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研究生: 林倩儀
Lin, Chien-I
論文名稱: 表面附著錫/二氧化錫之多層奈米碳管之合成與性質研究
Synthesis and Properties of Sn/SnO2 Coated Multi-Walled Carbon Nanotubes
指導教授: 林光隆
Lin, Kwang-Lung
學位類別: 碩士
Master
系所名稱: 工學院 - 材料科學及工程學系
Department of Materials Science and Engineering
論文出版年: 2013
畢業學年度: 101
語文別: 中文
論文頁數: 70
中文關鍵詞: 焊錫奈米碳管金屬/奈米碳管複合材料熱傳導係數
外文關鍵詞: Sn, carbon nanotube, metal/carbon nanotube, thermal conductivity
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  • 本實驗係利用不同的多壁奈米碳管表面處理與還原方式以製備錫/奈米碳管複合材料,即Sn/MWCNTs 粉末。實驗方法有三種,第一種方式為將市售奈米碳管藉硝酸氧化形成具結合力的表面結構(O-MWCNTs),繼以SnCl2 和HCl 的混合水溶液先在O-MWCNTs 表面鍵結SnO2 以形成SnO2/MWCNTs,再利用還原氣氛還原回焊以形成鍍錫的Sn/MWCNTs;第二種方式為利用強還原劑NaBH4 滴定含O-MWCNTs 的SnCl2 水溶液以形成Sn/MWCNTs;第三種方式則藉由具capping effect 的3,5-diaminobenzoic acid(DBA)有機酸改質市售碳管以形成DBA/MWCNTs 後, 再以還原劑NaBH4 滴定含DBA/MWCNTs 與SnCl2 水溶液的懸浮溶液。capping agent(DBA)的功用在於控制還原錫的形狀與大小,因此可在DBA/MWCNTs 表面附著均勻的奈米級純錫顆粒,稱為Sn-DBA/MWCNTs。此外,本研究利用迴焊步驟使銲錫覆蓋MWCNTs 表面。考量電子元件導熱及散熱之需求下,本實驗進一步將Sn-DBA/MWCNTs 壓成錠片並燒結,製成複合材料以進行熱導係數k 的量測, 並於結果發現燒結後Sn-DBA/MWCNTs 錠片之k 值較燒結前Sn-DBA/MWCNTs 錠片優良。

    This study tried to functionalize the surface of pristine multiwall carbon nanotubes(P-MWCNTs) with various methods. Thus treated MWCNTs were mixed with Sn ion containing solution to reduce Sn ion and to produce Sn/MWCNTs composite. One of the processes attempted was to oxidize the surface of P-MWCNTs with nitric acid treatment so as to provide appropriate surface for the following Sn deposit. The oxidized MWCNTs were then dispersed in SnCl2 solution to form SnO2 coated MWCNTs. The SnO2 coated CNTs were further reduced and reflowed under reducing atmosphere to form Sn/MWCNTs. The other process for producing Sn/MWCNTs was incorporated with the functionalization of MWCNTs with DBA, C7H8N2O2, as capping agent. The MWCNTs functionalized with DBA were then dispersed in SnCl2 solution followed by titrating with the reducing agent, NaBH4 solution. The size and theshape of particles coated on the wall could be manipulated by DBA. The SEM and TEM images showed that the surface of DBA/MWCNTs was uniformly coated with Tin particles and is termed Sn-DBA/MWCNTs. For the interest of thermal management in electronic packages the Sn-DBA/MWCNTs powders were pressed and then sintered for thermal conductivity evaluation. It was found that the thermal conductivity of sintered Sn-DBA/MWCNTs is better than the as pressed Sn-DBA/MWCNTs.

    中文摘要 Ⅰ 英文摘要 Ⅱ 致謝 Ⅲ 總目錄 Ⅳ 表目錄 Ⅵ 圖目錄 VII 第壹章 簡介 1 1-1 奈米碳管的發現 1 1-1-1 單壁奈米碳管之結構 3 1-1-2 多壁奈米碳管之結構 3 1-2 奈米碳管的性質 3 1-2-1 電性質 3 1-2-1-1 單壁奈米碳管之電性 3 1-2-1-2 多壁奈米碳管之電性 7 1-2-2 機械性質 7 1-2-3 熱性質 8 1-3 奈米碳管的有機改質 8 1-4 奈米碳管的應用 9 1-5 熱界面材料之種類與特性 10 1-5-1 熱界面材料的需求 10 1-5-2 熱界面材料的種類 10 1-5-3 熱傳導係數量測原理 11 1-5-4 奈米碳管與其複合材料之熱導性質 13 1-6 研究目的 14 第貳章 實驗方法與步驟 15 2-1 實驗構想 15 2-2 實驗流程 15 2-2-1 奈米碳管酸洗前處理(O-MWCNTs)15 2-2-2 酸洗奈米碳管表面附著金屬錫(Sn-MWCNTs)18 2-2-2-1 雙步驟還原法 18 2-2-2-2 單步驟還原法 19 2-2-3 改質奈米碳管表面附著金屬錫(Sn-DBA/MWCNTs)20 2-2-3-13,5-diaminobenzoic acid(DBA) /奈米碳管之合成 20 2-2-3-2 還原法合成Sn-DBA/MWCNTs 20 2-2-3-3 Sn-DBA/MWCNTs 壓錠及燒結 20 2-3 分析方式與試片準備 23 第參章 結果與討論 25 3-1 奈米碳管氧化程度 25 3-2 雙步驟還原法之奈米碳管形貌與成份分析 29 3-3 單步驟還原法之奈米碳管形貌與成份分析 38 3-4 化學改質後Sn-DBA/MWCNTs 性質分析與應用 44 3-5 鍍錫奈米碳管複合材錠片之熱傳導性質 54 3-6 未來研究方向之建議 61 第肆章 結論 62 參考文獻 63

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