩士論文加值系統

本論文的研究目的為利用熱裂解高分子聚乙二醇與觸媒之混合物製備不同型態之一維奈米碳簇材料(平板型奈米碳纖維、孔洞型奈米碳纖維及竹結狀奈米碳纖維)及探討在能源上之應用。主要分為兩大部分:第一部分(第二章至第四章)主要為對所開發出之不同型態之一維奈米碳簇材料進行材料檢測及探討不同反應條件(溫度、觸媒)對生成一維奈米碳簇材料之影響；第二部份(第五章及第六章)主要為研究不同型態之ㄧ維奈米碳簇材料在能源上(氫氣儲存、超級電容器)之應用。
在一維奈米碳簇材料之製備方面，分別以鎳系及鐵系觸媒研究探討其對生成一維奈米碳簇材料之影響。在第二章及第四章中，主要以聚乙二醇及氯化鎳觸媒混合之前驅物進行熱裂解反應，由實驗結果發現，可以利用不同反應溫度合成不同型態之一維奈米碳簇材料(600oC迳孔洞型、750 oC迳平板型)。當反應溫度為750 oC，可以合成高純度、高石墨化且直徑小且均一(10-20 nm)之平板型奈米碳纖維；當反應溫度為600 oC，可以合成具有石墨化及中孔洞型態之孔洞型奈米碳纖維。不同型態之ㄧ維奈米線材經SEM、TEM及SAED分析檢測，可以發現因溫度不同，觸媒形狀及結晶性在不同溫度下有明顯的差異，由不規則且雙晶結構(600 oC)轉變為規則且單晶結構(750 oC)。因不同型態及結構之觸媒，對一維線材之型態及結構有重大的影響，因此我們可以在不同溫度合成不同型態之ㄧ維奈米線材；在第三章中，主要是以不同之鐵系觸媒與聚乙二醇混合之前驅物進行熱裂解反應，由實驗結果發現，以硫酸鐵為觸媒、反應溫度在750 oC及硫酸鐵與PEG混和物重量比為1:1000，可以合成短及彎曲之竹結狀奈米碳纖維，當觸媒與高分子比例過大或過小均不能生成一維奈米碳材。
在氫氣儲存的測試方面(第五章)，主要是以平板型奈米碳纖維當作吸附材料，利用體積法檢測其儲氫量，由檢測結果得知，在壓力為4.83 MPa及溫度298 K，平板型奈米碳纖維的儲氫量為3.3 wt%，且經由XRD檢測分析，石墨層層間距在儲存氫氣前後有擴大及縮小之現象。
在超級電容器的應用方面(第六章)，主要是以孔洞型奈米碳纖維基一般商業化奈米碳管當作電極材料進行有系統之材料結構與電化學行為檢測，由實驗結果得知，具有石墨化、中孔洞、較高表面積及氧官能基(C-OH, C=O及COOH)含量較多的孔洞型奈米碳纖維(Cs=98.4Fg−1, onset frequency=1.31 kHz)比一般商業奈米碳管(Cs =17.8Fg−1, onset frequency =1.01 kHz)擁有較佳的電容行為。

In this thesis, we prepared high purity and uniform one-dimensional carbon nanomaterials (platelet graphite nanofibers (PGNFs), carbon nanofibers (CNFs), and porous CNFs) from thermal decomposition of a mixture containing of polyethylene glycol (PEG) and catalyst. These carbon nanomaterials can be formed and tailored through suitable control of the synthetic conditions (temperature/catalyst). We also studied the structure of these materials and explored their applications. Fundamentals of one-dimensional carbon nanomaterials were reviewed in chapter 1. The structure of these carbon nanomatrials and their energy applications were systematically studied and reportrd in chapters 2–5, respectively.
In chapter 2, PGNFs with high purity, high degree of graphitization, and a uniform diameter of 10-20 nm were synthesized from thermal decomposition of a mixture containing of PEG and nickel chloride (NiCl2) at 750 oC under nitrogen atmosphere. Thermogravimetry-differential scanning calorimetry-mass spectrometry was employed to study the thermal decomposition phenomena of the mixture (PEG/NiCl2) before the thermal process. The analysis clarified the synthesis growth mechanism of PGNFs from the mixture.
In chapter 3, CNFs exhibiting bamboo-like, hollow fibril morphology were prepared from the mixture of PEG and iron-based compounds such as Fe2(SO4)3．nH2O, Fe(NO3)．9H2O, or FeO(OH) by thermal process. CNFs can be formed with different PEG/catalyst ratios (100/1–1000/1) by weight at 750 oC. Catalyst effect was discussed for the formation of bamboo-like CNFs. The diameter of CNFs was about 30–50 nm while the length was a few micrometers.
In chapter 4, porous CNFs exhibited with mesopore, open edge, and graphitic structure were synthesized by thermal decomposition of PEG with the presence of nickel catalyst at 600 oC under nitrogen atmosphere. High purity of porous CNFs with a fiber diameter of 40–60 nm and a few micrometers in length can be synthesized on the wafer uniformly. Unlike the activation process of carbon fibers or template method to create pores, the mesopores of porous CNFs can be formed simultaneously while the fibers grew. Characterizations of porous CNFs found that, due to insufficient growth energy at 600 oC, the disordered graphene layers were generated from polycrystalline Ni catalysts and stacking of disorder graphene layers thereby created 4–¬6 nm mesopores with open edges. Porous CNFs with open edges, which are different from activated CNFs, were suggested to be a good medium for mass transport while graphene layers may serve as a good electrical conductive medium for the applications of electrode, catalyst supports, and adsorption.
In chapter 5, the hydrogen storage capacity of the PGNFs was measured using the volumetric method with the pressure up to 4.83 MPa at 298 K. The results show that the PGNFs possess a 3.3 wt% hydrogen storage capacity. X-ray diffraction analysis reveals that the d-spacing of graphene layers were expanded during hydrogen adsorption process and return back to the initial value after desorption of hydrogen.
In chapter 6, the textural and electrochemical properties of MCNFs were systematically compared with those of commercially available multi-walled carbon nanotubes (MWCNTs). The high ratio of mesopores and large amount of open edges of MCNFs with a higher specific surface area, very different from that of MWCNTs, are favorable for the penetration of electrolytes meanwhile the graphene layers of MCNFs serve as a good electronic conductive medium of electrons. The electrochemical properties of MCNFs and MWCNTs were characterized for the application of supercapacitors using cyclic voltammetry, galvanostatic charge–discharge method, and electrochemical impedance spectroscopic analyses. The MCNFs shows better capacitive performances (CS = 98.4 F g讣1 at 25 mV s讣1 and an onset frequency of behaving as a capacitor at 1.31 kHz) than that of MWCNTs (CS = 17.8 F g讣1 and an onset frequency at 1.01 kHz). This work demonstrates the promising capacitive properties of MCNFs for the application of electrochemical supercapacitors.

Contents
Abstract I
中文摘要 IV
Contents VI
List of Tables X
List of Figures XI
Chapter 1 Introduction 1
1.1 Brief history of one-dimensional carbon nanomaterials 1
1.2 Catalytic growth 4
1.3 Classification of carbon nanofilaments 13
1.4 Synthesis methods 18
1.5 Characteristics of CNFs 21
1.5.1 Adsorption characteristics 22
1.5.2 Density 26
1.5.3 Mechanical properties of CNFs 27
1.5.4. Electrical properties 28
1.6 Applications 31
1.6.1 Catalyst supports 31
1.6.2 Reinforcement 32
1.6.3 Lithium ion secondary batteries 34
1.6.4 Supercapacitor 36
1.6.5 Hydorgen storage 36
1.7 Objective and outlines 40
Chapter 2 In Situ Synthesis of Platelet Graphite Nanofibers from Thermal Decomposition of Poly(ethylene glycol) 41
2.1 Introduction of Graphite Nanofibers 41
2.2 Experimental 43
2.3 Results and Discussion 44
2.3.1 Thermal analysis of the Mixture (PEG-catalyst). 44
2.3.2 PGNFs Analysis. 47
2.4 Conclusion 54
Chapter 3 Synthesis of Carbon Nanofibers from a Liquid Solution Containing both Catalyst and Poly(ethylene glycol) 55
3.1 Introduction of CNTs/CNFs from polymer materials 55
3.2 Experimental 57
3.3 Results and discussion 58
3.3.1 Thermal analysis of PEG and the mixtures 58
3.3.2 The growth of CNFs 60
3.4 Conclusion 66
Chapter 4 Preparation and Characterization of Porous Carbon Nanofibers from Thermal Decomposition of Poly(ethylene glycol) 67
4.1 Introduction of Porous Carbon Materials 67
4.2 Experimental 69
4.3 Results and discussion 70
4.4. Conclusion 80
Chapter 5 Hydrogen Storage in Platelet Graphite Nanofibers 81
5.1 Introduction of Hydrogen Storage in Graphite Nanofibers 81
5.2. Experimental 84
5.3 Results and Discussion 86
5.3.1 Structural characteristics of the PGNFs 86
5.3.2 Hydrogen storage 88
5.3.3 XRD analysis 89
5.4. Conclusion 91
Chapter 6 Textural and Electrochemical Characterization of Porous Carbon Nanofibers as Electrodes for Supercapacitors 92
6.1 Introduction of One-dimensional Carbon Nanomaterials as Electrodes for Supercapacitors 92
6.2. Experimental 95
6.2.1 Preparation of porous CNFs 95
6.2.2 Electrochemical measurements 96
6.3 Results and discussion 98
6.3.1 Characterization of one dimension carbon nanomaterials 98
6.3.2 Electrochemical characterization 106
6.4 Conclusion 114
Chapter 7 Concluding Remarks 115
Reference 118
Appecdix 138
Publication list 146

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