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研究生： 阮韶銘
Siu Ming Yuen
論文名稱： 多壁碳奈米管/高分子奈米複合材料之製備與性質研究
Study on the Preparation and Characterization of Mutilwalled Carbon Nanotube/ Polymer Nanocomposites
指導教授： 馬振基
Chen-Chi M. Ma
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： 2008
畢業學年度： 96
語文別： 中文
論文頁數： 401
中文關鍵詞： 碳奈米管 、表面改質 、奈米複合材料 、聚醯亞胺 、環氧樹脂 、聚甲基丙烯酸甲脂 、XPS 、拉曼光譜, 、SEM 、TEM 、機械性質 、導電性 、熱性質
外文關鍵詞： Multiwalled carbon nanotube, surface modification, nanocomposites, polyimide, epoxy, PMMA, XPS, Raman spectroscopy, SEM, TEM, mechanical properties, electrical resistivity, thermal conductivity
相關次數： 點閱：3  下載：0 
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    • 本論文旨在探討多壁碳奈米管(Multiwalled Carbon Nanotube, MWCNT)之表面改質及不同改質方法對多壁碳奈米管/高分子奈米複合材料性質之影響。針對不同的高分子基材，多壁碳奈米管以不同的方式進行表面改質。將改質之多壁碳奈米管分別加入聚醯亞胺，環氧樹脂及聚甲基丙烯酸甲酯中，製備成不同之多壁碳奈米管/聚醯亞胺，環氧樹脂及聚甲基丙烯酸甲酯等奈米複合材料，並探討其分子運動性，形態學，導電性，機械性質及熱性質。本研究共分為四部份。
    本研究第一部份為多壁碳奈米管分別以硫酸/硝酸之混酸，自由基(free radical)，如vinyltriethoxysilane (VTES)改質。而酸改質之多壁碳奈米管分別接枝胺，可溶性聚醯亞胺由(4,4’-(Hexafluoroisopropylidene) diphthalic anhydride(6FDA)與4,4’-Diphenylmethane diisocyanate(MDI)反應而合成) 及矽醇(3-isocyanato-propyltriethoxysilane, IPTES and (3-aminopropyl) triethoxy-silane, APTES)。改質之多壁碳奈米管以FT-IR, Raman spectrum and X-ray photoelectron spectroscopy (XPS)鑑定其結構。未改質及各種已改質之多壁碳奈米管分別與聚醯亞胺混摻，製備成多壁碳奈米管/聚醯亞胺奈米複合材料。
    SEM及TEM電子顯微鏡照片顯示未改質多壁碳奈米管在聚醯亞胺基材中呈聚集狀態，而酸改質，胺接枝及可溶性聚醯亞胺接枝多壁碳奈米管在聚醯亞胺基材中分散均勻，矽醇改質多壁碳奈米管在聚醯亞胺基材中互相連接而聚醯亞胺分子則互穿於多壁碳奈米管網狀結構中。聚醯亞胺之表面及體積電阻因為多壁碳奈米管的加入而下降，其機械性質則因為多壁碳奈米管的加入而上升。
    酸改質多壁碳奈米管接枝上矽醇(3-isocyanato-propyltriethoxysilane(IPTES)及(3-aminopropyl)triethoxy- silane (APTES)及未改質多壁碳奈米管以自由基反應接枝上vinyltriethoxysilane(VTES)。矽醇改質之多壁碳奈米管加入至聚醯亞胺酸中，在300℃閉環時，聚醯亞胺酸閉環而成聚醯亞胺，同時矽醇改質多壁碳奈米管表面之矽醇則縮合，使多壁碳奈米管互相連接而成為多壁碳奈米管網狀結構，聚醯亞胺分子則互穿於多壁碳奈米管網狀結構中。其體積電阻因矽醇改質多壁碳奈米管的加入而明顯下降，在相同之多壁碳奈米管含量下，其下降幅度比加入酸改質多壁碳奈米管更為明顯。
    第二部份為在多壁碳奈米管/環氧樹脂奈米複合材料，未改質多壁碳奈米管及矽醇改質多壁碳奈米管(IPTES)與環氧樹脂摻混，從SEM電子顯微鏡觀察，未改質之多壁碳奈米管在環氧樹脂基材中聚集。環氧樹脂之表面電阻及其體積電阻因多壁碳奈米管的加入而下降。本研究以3-isocyanato-propyltriethoxysilane (IPTES)接枝上DGEBA-type之環氧樹脂及酸改質多壁碳管，將兩者混合，加入交聯劑製備而成矽醇改質多壁碳奈米管(IPTES-MWCNT)/環氧樹脂奈米複合材料。SEM及TEM電子顯微鏡顯示矽醇改質多壁碳奈米管在環氧樹脂中分散均勻，固態13C NMR顯示加入1.0wt%矽醇改質多壁碳奈米管之環氧樹脂之分子運動性下降。以DSC測試之環氧樹脂之玻璃轉移溫度從192.6℃(接枝上IPTES之環氧樹脂)上升至212.5℃ (1.0wt% IPTES-MWCNT)。以DMA測試之環氧樹脂在50℃下之儲存模數(storage modulus)因矽醇改質多壁碳奈米管的加入而上升。環氧樹脂加入1.0wt%矽醇改質多壁碳奈米管，其拉伸及抗折強度分別增加41.65%及145.7%；環氧樹脂加入0.8wt%矽醇改質多壁碳奈米管，其楊氏係數及抗折模數分別增加52.8%及31.1%。
    第三部份為多壁碳奈米管以溶膠-凝膠法包覆上一層二氧化鈦，並以矽醇(3-(aminopropyl)triethoxysilane ,APTES)改質二氧化鈦包覆之多壁碳奈米管(AT-MWCNT)並以X-ray photoelectron spectroscopy鑑定，將AT-MWCNT加入DGEBA-type之環氧樹脂中，硬化而成二氧化鈦包覆多壁碳奈米管/環氧樹脂奈米複合材料。其中經過APTES改質之二氧化鈦包覆多壁碳奈米管表面含有胺官能基，能與環氧樹脂反應。二氧化鈦包覆多壁碳奈米管對環氧樹脂之補強效果比未改質多壁碳奈米管優異。在二氧化鈦包覆之多壁碳奈米管系統中，提升二氧化鈦的含量，以X-ray photoelectron spectroscopy (XPS)及X-ray diffraction (XRD) 鑑定二氧化鈦包覆多壁碳奈米管，而環氧樹脂則選用矽醇(APTES)作為交聯劑。TEM電子顯微鏡顯示二氧化鈦已包覆在多壁碳奈米管表面，而加入環氧樹脂後仍未脫落，而且二氧化鈦包覆多壁碳奈米管在環氧樹脂基材中分散均勻。環氧樹脂之機械性質因二氧化鈦包覆多壁碳奈米管的加入而明顯提升。
    第四部份為多壁碳奈米管/聚甲基丙烯酸甲酯奈米複合材料，酸改質之多壁碳奈米管接枝上矽醇(3-isocyanato- propyltriethoxysilane, IPTES)。而可交聯之聚甲基丙烯酸甲酯則以甲基丙烯酸甲酯及Vinyltriethoxysilane (VTES)進行共聚合(PMMA-VTES)。矽醇接枝之多壁碳奈米管加入PMMA-VTES基材中而成矽醇接枝多壁碳奈米管/PMMA-VTES奈米複合材料。矽醇之縮合度因矽醇接枝多壁碳奈米管的加入而下降，而矽醇接枝多壁碳奈米管在PMMA-VTES基材中則分散均勻。PMMA-VTES之導電及導熱性都因多壁碳奈米管的加入而上升，而其熱穩定性亦因多壁碳奈米管的加入而明顯增加。

    In this research,multi-walled carbon nanotube(MWCNT) was modified with different conditions. The modified MWCNT was analyzed by FT-IR, Raman spectrum and X-ray photoelectron spectroscopy (XPS). The unmodified and modified MWCNT were added to polyimide, epoxy and PMMA to prepare MWCNT/polyimide, MWCNT/epoxy and MWCNT/PMMA nanocomposites. This dissertation contains four parts.
    The first part was the preparation and characterization of MWCNT/polyimide composites. Unmodified, acid-modified, amine-modified and soluble polyimide grafted multiwalled carbon nanotube (MWCNT) were added separately to the polyamic acid and heated to 300℃ to form polyimide/carbon nanotube composite. SEM and TEM microphotographs show that acid-modified MWCNT, amine-modified and soluble polyimide grafted MWCNT dispersed uniformly in the polyimide matrix. Silane modified MWCNTs formed interpenetrate network in polyimide network. Effect of the MWCNTs on the surface and volume electrical resistivities of the MWCNT/PI composites has been investigated. Mechanical properties of the nanocomposites were enhanced significantly by modified MWCNTs. Acid modified multiwalled carbon nanotubes (MWCNTs) were grafted with 3-isocyanato-propyltriethoxysilane(IPTES) and (3-aminopropyl) triethoxysilane (APTES); Unmodified multiwalled carbon nanotubes (MWCNTs) were grafted with vinyltriethoxysilane(VTES). Silane grafted MWCNTs were then mixed with the polyamic acid(BDTA/ODA) and heated to 300℃ to form a carbon nanotube/polyimide composite. During the imidization processes, the silanes on the MWCNT surface reacted with each other. TEM microphotographs showed that the silane grafted MWCNTs were connected. The composite material possesses an interpenetrating network in which polyimide molecules were interpenetrated into the MWCNT network. The electrical resistivity of silane grafted MWCNT/polyimide decreased very significantly compared to those only containing acid treated MWCNTs for the same loading with MWCNTs.
    The second part was the preparation of MWCNT/epoxy composites, multiwalled Carbon nanotubes (MWCNT)/Epoxy Composites have been prepared. The characteristics and morphological properties were studied. SEM microphotographs showed that MWCNTs were aggregated in the epoxy resin. Epoxy resin and acid modified multiwalled carbon nanotube(MWCNT) were treated with 3-isocyanato- propyltriethoxy-silane (IPTES). SEM and TEM microphotographs of the MWCNT/epoxy composites have been investigated. The molecular motion of silane modified MWCNT/Epoxy composites were studied using high-resolution solid-state 13C NMR. Results show that 1.0wt% silane modified MWCNT/Epoxy exhibits less molecular motion than that of the lower silane modified MWCNT content. Dynamic mechanical analysis (DMA) data of the MWCNT/Epoxy composites showed the storage modulus (at 50℃) and Tgs of the IPTES modified Epoxy increased with IPTES-MWCNT content. Tensile strength and Young’s Modulus of cured silane modified MWCNT(1.0wt%)/Epoxy composites increased significantly comparing to the neat epoxy.
    In the third part, a unique titanium oxide (TiO2) coated multiwalled carbon nanotube(MWCNT)/Epoxy has been prepared. Multiwalled carbon nanotubes were coated with a layer of TiO2 and then modified with 3-(aminopropyl)triethoxysilane (APTES). The TiO2 coated MWCNT and APTES modified TiO2 coated MWCNT(AT-MWCNT) were analyzed by X-ray photoelectron spectroscopy(XPS). The AT-MWCNT was added to the Diglycidyl ether of bisphenol A type epoxy to prepare silane grafted TiO2 coated MWCNT/epoxy composites. The amine functional groups on AT-MWCNT surface reacted with epoxy. Consequently, the adhesion between MWCNT and epoxy was improved. Mechanical properties of the AT-MWCNT/epoxy composites increased dramatically. The TiO2 coated MWCNTs/epoxy system was cured with silane. Silane may react with TiO2 surface and improves the adhesion between the MWCNT and epoxy matrix. X-ray photoelectron spectroscopy and X-ray diffraction (XRD) were utilized to analyze the TiO2 coated MWCNTs. TEM microphotographs showed the effect of titanium (IV) n-butoxide on the morphology of the TiO2 coated MWCNT. The dispersion of TiO2 coated MWCNT in the epoxy matrix is better than that of unmodified MWCNT. Mechanical properties of the MWCNT/epoxy composites were improved significantly by the TiO2 coated MWCNTs.
    The fourth part was the preparation of MWCNT/PMMA composites. Mutiwalled carbon nanotubes (MWCNT) were modified using 3-isocyanato- propyltriethoxysilane (IPTES). Crosslinkable PMMA was prepared from MMA monomer and Vinyltriethoxysilane (VTES) (PMMA-VTES).The IPTES-modified MWCNT (Si-MWCNT) was mixed with the PMMA-VTES copolymer and crosslinked with catalyst to form Si-MWCNT/PMMA-VTES composites. The degree of condensation of tri-distribution structure of the Si-MWCNT/PMMA-VTES composites decreases as the Si-MWCNT content increases. The morphology of the Si-MWCNT/PMMA-VTES composites was analyzed by SEM and TEM. The MWCNTs were well dispersed in the PMMA-VTES matrix. Surface and volume electrical resistivity decreased as the MWCNT content increased. The thermal conductivity of the PMMA-VTES composites increased by 87.5% when 0.99wt% Si-MWCNT content was added to neat PMMA-VTES. The thermal stability of the PMMA-VTES in nitrogen and air increased significantly even when a small quantity (0.5wt%) of Si-MWCNT was added.

    中文摘要 Abstract 謝誌 目錄 Scheme目錄 圖目錄 表目錄 第一章 緒論 1-1 前言 1-2 本研究之目的與研究方向 1-3 參考文獻 第二章 基礎理論 2-1 碳奈米管之特性 2-1.1 碳奈米管之基本性質 2-1.2 碳奈米管之種類及個別性質 2-2 碳奈米管的製備方法 2-2-1 火焰生成法 2-2-2 雷射蒸發╱剝離法 2-2-3 電弧放電法 2-2-4 化學氣相沉積法 2-3 碳奈米管的檢測與分析方法 2-3-1 結構分析 2-3-2 吸附性分析 2-4 碳奈米管之純化技術 2-4-1 以氧化法純化多壁碳奈米管 2-4-2 以嵌入觸媒後進行氧化 2-4-3 以離心、過濾及色層析法純化多壁型碳奈米管 2-4-4 單壁碳奈米管之純化 2-5 碳奈米管之表面改質及“溶液”配製 2-5-1 碳奈米管改質 2-5-2 配製碳奈米管有機溶液 2-6 碳奈米管管中化學原理及特性 2-6-1 碳奈米管開口中空管的吸附行為 2-6-2 碳奈米管內的填充 2-6-3“奈米試管” 2-7 碳奈米管的應用 2-8 高分子-碳奈米管複合材料 2-9 參考文獻 第三章 文獻回顧 3-1碳奈米管/環氧樹脂奈米複合材料 3-2 碳奈米管/聚醯亞胺奈米複合材料 3-3 碳奈米管/聚甲基丙烯酸甲酯奈米複合材料 3-4 聚奈米管/PP奈米複合材料 3-5 碳奈米管/PA奈米複合材料 3-6 碳奈米管/PE奈米複合材料 3-7 碳奈米管/PET及PBT奈米複合材料 3-8 其他碳奈米管/高分子奈米複合材料 3-9 參考文獻 第四章 實驗部份 4-1實驗流程 4-2 實驗材料 4-3 實驗儀器設備 4-4 實驗方法 4-4-1多壁碳奈米管表面改質 4-4-2多壁碳奈米管/高分子奈米複合材料之製備 4-5碳奈米管/高分子奈米複合材料之測試 4-5-1多壁碳奈米管╱聚醯亞胺奈米複合材料之結構鑑定及性質 測試 4-5-2 多壁碳奈米管╱聚甲基丙烯酸甲酯奈米複合材料之結構鑑 定及性質測試 4-5-3多壁碳奈米管/環氧樹脂奈米複合材料之性質檢測 第五章 酸改質、胺接技及可溶性聚醯亞胺接枝多壁碳奈米管/聚醯亞胺複合材料 5-1前言 5-2實驗部份 5-2-1 實驗材料 5-2-2 酸改質多壁碳奈米管 5-2-3 胺接枝多壁碳奈米管 5-2-4 可溶性聚醯亞胺接枝多壁碳奈米管 5-2-5 ODA/BTDA聚醯亞胺的前驅物poly(amic acid)之合成 5-2-6多壁碳奈米管╱聚醯亞胺奈米複合材料之製備 5-2-7改質多壁碳奈米管及多壁碳奈米管╱聚醯亞胺奈米複合材料 之結構鑑定及性質測試 5-2-8 1H Nuclear Magnetic Resonance(1H NMR) 5-2-9 掃瞄式電子顯微鏡(scanning electron microscope) 5-2-10 穿透式電子顯微鏡(Transmission electron microscope) 5-2-11 拉伸性質(Tensile properties) 5-2-12 電氣性質(Electrical properties) 5-2-13 玻璃轉移溫度(Glass transition temperature (Tg)) 5-3-1傅立葉轉換紅外線光譜 (Fourier-transform infrared spectroscopy) 5-3-2 可溶性聚醯亞胺接枝多壁碳奈米管之1H NMR光譜 5-3-3 MWCNT/polyimide奈米複合材料之電子顯微鏡(scanning electron microscope, SEM and Transmission electron microscopy, TEM) 5-3-4 多壁碳奈米管/聚醯亞胺奈米複合材料之導電性(Electrical conductivity) 5-3-5 MWCNT/polyimide奈米複合材料之拉伸性質(Tensile properties) 5-3-6 MWCNT/polyimide奈米複合材料之玻璃轉移溫度(Glass transition temperatures,Tgs) 5-4 結論 5-5 參考文獻 第六章 矽醇改質多壁碳奈米管/聚醯亞胺奈米複合材料 6-1 前言 6-2實驗部份 6-2-1 實驗材料 6-2-2 酸改質多壁碳奈米管 6-2-3 以3-Isocyanatopropyltriethoxysilane (IPTES)接枝上酸改質多壁碳奈米管 6-2-4 以(3-Aminopropyl)triethoxysilane (APTES)接枝上酸改質多壁碳奈米管 6-2-5 以Vinyltriethoxysilane (VTES) 接枝上未改質多壁碳奈米管 6-2-6 ODA/BTDA聚醯亞胺的前驅物poly(amic acid)之合成 6-2-7多壁碳奈米管╱聚醯亞胺奈米複合材料之製備 6-2-8改質多壁碳奈米管及多壁碳奈米管╱聚醯亞胺奈米複合材料 之結構鑑定及性質測試 6-2-9 掃瞄式電子顯微鏡(scanning electron microscope) 6-2-10 穿透式電子顯微鏡(Transmission electron microscope) 6-2-11 拉伸性質(Tensile properties) 6-2-12電氣性質(Electrical properties) 6-3 結果與討論 6-3-1傅立葉轉換紅外線光譜 (Fourier-transform infrared spectroscopy) 6-3-2 VTES改質多壁碳奈米管之拉曼光譜(Raman spectrum) 6-3-3 矽醇改質碳奈米管之X-ray photoelectron spectroscopy (XPS) 6-3-4 矽醇改質碳奈米管/聚醯亞胺奈米複合材料之29Si固態核磁 共振分析(29Si solid state nuclear magnetic resonance (NMR)) 6-3-6 矽醇改質碳奈米管/聚醯亞胺奈米複合材料之導電性質 6-3-7 矽醇改質碳奈米管/聚醯亞胺奈米複合材料之機械性質 6-4結論 第七章 多壁碳奈米管/環氧樹脂複合材料 7-1 前言 7-2 實驗部分 7-2-1 實驗藥品 7-2-2 多壁碳奈米管/環氧樹脂奈米複合材料之製備 7-2-3 多壁碳奈米管/環氧樹脂奈米複合材料之性質檢測 7-5 結果與討論 7-5-1多壁碳奈米管/環氧樹脂奈米複合材料之形態觀察 7-5-2 多壁碳奈米管/環氧樹脂奈米複合材料之熱性質分析 7-5-3多壁碳奈米管/環氧樹脂奈米複合材料之電性分析 7-5結論 7-6 參考文獻 第八章 矽醇改質碳奈米管/環氧樹脂奈米複合材料 8-1前言 8-2 實驗部份 8-2-1 實驗材料 8-2-2 多壁碳奈米管之表面改質 8-2-3 多壁碳奈米管/環氧樹脂奈米複合材料之製備 8-2-4 多壁碳奈米管/環氧樹脂奈米複合材料之性質測試 8-3 結果與討論 8-3-1傅立葉轉換紅外線光譜 (Fourier transform infrared spectroscopy, FT-IR) 8-3-2 X-ray photoelectron spectroscopy (XPS) 8-3-3 多壁碳奈米管/環氧樹脂奈米複合材料之29Si 及13C 固態 NMR分析 8-3-4 多壁碳奈米管/環氧樹脂奈米複合材料之13C NMR CP/MAS 及分子運動性 8-3-5 矽醇改質多壁碳奈米管/環氧樹脂奈米複合材料之玻 璃轉移 溫度 8-3-6 矽醇改質多壁碳奈米管/環氧樹脂奈米複合材料之形態分析 8-3-7 矽醇改質多壁碳奈米管/環氧樹脂奈米複合材料機械性質 8-3-8矽醇改質多壁碳奈米管/環氧樹脂奈米複合材料導電性質 8-4 結論 8-5 參考文獻 第九章 二氧化鈦包覆多壁碳奈米管/環氧樹脂奈米複合材料 9-1前言 9-2實驗部份 實驗流程 9-2-1實驗材料 9-2-2 二氧化鈦包覆多壁碳奈米管 9-2-3 二氧化鈦包覆碳奈米管/環氧樹脂奈米複合材料之製備 9-2-4 二氧化鈦包覆碳奈米管/環氧樹脂奈米複合材料之結構鑑定及性質測試 9-3 結果與討論 9-3-1 X-ray photoelectron spectroscopy (XPS) 9-3-2 二氧化鈦包覆碳奈米管/環氧樹脂奈米複合材料之形態分析 9-3-3 二氧化鈦包覆碳奈米管/環氧樹脂奈米複合材料之機械性質 9-3-4 二氧化鈦包覆碳奈米管/環氧樹脂奈米複合材料之體積電阻 9-4結論 9-5參考文獻 第十章 二氧化鈦包覆多壁碳奈米管/聚倍半矽氧烷 /環氧樹脂奈米複合材料 10-1 前言 10-2-1實驗材料 10-2-2 二氧化鈦包覆多壁碳奈米管 10-2-3 二氧化鈦包覆碳奈米管/聚倍半矽氧烷/環氧樹脂奈米複合材料之製備 10-2-4 二氧化鈦包覆碳奈米管/聚倍半矽氧烷/環氧樹脂奈米複合材料之結構鑑定及性質測試 10-3 結果與討論 10-3-1 X-ray diffraction (XRD) 10-3-2 X-ray photoelectron spectroscopy (XPS) 10-3-3 形態學分析 10-3-3 二氧化鈦包覆碳奈米管/聚倍半矽氧烷/環氧樹脂奈米複合 材料之機械性質 10-3-4 二氧化鈦包覆碳奈米管/聚倍半矽氧烷/環氧樹脂奈米複合 材料之體積電阻 10-4 結論 10-5 參考文獻 第十一章 矽醇改質碳奈米管/聚甲基丙烯酸甲酯奈米複合材料 11-1 前言 11-2實驗部份 11-2-1實驗材料 11-2-2實驗步驟 11-3結果與討論 11-3-1傅立葉轉換紅外線光譜 (Fourier transform infrared spectroscopy, FT-IR) 11-3-2多壁碳奈米管/PMMA-VTES奈米複合材料29Si固態核磁共振分析(29Si solid state nuclear magnetic resonance, NMR))結果 11-3-3多壁碳奈米管/PMMA-VTES奈米複合材料形態分析 11-3-4多壁碳奈米管/PMMA-VTES奈米複合材料之表面及體積電阻 11-3-5多壁碳奈米管/PMMA-VTES奈米複合材料之熱傳導係數 11-3-6多壁碳奈米管/PMMA-VTES奈米複合材料之熱穩定性分析 11-4 結論 11-5參考文獻 第十二章 總結論 12-1結論 本論文之研究成果已發表之相關著作 國外期□論文 國內期□論文 國際研討會論文 國內研討會論文 本研究成果已申請專利 個人簡歷 Scheme 5 1 Acid modification of MWCNT Scheme 5 2 Amine modification (grafting) of MWCNT (R=CH2CH2NH2) Scheme 5 3 Polyimide grafted on the acid modified MWCNs Scheme 5 4 Preparation of polyimide Scheme 6 1 Perparation of silane grafted carbon nanotubes/polyimide composites Scheme 6 2 IPTES grafted of MWCNT Scheme 6 3 Attachment of APTES with acid modified MWCNT Scheme 6 4 Modification of MWCNT by VTES Scheme 8 1 Modification of MWCNT by IPTES Scheme 8 2 Modification of DGEBA-type Epoxy by IPTES Scheme 8 3 Preparation of Si-MWCNT/Epoxy composites Scheme 11 1 Modification of MWCNT by IPTES Scheme 11 2 Synthesis of PMMA-VTES copolymer Scheme 11 3 Preparation of Si-MWCNT/ PMMA-VTES nanocomposites Figure 2–1碳系材料結構圖 Figure 2–2碳奈米管結構 Figure 2–3 單壁碳奈米管管束的示意圖及高解析度電子顯微鏡的 觀察結果 Figure 2–4多壁碳奈米管可能的結構：左.同心圓柱結構　中.同心多 邊形右.蛋卷結構 Figure 2–5 bamboo 型碳奈米管形成示意圖 Figure 2–6 TEM pictures of bamboo-like carbon nanotube Figure 2–7電弧法生成碳奈米管裝置示意圖 Figure 2–8電弧法生成碳奈米管裝置示意圖 Figure 2–9 電弧法連續合成碳奈米管裝置示意圖 Figure 2–10 CSIRO所發展之碳奈米管整齊排列生長裝置簡圖 Figure 2–11 TEM及SEM裝置示意 Figure 2–12 HRTEM, 1: Electronen cannon in the upper part of the column. 2 Electro-magnetic lenses to direct and focus the electron beam inside the column. 3: Vacuum pumps system. 4: Opening to insert a grid with samples into the high-vacuum chamber for observation. 5: Operation panels (left for alignment; right for magnification and focussing; arrows for positioning the object inside the chamber). 6: Screen for menu and image display. 7: Water supply to cool the instrument. Figure 2–13 TPD比較圖譜。a為SWNT，b為活性碳 Figure 2–14以混酸(氧化法)改質碳奈米管 Figure 2–15 醯氯化改質碳奈米管 Figure 2–16異氰酸化法改質碳奈米管27 Figure 2–17 磺化法改質碳奈米管 Figure 2–18胺化法改質碳奈米管 Figure 2–19不同氣氛下單壁碳奈米管的電導性(a)氧氣保護下在200ppm NO2時單根半導體型單壁碳奈米管的感應電導; (b)氬氣保護下含l%NH3時單根單壁碳奈米管的感應電導 Figure 2–20填充在單璧奈米碳管中金屬Ru的高分辯電子顯微鏡 照片 Figure 2–21填充在多壁碳奈米管中氧化杉的高分辨電子顯微鏡 照片 Figure 2–22填充有銀顆粒的碳奈米管的高分辨像 Figure 2–23燃料電池反應示意圖 Figure 3–1 製備Epoxy/CNT用來黏接兩個graphite fiber/epoxy複合 材料示意圖 Figure 3–2 摻混1wt%及5wt% MWCNT之epoxy的拉伸測試 Figure 3–3 Epoxy/CNT摻混block copolymer（CCOE）、沒摻混block copolymer（CE）、僅block copolymer /epoxy（COE）及純 epoxy（ER）的拉伸測試結果 Figure 3–4 Copolymer在溶液中具有分散CNT的功能 Figure 3–5 Stress/strain responses of MWCNTs/epoxy composites. (a) 3 wt.% type I, (b) 6 wt.% type I, (c) 3 wt.% type II and (d) 6 wt.% type II. Figure 3–6不同程度CNT添加量之動態流變分析的結果 Figure 3–7 Epoxy的直流導電度隨CNT之添加的變化情形 Figure 3–8 FSWCNT/Epoxy的 (a)儲存模數 (b)損失因子 Figure 3–9 Transmission optical micrographs of epoxy composites containing 0.01 wt% multi-wall carbon nanotubes during curing at 80℃in a DC field of 100 V/cm. The bottom image shows the resulting nanotube network structure in a fully processed bulk composite cured under these conditions Figure 3–10 Transmission optical micrographs of epoxy composites containing 0.01 wt% multi-wall carbon nanotubes during curing at 80 8C in an AC field of 100 V/cm. The bottom image shows the resulting nanotube network Figure 3–11Typical tensile stress–strain curves of carbon nanotube composites and the relative matrices. (a) and (b) Samples with the soft matrices (with 9 wt% hardener and 48 h curing time for (a) and 72 h for (b)), carbon nanotubes show a significant reinforcement role and the fracture strain of nanocomposites shows no evident decrease. (c) and (d) Samples with the stiffer matrices (with 12 wt% and 13 wt% for (c) and (d), respectively, and 48 h curing time), carbon nanotubes play a slight reinforcement role. Figure 3–12 Raman spectra of the raw SWNT, purified by H2O2 reflux and with the two-step reflux process. Figure 3–13 Impedance spectroscopy plots of the composite samples containing different types of nanotubes: (a) MWCNTs; (b) chemically treated SWNTs; (c) ball-milled SWNTs; (d) electrical conductivity at 1 Hz of the composite materials as a function of nanotube content Figure 3–14 Thermal conductivity of composite materials as a function of nanotube concentration. The dashed line represents the conductivity of pure epoxy Figure 3–15 Nanocomposite structure development after processing at different gap settings (a) 50μm, (b) 20μm , (c) 10μm and (d) 5μm Figure 3–16Carboxylation reaction of carbon nanotube under UV/O3 treatment Figure 3–17 Chemical reaction between amino-functionalized MWCNTs and epoxy Figure 3–18 XRD樣品 (a)純PI (b)~(d) 5、9、12wt％碳管含量的PI-MWCNT (e)純多壁碳管 Figure 3–19 PI-MWCNT在不同碳管含量的拉伸及抗張強度的變化 Figure 3–20 PI-MWCNT在不同碳管含量下，導電性的變化(10 kHz) Figure 3–21 PI-MWCNT在不同碳管含量下，介電常數的變化 (10 kHz) Figure 3–22 製備聚亞醯胺及碳奈米管複合材料薄膜之流程 Figure 3–23 PAA-MWCNT薄膜之DSC曲線 Figure 3–24左圖為PI-MWCNT在MWCNT-Ι之含量1.14vol％ SEM圖；右圖為PI-MWCNT在MWCNT- □ 之含量1.14vol％SEM圖 Figure 3–25 PI-MWCNT在不同碳管含量下，Young’s modulus曲線 Figure 3–26 純PI和PI-MWCNT碳管含量1.14和3.71vol％之三種 比例在溫度控制從 -150℃~300℃下，所得之儲存模數 和消失模數 Figure 3–27 室溫下測試PI-MWCNT在不同碳管含量下之電阻曲線 Figure 3–28 EP膜片以光學顯微鏡觀測所得之圖 Figure 3–29 P膜片以光學顯微鏡觀測所得之圖 Figure 3–30 EP膜片以HRSEM觀測所得之圖 Figure 3–31 P薄膜以HRSEM觀測所得之圖 Figure 3–32 Structure of R-BAPB polyimide Figure 3–33 G’ and (b) (a) PMMA/purified MWCNTs and (b) PMMA/ m-MWCNTs composites versus and G” of (c) PMMA/ purified MWCNTs and (d) PMMA/m-MWCNTs composites versus at frequency at 200 ℃ with various nanotube loading Figure 3–34 The structures of various silane compounds Figure 3–35 The scheme of a MWCNT/PMMA based gas sensor Figure 3–36 Field-emission SEM images of PU–SWCNT composite: (a, c) fracture plane parallel to pressure direction (symbolized with Y in stress model) and (b, d) fracture plane perpendicular to pressure direction (symbolized with X in stress model) Figure 3–37 Synthesis of Nylon 6-SWNT Composite by Ring-Opening Polymerization of Caprolactam in the Presence of SWNTs Figure 3–38 Suggested Covalent Bonding of Polyethylene to F-SWNTs during Shear Mixing Processing Figure 3–39 A comparison of complex and steady shear viscosities Figure 3–40 TEM micrographs of cryo-microtomed nanocomposites for different MWCNT loadings, m: (a) 0.5 wt% and (b) 4.8 wt%. The scale bar is 250 nm Figure 3–41 SEM micrographs of CNTs/PET composites. Concentration of CNTs: (a) 0.5 wt%, (b) 2 wt%, (c) 4 wt% and (d) 10 wt% 131 Figure 3–42 η*of (a) PET/MWCNT nanocomposites with different MWCNT contents at 270℃ and (b) PET/MWCNT 2.0 nanocomposites at different temperatures as a function of frequency (ω) Figure 3–43 Effect of MWCNTs on (a) G’ and (b) G” of PET/MWCNT nanocomposites at 270℃ as a function of frequency(ω) Figure 3–44 Schematic diagram of electrospinning apparatus Figure 3–45 MWCNT接枝poly(acrylic acid) Figure 3–46TEM images of the pristine MWCNTs (a), HOEt-MWCNTs (b), MWCNT-g-PAA (c), and the HRTEM image of MWCNT-g-PAA (d). The inset photographs show the stability in water (after sonication for 30 min) of HOEt-MWCNTs (t ) 0) (A), MWCNT-g-PAA (t ) 0) (B), HOEt-MWCNTs (t ) 2 days) (C), and MWCNT-g-PAA (t ) 30 days) (D). The concentration of either the HOEt-MWCNTs or the MWCNT-g- PAA in the bottles is 3 mg/mL Figure 3–47 Schematic showing the change in nanotube microstructure that occurs as the pH of poly(acrylic acid) is changed. At low pH, the polymer is uncharged and highly coiled with extensive intrachain hydrogen bonding. At high pH, the carboxylic acid groups are deprotonated and the polymer is more extended as the negatively charged side groups repel one another Figure 3–48 Schematic diagram of preparation of sandwich-like SWNT/PEEK composites Figure 3–49 Fabrication procedure of MWCNT/poly(furfuryl) nanocomposites Figure 4–1 Setup of the thermal conductivity measurement Figure 5–1 FTIR spectra of (a) unmodified MWCNT, (b) acid modified MWCNT, (c) amine-modified MWCNT, (d) PI-g-MWCNT Figure 5–2 (a) 1H NMR of polyimide grafted MWCNT, (b) Chemical structure of polyimide grafted MWCNT Figure 5–3 SEM microphotographs of the MWCNT , (a) unmodified MWCNT (50,000x),(b) acid modified MWCNT (50,000x) (c) amine modified MWCNT (50,000x) Figure 5–4TEM microphotographs of (a)acid modified MWCNT(x100,000), and (b) polyimide grafted MWCNT (x40,000) Figure 5–5 SEM microphotographs of (a,b)neat polyimide (a.x50000 ; b.x10000) (c,d) Unmodified MWCNT composites polyimide (c.x50000 ; d.x10000) (e,f) acid modified MWCNT composites polyimide (e.x50000 ; f.x10000) (g,h) amine modified MWCNT composites polyimide (g.x50000 ; h.x10000) Figure 5–6 SEM microphotographs of 5.0 phr polyimide grafted MWCNT/Polyimide composites (a)x1,000, (b)x10,000 (c)x50,000 Figure 5–7TEM microphotographs of 6.98wt% of (a,b) Unmodified MWCNT/polyimide composites (a.x10,000, b.x50,000); (c,d)acid modified MWCNT/ composites polyimide (c.x10,000, d.x50,000);(e,f)amine modified CNT composites polyimide (e.x50,000, f.x100,000) (g,h) acid modified MWCNT/ composites polyimide (g.x10,000, h.x50,000) Figure 5–8 Effect of CNT content on the electrical resistivity of the MWCNT/polyimide nanocomposite (a)surface resistivity (b)volume resistivity Figure 5–9 Effect of CNT content on the tensile properties in the MWCNT/polyimide Figure 6–1 FTIR spectra of (a) isocyanatopropyltriethoxysilane(IPTES) modified MWCNT (b) (3-Aminopropyl)triethoxysilane (APTES) modified MWCNT (c) Vinyltriethoxysilane (VTES) modified MWCNT Figure 6–2 Raman spectra of (a) unmodified MWCNT (b) VTES-MWCNT-1 (c) VTES-MWCNT-2 (d) VTES-MWCNT-3 Figure 6–3 X-ray photoelectron spectroscopy(XPS) spectra of (a,b)IPTES-MWCNT-1,(c,d) IPTES-MWCNT-2 and (e,f) IPTES-MWCNT-3 Figure 6–4 X-ray photoelectron spectroscopy(XPS) spectra of (a,b) APTES-MWCNT-1, (c,d) APTES-MWCNT-2 and (e,f) APTES-MWCNT-3 Figure 6–5 X-ray photoelectron spectroscopy (XPS) spectra of (a,b) Unmodified MWCNT, (c,d) VTES-MWCNT-1, (e,f) VTES-MWCNT-2 and (g,h) VTES-MWCNT-3 Figure 6–6 Structure of (a) tri-substituted siloxane bonds (T shift) and (b) tetra-substituted siloxane bonds (Q shift) Figure 6–7 29Si solid-state NMR spectra of cured IPTES-MWCNT/Poly- imide composites with various IPTES-MWCNT ratios and contents: IPTES:MWCNT (wt%) (a) 1:1 (1.0wt%) (b) 1:1 (7.5wt%) (c) 2:1 (1.0wt%) (d) 2:1 (7.5wt%) (e) 3:1 (1.0wt%) (f) 3:1 (7.5wt%) Figure 6–8 29Si solid-state NMR spectra of cured APTES-MWCNT/Polyimide composites Figure 6–9 29Si solid-state NMR spectra of cured PVTES-MWCNT /Polyimide composites with PVTES-MWCNT content: (a) PVTES-MWCNT-1 (0.99wt%) (b) PVTES-MWCNT-1 (6.98wt%) (c) PVTES-MWCNT=2 (0.99wt%) (d) PVTES- MWCNT-2 (6.98wt%) (e) PVTES-MWCNT-3 (0.99wt%) (f)PVTES-MWCNT-3(6.98wt%) Figure 6–10 SEM microphotographs of IPTES-MWCNT/Polyimide composites with IPTES:MWCNT (a) 1:1(x1000), (b) 1:1 (x50000) (c) 2:1(x1000), (d)2:1(x50000) (e)3:1(x1000), (f)3:1(x50000) Figure 6–11 TEM microphotographs of IPTES-MWCNT/Polyimide composites with IPTES:MWCNT (a) 1:1(x10,000), (b) 1:1(x50,000) (c)2:1(x10,000), (d)2:1(x50,000) (e) 3:1 (x10,000), (f)3:1(x50,000) Figure 6–12 SEM microphotographs of APTES-MWCNT/Polyimide composites: (a) APTES-MWCNT-1 (x1000), (b) APTES- MWCNT-1 (x50000) (c) APTES-MWCNT-2 (x1000), (d) APTES-MWCNT-2 (x50000) (e) APTES-MWCNT- 3(x1000), (f) APTES-MWCNT-3(x50000) Figure 6–13 TEM microphotographs of APTES-MWCNT/Polyimide composites APTES-MWCNT-1 (a) x10,000, (b) x50,000 APTES-MWCNT-2 (c)x10,000, (d) x50,000 APTES- MWCNT-3 (e)x10,000, (f) x50,000 Figure 6–14 SEM microphotographs of PVTES-MWCNT/Polyimide composites (a)PVTES-MWCNT-1(1000x), (b) PVTES- MWCNT-1(50000x) (c)PVTES-MWCNT-2 (1000x), (d)PVTES-MWCNT-2(50000x) (e)PVTES- MWCNT- 3(1000x), (f) PVTES-MWCNT-3(50000x) Figure 6–15 TEM microphotographs of PVTES-MWCNT/Polyimide composites (a)PVTES-MWCNT-1(x10,000), (b) PVTES- MWCNT-1(x50,000) (c)PVTES-MWCNT-2(x10,000), (d) PVTES-MWCNT-2(x50,000) (e)PVTES-MWCNT-3 (x10,000), (f) PVTES-MWCNT-3(x50,000) Figure 6–16 Effect of MWCNT content on volume resistance of the MWCNT/polyimide composite :(a) IPTES-MWCNT/ Polyimide, (b) APTES-MWCNT/Polyimide, (c) VTES- MWCNT/Polyimide Figure 6–17 Effect of MWCNT content on Absolute derivative of the MWCNT /polyimide composite (a) IPTES-MWCNT/ Polyimide, (b) APTES-MWCNT/Polyimide (c) VTES- MWCNT/Polyimide Figure 6–18 Effect of MWCNT content on the tensile stress in the MWCNT/polyimide composite (a) IPTES-MWCNT, (b)APTES-MWCNT, (c) VTES-MWCNT Figure 6–19 Effect of MWCNT content on the Young’s modulus stress in the MWCNT/polyimide composite (a) IPTES-MWCNT, (b) APTES-MWCNT, (c) VTES-MWCNT Figure 7–1 Setup of the thermal conductivity measurement Figure 7–2 SEM microphotograph of the 1wt% MWCNT/Epoxy nanocomposite, (a). x30,000 and (b）x45,000 Figure 7–3 Effect of CNT content on the (a) glass transition temperature (Tg) (b) thermal expansion coefficient of the MWCNT/Epoxy nanocomposites Figure 7–4 Effect of MWCNT content on the normalized thermal conductivity of the MWCNT/Epoxy nanocomposites(km is thermal conductivity of nanocomposites and k0 is thermal conductivity of neat epoxy) Figure 7–5 Effect of CNT content on (a) surface resistivity and (b)bulk resistivity Figure 7–6 Effect of MWCNT content on dielectric constant, (a) ε’ (real part) of the MWCNT/Epoxy nanocomposites and (b) ε” (imaginary parts) of the MWCNT/Epoxy nanocomposites Figure 8–1 FT-IR spectra of (a) acid modified MWCNT; (b)isocyanatopropyltriethoxysilane modified MWCNT Figure 8–2 FT-IR spectra of the reaction between epoxy resin and isocyanatopropyltriethoxysilane Figure 8–3 X-ray photoelectron spectroscopy(XPS) spectra of (a,b)Unmodified MWCNT, (c,d) acid modified MWCNT and (e,f) IPTES modified MWCNT Figure 8–4 The solid-state 29Si NMR spectra of (a) Epoxy composities. (b) 1.0phr Silane modified MWCNT/Epoxy (c) tri-substituted siloxane bonds (T shift) Figure 8–5 (a) The solid-state 13C NMR CP/MAS spectra of silane modified MWCNT/Epoxy (numbers are correlated to Figure 8-5(b)) (b)Chemical structure of cured silane modified Epoxy Figure 8–6 DSC data of the Silane modified MWCNT/Epoxy compo- sites. (a) DSC curve of Silane modified MWCNT/Epoxy composites (b) Derivative of DSC curve of the Silane modi- fied MWCNT/Epoxy composites Figure 8–7 DMA analysis of the MWCNT/Epoxy composites (a)storage modulus (b) tan delta Figure 8–8 SEM microphotographs of the 1.0phr MWCNT/Epoxy composites (a) x5,000 (b) x 50,000 Figure 8–9 SEM microphotographs of the 1.0phr MWCNT/Epoxy composites Figure 8–10 Effect of MWCNT content on the (a)Tensile strength, (b) Young’s modulus of silane modified MWCNT/Epoxy nanocomposite Figure 8–11 Effect of MWCNT content on the (a) Flexural strength, (b) Flexural modulus of silane modified MWCNT/Epoxy nanocomposite Figure 8–12 Effect of MWCNT content on the (a)surface electrical resistivity Figure 9–1 MWCNT coated with TiO2 and modification with (3-aminopropyl)- triethoxysilane Figure 9–2 X-ray photoelectron spectroscopy(XPS) spectra of (a,b) Unmodified MWCNT, (c,d) TiO2 coated MWCNT and (e,f) APTES modified TiO2 coated MWCNT Figure 9–3 TEM microphotographs of the (a) TiO2 coated MWCNT (b) 0.99wt% unmodified MWCNT/Epoxy composites (c) 0.99wt% of AT-MWCNT/Epoxy composites Figure 9–4 SEM microphotographs of 0.99wt% (a)unmodified MWCNT/Epoxy composites (b)AT-MWCNT/Epoxy composites Figure 9–5 Effect of CNT content on (a)Tensile strength, (b)Young’s Modulus of the MWCNT/Epoxy composite Figure 9–6 Effect of CNT content on (a) Flexure strength and (b) Flexure Modulus of the MWCNT/Epoxy composite Figure 9–7 Effect of MWCNT content on volume electricity resistivity of the MWCNT/Epoxy composite Figure 10–1 XRD of the MWCNTs Figure 10–2 X-ray photoelectron spectroscopy(XPS) spectra of (a,b) Unmodified MWCNT, (c,d) T-30, (e,f) T-300 and (g,h) T-3000 Figure 10–3 TEM microphotographs (x 25,000) of (a) T-30, (b), T-300, (c) T-3000 Figure 10–4 TEM microphotographs (x 25,000) of 0.99wt% of (a)unmodified MWCNT/PSSQ/Epoxy, (b), T-30/PSSQ/Epoxy, (c) T-300/PSSQ/Epoxy and (d) T-3000/PSSQ/Epoxy Figure 10–5 Effect of MWCNT content on mechanical properties of the MWCNT/PSSQ/Epoxy composites (a) Tensile strength, (b) Young’s Modulus, (c) Flexure strength and (d) Flexure Modulus Figure 10–6 Effect of MWCNT content on volume electricity resistivity of the TiO2 coated MWCNT/PSSQ/Epoxy composite Figure 11–1 FT-IR spectra of (a) acid modified MWCNT (b)isocyanatopropyltriethoxysilane modified MWCNT Figure 11–2 29Si solid-state NMR spectra of cured PMMA-VTES composites with Si-MWCNT content (a) 0 (b)0.5 (c)0.99 (d)1.96 (e)2.91 and (f)3.85 wt% Figure 11–3 Structure of (a) tri-substituted siloxane bonds (T shift) and (b) tetra-substituted siloxane bonds (Q shift) Figure 11–4 SEM microphotographs of the 3.85wt% MWCNT/PMMA-VTES nanocomposite, (a). x10,000 and (b) x50,000 Figure 11–5 TEM microphotographs of the 3.85wt% MWCNT/PMMA-VTES nanocomposite, (a). x40,000 and (b)x100,000 Figure 11–6 Effect of CNT content on the (a) surface resistivity (b) volume resistivity of Si-MWCNT/PMMA- VTES nano- composites Figure 11–7 Effect of MWCNT content on the thermal conductivity of Figure 11–8 TGA curves of Si-MWCNT/PMMA-VTES composite Table 2 1碳奈米管的物理性質 Table 2 2單壁及多壁碳奈米管之性質比較 Table 3 1各類改質碳管所用的溶劑與編號 Table 3 2 Specification of nanoparticles applied in the studies Table 3 3 Mechanical properties of pure epoxy and CNT/epoxy composites Table 3 4 EP-SWNT薄膜在常溫下的性質比較 Table 3 5 P-SWNT薄膜在常溫下的性質比較 Table 3 6 EP-SWNT薄膜電阻抗值 Table 3 7 P-SWNT薄膜電阻抗值 Table 3 8 Slopes of G’ versus frequency and of G” versus frequency for PMMA/ MWCNTs composites Table 3 9 Mechanical Properties of Nylon and Nylon 6-SWNT Composite Fibers Table 3 10 Mechanical Properties of the SWNT/PE Composites and Pure PE Table 3 11 DSC Results for the PET/MWCNT Nanocomposites with respect to the MWCNT Content Table 3 12 Thermal Stability of the PET/MWCNT Nanocomposites as a Function of the MWCNT Content Table 5 1 Glass transition temperature (Tg) of the MWCNT/polyimide Nanocomposite Table 5 2 Properties of the MWCNTs/polyimide composites Table 6 1 The ratios of IPTES to acid modified MWCNT for IPTES modified MWCNT Table 6 2 The ratios of APTES to acid modified MWCNT for APTES- MWCNT Table 6 3 The ratios of VTES to unmodified MWCNT for PVTES modified MWCNT Table 6 4 Percentages of T- and Q- substitution of IPTES-MWCNT/polyimide composites Table 6 5 Percentages of T- and Q- substitution of APTES-MWCNT/polyimide composites Table 6 6 Percentages of T- and Q- substitution of PVTES-MWCNT/polyimide composites Table 8 1 T1ρH spin lock relaxation time measured at 300K of correspondingsegmental motions of silane modified MWCNT/Epoxy composites. (Carbon numbers are correlated to Figure 8-5b)) Table 9 1 Atomic percentage determined using the XPS spectra Table 10 1 The condition of TiO2 coated on MWCNT Table 10 2 Properties of the MWCNTs/polyimide composites Table 11 1 Degree of condensation of Tri-substituted distribution Table 11 2 Thermal stability of Si-MWCNT/PMMA-VTES Table 12 1 Properties of the MWCNT/Polymer composites

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    第八章參考文獻
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    第九章參考文獻
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    第十章參考文獻
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    [2] H Geng, R Rosen, B Zheng, H Shimoda, L Fleming, JZ Liu. Fabrication and Properties of Composites of Poly(ethylene oxide) and Functionalized Carbon Nanotubes. Advanced Materials 2002;14: 1387-1390.
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    第十一章參考文獻
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