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研究生:鄭國光
研究生(外文):Kuo-Kuang Cheng
論文名稱:蕊鞘熔融紡絲製備碳奈米纖維及其化學活化之研究
論文名稱(外文):Carbon nanofibers and chemically activated carbon nanofibers by core/sheath melt-spinning technique
指導教授:許子建許子建引用關係許子建許子建引用關係許子建許子建引用關係
指導教授(外文):Tzu-Chien HsuTzu-Chien HsuTzu-Chien Hsu
學位類別:博士
校院名稱:國立中山大學
系所名稱:材料與光電科學學系研究所
學門:工程學門
學類:材料工程學類
論文種類:學術論文
論文出版年:2011
畢業學年度:99
語文別:英文
論文頁數:177
中文關鍵詞:化學活化活性碳奈米纖維碳奈米纖維蕊鞘熔融紡絲原子力顯微鏡
外文關鍵詞:carbon nanofiberscore/sheath melt-spinningatomic force microscopyactivated carbon nanofiberschemical activation
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本研究是以熔融紡絲技術製備碳奈米纖維(CNF)與活性碳奈米纖維(ACNF)。對於以無溶劑的聚丙烯/(酚醛-聚乙烯)聚合物經蕊鞘熔融紡絲技術製備碳奈米纖維的特別方法,有三個主要步驟:首先將聚丙烯(蕊部)與酚醛-聚乙烯(鞘部)共同熔融壓出紡絲形成蕊鞘纖維,其次將蕊鞘纖維穩定化得到碳纖維前驅物,最後將碳纖維前驅物於高溫下碳化形成碳奈米纖維。由掃描式電子顯微鏡與穿透式電子顯微鏡圖顯示碳奈米纖維的直徑約100-600 nm,纖維長度大於80μm,且酚醛樹脂形成碳奈米纖維的碳化率約達45 %,這些表面平滑的碳奈米纖維束呈現方向性且捲曲成纖維狀排列。由X射線繞射儀、能量散佈X射線、拉曼光譜與選區電子繞射顯示碳奈米纖維的結構具有石墨顆粒均勻地分佈在一個無定形碳材中的混合相無定形碳材料,成分含有碳元素90 %,含氧元素10 %。
以熔融紡絲技術製備碳奈米纖維為基礎,製備一系列活性碳奈米纖維並以掃描式電子顯微鏡、穿透式電子顯微鏡、X射線繞射儀、能量散佈X射線、拉曼光譜與原子力顯微鏡分析表面形態及微細結構也特別以原子力顯微鏡作定性與定量的表面形態分析。活性碳奈米纖維的結構也具有石墨顆粒均勻地分佈在一個無定形碳材中的混合相無定形碳材料,並含有碳元素73 %,含氧元素27 %。活性碳奈米纖維的總孔洞體積比碳奈米纖維還大,此是氫氧化鉀的化學活化效應使活性碳奈米纖維的微孔體積增加,而磷酸的化學活化效應使活性碳奈米纖維的中孔體積增加。提高氫氧化鉀的濃度可使活性碳奈米纖維的比表面積與微孔體積變大,也使平均孔洞直徑變小的趨勢。

In this study, we developed the manufacturing pathways of carbon nanofibers (CNF) and activated carbon nanofibers (ACNF) via the “melt-spinning” method. A novel route based on the solvent-free core/sheath melt-spinning of polypropylene/ (phenol formaldehyde-polyethylene) (PP/(PF-PE)) to prepare CNF. The approach consists of three main steps: co-extrusion of PP (core) and a polymer blend of PF and PE (sheath), followed by melt-spinning, to form the core/sheath fibers; stabilization of core/sheath fibers to form the carbon fiber precursors; and carbonization of carbon fiber precursors to form the final CNF. Both scanning electron microscopy and transmission electron microscopy images reveal long and winding CNF with diameter 100 - 600 nm and length greater than 80 μm. With a yield of ~ 45 % based on its raw material PF, the CNF exhibits regularly oriented bundles which curl up to become rolls of wavy long fibers with clean and smooth surface. Results from X-ray diffractometry, energy dispersive X-ray, Raman spectroscopy, and selected area electron diffraction patterns further reveal that the CNF exhibits a mixed phase of carbon with graphitic particles embedded homogeneously in an amorphous carbon matrix. The carbon atoms in CNF are evenly distributed in a matrix having a composition of 90 % carbon element and 10 % in oxygen element.
A series of ACNF have also been prepared based on the chemical activation on the thus-prepared CNF; their morphological and microstructure characteristics were analyzed by scanning electron microscopy, atomic force microscopy (AFM), Raman spectroscopy, and X-ray diffractometry, with particular emphasis on the qualitative and quantitative AFM analysis. The effect of activating agent, potassium hydroxide and phosphorous acid, is compared; factors affecting the surface morphology and microstructure of ACNF are analyzed. The ACNF also exhibits a mixed phase of carbon with graphitic particles embedded homogeneously in an amorphous carbon matrix. The resulting ACNF consists of 73 % C element and 27 % O element. The total pore volume of the all activated ACNF is larger than that of un-activated CNF. It can be inferred that chemical activation by KOH results in increased micropore volume in carbon nanofibers; while the micropores produced by the chemical activation of H3PO4 may further be activated and then enlarged to become the mesopores at the expense of micropore volume. For the concentration effect of KOH on ACNF, it can be inferred that high concentration KOH activation results in increased SBET and micropore volume in carbon nanofibers. The average pore diameter of ACNF gradually decreases as the KOH concentration increases.

論文審定書 i
Acknowledgement ii
摘要 iii
Abstract iv
Table of contents v
List of figures viii
List of tables xiii
List of schemes xiv
List of abbreviations xv

Chapter 1 Introduction
1.1 Carbon nanofibers……………………………… 1
1.2 Activated carbon nanofibers……………………8
1.3 Objectives of this study………………………...9

Chapter 2 Literature review - general survey…….13
2.1 Vapor-grown method…………………………14
2.1.1 Chemical vapor deposition………………..14
2.1.2 Arc-discharge………………………………18
2.1.3 Laser-ablation……………………………20
2.2 Polymer spinning……………………………..22
2.2.1 Polymer blends by core-shell microspheres..22
2.2.2 Electro-spinning…………………………….28
2.2.3 Core/sheath fibers and matrix-fibril fibers…30
2.3 Activation of carbon nanofibers…………………35
2.3.1 Chemical activation………………………….36
2.3.2 Physical activation…………………………...40

Chapter 3 Amorphous carbon nanofibers by phenol formaldehyde-based polymer blend
3.1 Previous work on carbon nanofibers……….....43
3.2 Materials and Methods………………..........46
3.2.1 Materials…………………………………….46
3.2.2 Experiments…………………………………....49
3.2.3 Characterizations……………………............53
3.3 Results and Discussion
3.3.1 Spinning properties of core/sheath fibers…55
3.3.2 Cross-section and morphology of fibers….59
3.3.3 Thermal properties of carbon fibers precursors ...72
3.3.4 Morphology of carbon nanofibers …………..78
3.3.5 Microstructure of carbon nanofibers ………..84
3.4 Summary………………………………………..94

Chapter 4 Activated amorphous carbon nanofibers by chemical activation
4.1 Previous work on activated carbon nanofibers…96
4.2 Materials and Methods………………………….99
4.2.1 Materials………………………………………..99
4.2.2 Experiments……….........................................99
4.2.3 Characterizations……………………...........104
4.3 Results and discussion………………………107
4.3.1 Morphological characterization (SEM, AFM and STM)……………..107
4.3.2 Microstructure Identification (XRD, SAED and Raman)…………….121
4.3.3 Surface area characterization……....126
4.3.4 Comparison on chemical activation methods…………..135
4.4 Summary…………………………..........137

Chapter 5 Concluding remarks
5.1 Conclusions .......................................................140
5.2 Recommendations for further works................144

References………………………………….....147
Vitae……………………………………….....160

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