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微波輔助快速官能基化多壁奈米碳管暨其複合材料之應用 = Rapidly ...
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國立高雄大學化學工程及材料工程學系碩士班
微波輔助快速官能基化多壁奈米碳管暨其複合材料之應用 = Rapidly Microwave-Assisted Functionalizations of Multi-Wall Carbon Nanotubes and Their Applications in Nanocomposites
紀錄類型:
書目-語言資料,印刷品 : 單行本
並列題名:
Rapidly Microwave-Assisted Functionalizations of Multi-Wall Carbon Nanotubes and Their Applications in Nanocomposites
作者:
謝孟男,
其他團體作者:
國立高雄大學
出版地:
[高雄市]
出版者:
撰者;
出版年:
2012[民101]
面頁冊數:
119面圖,表格 : 30公分;
標題:
奈米碳管
標題:
Carbon nanotubes
電子資源:
http://handle.ncl.edu.tw/11296/ndltd/94900943724856282524
附註:
106年10月31日公開
附註:
參考書目:面101-108
摘要註:
多壁奈米碳管(CNT)具有高長徑比,在受外力作用時會彎曲形變並且有很好的恢復特性,還具有高強度、韌性佳及化學性質穩定等優點,是理想的補強材料。本實驗利用微波輔助快速官能基化的方法,改善CNT 在乙烯基酯樹脂(vinyl ester,VE)(內含55 wt% 苯乙烯(SM))中之分散性,以Grafting from 和Grafting to 的接枝方式,在CNT表面依序接上vinyltrimethoxysilane (VTMS)及methacryl-oxypropyl- trimethoxysilane (MATMS)。VTMS 具有乙烯基,在微波輔助下,以自由基機構可快速與CNT 上的碳碳雙鍵反應而接枝上去。MATMS 之烷氧基可與接枝上去之VTMS 之烷氧基在水解後行縮合反,MATMS 上未反應之甲基丙烯酸基可與乙烯基酯樹脂之乙烯基反應並產生交聯,可將有機相與無機相之間以共價鍵相連結,如此可使複合材料在受力時能將應力能量,從基材相有效地傳送到CNT 上,而CNT 之優異機械性質可抵抗應力,因而可提升複合材料之機械強度。本實驗之改質碳管(CNT-VTMS-MATMS),以0.5, 1,及2 phr 添加量加入內含1 phr BPO (benzoyl peroxide)之VE 中,均勻混合後,以(1) 100 oC- 4 h 及 (2) 120 oC-10 h 兩階段加溫程序進行硬化。硬化之複合材料,由SEM 之調查結果顯示,改質碳管能均勻分散在樹脂基材當中。由DSC 的調查可知,Tg 隨改質碳管添加量上升而下降,在改質碳管添加量為2.0 phr 時,Tg 下降了約47 oC。由DMA 的調查得知,樹脂在改質碳管添加量為2.0 phr 時,因改質碳管上VTMS-MATMS 柔軟片段的導入複合材料中,其Tan θ 之峰值由148.68 oC 下降到144.74 oC,在27 oC 下之儲存模數提升45.67%,且在100 oC 下亦能保持此增強效果,證明碳管上之官能基能與基材間能形成共價鍵結。在27 oC下之損失模數提升37.2%,推論此複合材料比純樹脂在外力衝擊時,較能吸收衝擊能量,進而提升複合材料之耐衝擊性質。 Multi-walled carbon nanotubes (CNT) are known to have high aspect ratio, high mechanical strength, excellent toughness, and high chemical resistance, and thus are an ideal reinforcement for polymer composites. In this study, a rapid microwave-assisted functionalization of CNT was conducted to improve the dispersion of CNT in the vinyl ester resin (vinyl ester, VE) (containing 55 wt% styrene (SM)) via "Grafting from" and "Grafting to" methods that allowed vinyltrimethoxysilane (VTMS) and methacryl-oxypropyl-trimethoxysilane (MATMS) to attach to the surface of CNT sequentially to obtain surface-modified CNT denoted by CNT-VTMS-MATMS. The vinyl groups of VTMS could react with the C=C double bonds on the sidewall of CNT via free radical reactions under microwave irradiation so that the VTMS was covalently attached to the surface of CNT. The alkoxyl group of MATMS and the alkoxyl group of VTMS attached to the surface of CNT could covalently bond together by condensation reactions after hydrolyses. The methacryl group of MATMS on the CNT-VTMS-MATMS could crosslink with the methacryl group of VE so that the polymer and CNT were covalently bonded together to form networked composites, leading to efficient load transfers from matrix to CNT upon an external stress and showing enhanced mechanical strengths. The samples containing 0.5, 1, and 2 phr CNT-VTMS-MATMS in VE were heated at 100 oC for 4 h followed by heating at 120 oC for 10 h to examine the CNT dispersion via a scanning electron microscopy (SEM) and the effects of CNT-VTMS-MATMS on Tg and mechanical properties via a differential scanning calorimeter (DSC) and a dynamic mechanical analyzer (DMA). SEM images found that the CNT-VTMS-MATMS could homogeneously disperse in VE matrices. DSC data revealed that Tg of the composite containing 2 phr CNT-VTMS-MATMS was decreased by 22.9 oC. DMA data revealed that the storage modulus for the composite containing 2 phr CNT-VTMS-MATMS at 27 oC was enhanced by 45.67%, with similar enhancement observed at 100 oC, an indication that strong covalent bonds were formed between the modified CNT and VE. The composite containing 2 phr CNT-VTMS-MATMS exhibited an increased loss modulus by 37.2% at 27 oC, an indication that the composite could absorb more impact energy than the pristine VE resin. The introduction of the soft Si-O-Si segments was found to decrease the Tan θ peak from 148.68 oC to 144.74 oC for the composite containing 2 phr CNT-VTMS-MATMS.
微波輔助快速官能基化多壁奈米碳管暨其複合材料之應用 = Rapidly Microwave-Assisted Functionalizations of Multi-Wall Carbon Nanotubes and Their Applications in Nanocomposites
謝, 孟男
微波輔助快速官能基化多壁奈米碳管暨其複合材料之應用
= Rapidly Microwave-Assisted Functionalizations of Multi-Wall Carbon Nanotubes and Their Applications in Nanocomposites / 謝孟男撰 - [高雄市] : 撰者, 2012[民101]. - 119面 ; 圖,表格 ; 30公分.
106年10月31日公開參考書目:面101-108.
奈米碳管Carbon nanotubes
微波輔助快速官能基化多壁奈米碳管暨其複合材料之應用 = Rapidly Microwave-Assisted Functionalizations of Multi-Wall Carbon Nanotubes and Their Applications in Nanocomposites
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多壁奈米碳管(CNT)具有高長徑比,在受外力作用時會彎曲形變並且有很好的恢復特性,還具有高強度、韌性佳及化學性質穩定等優點,是理想的補強材料。本實驗利用微波輔助快速官能基化的方法,改善CNT 在乙烯基酯樹脂(vinyl ester,VE)(內含55 wt% 苯乙烯(SM))中之分散性,以Grafting from 和Grafting to 的接枝方式,在CNT表面依序接上vinyltrimethoxysilane (VTMS)及methacryl-oxypropyl- trimethoxysilane (MATMS)。VTMS 具有乙烯基,在微波輔助下,以自由基機構可快速與CNT 上的碳碳雙鍵反應而接枝上去。MATMS 之烷氧基可與接枝上去之VTMS 之烷氧基在水解後行縮合反,MATMS 上未反應之甲基丙烯酸基可與乙烯基酯樹脂之乙烯基反應並產生交聯,可將有機相與無機相之間以共價鍵相連結,如此可使複合材料在受力時能將應力能量,從基材相有效地傳送到CNT 上,而CNT 之優異機械性質可抵抗應力,因而可提升複合材料之機械強度。本實驗之改質碳管(CNT-VTMS-MATMS),以0.5, 1,及2 phr 添加量加入內含1 phr BPO (benzoyl peroxide)之VE 中,均勻混合後,以(1) 100 oC- 4 h 及 (2) 120 oC-10 h 兩階段加溫程序進行硬化。硬化之複合材料,由SEM 之調查結果顯示,改質碳管能均勻分散在樹脂基材當中。由DSC 的調查可知,Tg 隨改質碳管添加量上升而下降,在改質碳管添加量為2.0 phr 時,Tg 下降了約47 oC。由DMA 的調查得知,樹脂在改質碳管添加量為2.0 phr 時,因改質碳管上VTMS-MATMS 柔軟片段的導入複合材料中,其Tan θ 之峰值由148.68 oC 下降到144.74 oC,在27 oC 下之儲存模數提升45.67%,且在100 oC 下亦能保持此增強效果,證明碳管上之官能基能與基材間能形成共價鍵結。在27 oC下之損失模數提升37.2%,推論此複合材料比純樹脂在外力衝擊時,較能吸收衝擊能量,進而提升複合材料之耐衝擊性質。 Multi-walled carbon nanotubes (CNT) are known to have high aspect ratio, high mechanical strength, excellent toughness, and high chemical resistance, and thus are an ideal reinforcement for polymer composites. In this study, a rapid microwave-assisted functionalization of CNT was conducted to improve the dispersion of CNT in the vinyl ester resin (vinyl ester, VE) (containing 55 wt% styrene (SM)) via "Grafting from" and "Grafting to" methods that allowed vinyltrimethoxysilane (VTMS) and methacryl-oxypropyl-trimethoxysilane (MATMS) to attach to the surface of CNT sequentially to obtain surface-modified CNT denoted by CNT-VTMS-MATMS. The vinyl groups of VTMS could react with the C=C double bonds on the sidewall of CNT via free radical reactions under microwave irradiation so that the VTMS was covalently attached to the surface of CNT. The alkoxyl group of MATMS and the alkoxyl group of VTMS attached to the surface of CNT could covalently bond together by condensation reactions after hydrolyses. The methacryl group of MATMS on the CNT-VTMS-MATMS could crosslink with the methacryl group of VE so that the polymer and CNT were covalently bonded together to form networked composites, leading to efficient load transfers from matrix to CNT upon an external stress and showing enhanced mechanical strengths. The samples containing 0.5, 1, and 2 phr CNT-VTMS-MATMS in VE were heated at 100 oC for 4 h followed by heating at 120 oC for 10 h to examine the CNT dispersion via a scanning electron microscopy (SEM) and the effects of CNT-VTMS-MATMS on Tg and mechanical properties via a differential scanning calorimeter (DSC) and a dynamic mechanical analyzer (DMA). SEM images found that the CNT-VTMS-MATMS could homogeneously disperse in VE matrices. DSC data revealed that Tg of the composite containing 2 phr CNT-VTMS-MATMS was decreased by 22.9 oC. DMA data revealed that the storage modulus for the composite containing 2 phr CNT-VTMS-MATMS at 27 oC was enhanced by 45.67%, with similar enhancement observed at 100 oC, an indication that strong covalent bonds were formed between the modified CNT and VE. The composite containing 2 phr CNT-VTMS-MATMS exhibited an increased loss modulus by 37.2% at 27 oC, an indication that the composite could absorb more impact energy than the pristine VE resin. The introduction of the soft Si-O-Si segments was found to decrease the Tan θ peak from 148.68 oC to 144.74 oC for the composite containing 2 phr CNT-VTMS-MATMS.
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