Facile Methods for Nanoscale PAN Carbonization｜國立清華大學博碩士論文庫

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研究生：	王梓仲 Wang, Tzu-Chung
論文名稱：	Facile Methods for Nanoscale PAN Carbonization 奈米尺度下聚丙烯腈碳化之研究
指導教授：	何榮銘 Ho, Rong-Ming
口試委員:
學位類別：	博士 Doctor
系所名稱：	工學院 - 化學工程學系 Department of Chemical Engineering
論文出版年：	2009
畢業學年度：	98
語文別：	英文
論文頁數：	125
中文關鍵詞：	聚丙烯腈、碳化、奈米碳材、高分子鏈排整、高分子團聯共聚物、溶劑退火法
外文關鍵詞：	polyacrylonitrile, carbonization, nanocarbon materials, polymer chain orientation, block copolymers, solvent annealing
相關次數：	點閱：2 下載：0
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A series of degradable block copolymers, poly(acrylonitrile)-b-poly(ε-caprolactone) (PAN-PCL), have been synthesized by sequential living polymerization in this study. Well-defined, microphase-separated PAN-PCL microdomains were efficiently achieved in bulk by using appropriate solvents for casting. The microphase-separated lamellar samples were then used as templates to produce mesoporous carbon at which large amounts of porous texture in carbonized PAN matrix were formed after the degradation of PCL due to randomly oriented lamellar texture (namely, interconnection of PCL microdomains). Mesoporous carbon materials might be prepared as demonstrated by transmission electron microscopy (TEM), field emission scanning electron microscopy (FESEM) and small-angle X-ray scattering. In contrast to the thermal stability of the carbonization of PAN homopolymers, notably, the carbonization procedure can be achieved in PAN-PCL BCPs system regardless of the stretching process (i.e., an essential process to improve the thermal stability of PAN during carbonization). We speculate that this unique feature for the carbonization of PAN-based copolymers might be attributed to the stretching chain conformations of PAN molecules under microphase-separated structures.
To further examine the methods for induction of chain stretching under nanoscale dimension, carbonization approach without chemical linkage (namely PAN homopolymers under confinement) were studied. PAN homopolymers were filled into inorganic hundred-nanometer-sized templates, anodized alumina oxides (AAOs), via direct capillary force. With a specific pore-filling process, a solvent-annealing process, graphite-like nanotubes can be fabricated from PAN pore-filling AAO templates. Thus, AAO templates acted as scaffolds supporting the formation of carbon nanotubes through carbonization, and were subsequently etched away, leaving behind the carbon nanotubes. To achieve appropriate molecular packing for carbonization, the anisotropic molecular orientation of PAN chains was induced by solvent annealing due to the capillary-filling process. Consequently, hundred-nanometer-sized carbon nanotubes formed after carbonation, as demonstrated by TEM and FESEM observations. Importantly, the carbon nanotubes with a graphite-like structure and high crystallinity can be fabricated, as demonstrated by selected area electron diffraction results. Notably, these carbon nanotubes cannot be fabricated using the conventional solution-wetting process. The formation of a core-shell cylinder texture was also demonstrated via multiple filling processes. Herein, facile methods for nanoscale PAN carbonization were demonstrated. In a microphase-separed system, the stretching chain conformation for carbonization could be achieved by the immiscibility of each block. For homopolymers, the stretching chain conformation could be formed by capillary force and preserved by controlling the evaporation dynamically. These approaches for nanoscale PAN carbonization can provide a convenient and promising way to fabricate carbon materials with various nanostructures, well-controlled sizes and high crystallinity.

Abstract    I
Acknowledgement    III
Contents    V
List of Tables    VIII
Scheme Caption    VIII
Figures Captions    IX
Chapter 1 Introduction    1
       1.1 Carbon Materials with Nanostructures    1
    1.1-1 The Carbon Element    2
    1.1-2 Synthesis of Carbon Nanotubes    5
    1.1-3 Properties and Applications of Carbon Nanotubes    8
    1.1-4 Carbon Fiber    10
    1.1-5 Mesoporous Carbon Materials    11
    1.2 Carbonization of PAN    13
       1.2-1 Stabilization Process    14
       1.2-2 The Importance of Fiber Stretching    16
       1.2-3 Carbonization Process    17
    1.3 PAN-based Block Copolymers    …………………...19
    1.3-1 Self-assembly of Block Copolymers    19
    1.3-2 Poly(acrylonitrile)-b-poly(n-butyl acrylate) (PAN-PBA)    23
    1.3-3 Poly(acrylonitrile)-b-poly(styrene) (PAN-PS)    25
    1.3-4 Poly(acrylonitrile)-b-poly(acrylic acid) (PAN-PAA)    27
    1.3-5 Poly(acrylonitrile)-b-poly(ethylene oxide) (PAN-PEO)    29
    1.4 Nanotubes from Template Wetting    31
          1.4-1 Template-based Synthesis    32
          1.4-2 Polymer Melt Wetting    34
    1.4-3 Solution Wetting    40
    1.4-4 Specific Behaviors under Confined Nanostructures    44
Chapter 2 Objectives    50
Chapter 3 Experimental    53
    3.1 Materials    53
    3.1-1 Synthesis of PAN-PCL block copolymers    53
    3.1-2 PAN homopolymer    55
    3.1-3 AAO templates    55
       3.2 Sample Preparation    56
    3.2-1 PAN-PCL bulk samples    56
    3.2-2 Carbon Nanotube Preparation from Pore-filling Template    56
    3.2-3 SiO2/Carbon Composites    57
    3.2-4 Ag/Carbon Composites    57
       3.3 Instruments    58
    3.3-1 Thermogravimetric Analysis (TGA)    58
    3.3-2 Small-angle X-ray Scattering (SAXS)    58
    3.3-3 Transmission Electron Microscopy (TEM)    59
    3.3-4 Field-Emission Scanning Electron Microscopy (FESEM)    60
Chapter 4 Results and Discussion    61
4.1 Carbonization of PAN in Self-assembled PAN-PCL Block Copolymers    61
          4.1-1 Microphase-separated Morphology of PAN-PCL    61
          4.1-2 Stabilization of PAN in PAN-PCL    65
    4.1-3 Degradation of PCL in PAN-PCL    69
    4.1-4 Carbonization of Mesoporous PAN    72
    4.1-5 Confinement effect on Carbonization    75
4.2 Carbonization of PAN in Solvent-annealed Nanotubes    .79
    4.2-1 Morphologies of AAO     79
          4.2-2 Carbon Nanotubes from Solution-wetting Process    82
          4.2-3 Carbon Nanotubes from Solvent-annealing Process    87
    4.2-4 Mechanism of Chain Orientation Induced by Solvent-annealing Process    92
4.3 Inorganic/Carbon Nanotubes Core-shell Cylinder Structure    101
    4.3-1 SiO2/Carbon Core-shell Cylinders via Sol-gel Process    101
          4.3-2 Ag/Carbon Core-shell Cylinders via Nanoparticles Synthesis    105
Chapter 5 Conclusions    108
Chapter 6 References    111
Publications    125

                                

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