奈米碳管強化聚甲基丙烯酸甲酯之奈米複合材料的熱傳性質研究

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研究生：	洪文泰 Wen-Tai Hong
論文名稱：	奈米碳管強化聚甲基丙烯酸甲酯之奈米複合材料的熱傳性質研究 Investigations on the thermal conductivity of composites reinforced with carbon nanotubes
指導教授：	戴念華 Nyan-Hwa Tai
口試委員:
學位類別：	碩士 Master
系所名稱：	工學院 - 材料科學工程學系 Materials Science and Engineering
論文出版年：	2007
畢業學年度：	95
語文別：	中文
論文頁數：	110
中文關鍵詞：	奈米複合材料、奈米碳管、聚甲基丙烯酸甲酯、熱傳導係數
外文關鍵詞：	Nanocomposites, carbon nanotube, PMMA, thermal conductivity
相關次數：	點閱：2 下載：0
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在本研究以共沉澱法製備奈米碳管複合材料並以暫態平面法測量複合材料的熱導係數。另外，也利用過濾碳管溶液製作奈米碳管薄膜，並利用雷射閃光法測量其熱擴散係數進而計算其熱導係數，如此可以得知奈米碳管薄膜及其所強化的奈米複合材料之熱傳係數，此實驗值將與理論值作比較。除此，純化過程、量測溫度與碳管的異向性大幅影響複合材料的熱導係數，本研究中將加以探討影響的機制。
純化對於碳管熱導性質的影響是利用掃描式電子顯微鏡、熱重分析儀與拉曼等儀器來分析。掃描式電子顯微鏡分析奈米碳管純化前後的差異，發現純化後的碳管存在的金屬粒子變少。熱重的結果顯示純化的確改善了碳管的熱穩定性質；由拉曼分析得知碳管在純化過程會造成表面結構的破壞。在室溫下，單壁奈米碳管薄膜的熱導係數為2.24 W/m K，多壁奈米碳管薄膜為0.36 W/m K。另一方面，單壁與多壁奈米碳管薄膜的熱導係數並未隨著溫度的增加而上升，而是逐漸下降的。本研究對奈米複合材料的熱傳導係數進行研究，結果顯示添加4.0 wt%未純化的多壁奈米碳管對於複合材料熱導性質的提升量最高，可達到基材熱導係數的十倍以上。大致說來，奈米碳管複合材料的熱導係數皆隨著碳管含量與溫度的增加而上升。

In this work, we prepared carbon nanotubes/polymethyl methacrylate(CNTs/PMMA) composites and measured its thermal conductivity by the Transient Plane Source (TPS) method. Moreover, we prepared CNTs buckypapers from CNTs suspension and measured its thermal diffusivity by the laser flash method for calculating the thermal conductivity of the buckypapers. The thermal conductivity of the composites fabricated from buckypapers was also investigated, the results were compared with the theoretical predictions. The effects of purification, test temperature and anisotropy of CNTs on thermal conductivity of the composites were investigated.
The influences of the purification process on CNTs was analyzed by Thermogravimetry Analyzer (TGA)、Raman Scattering Spectrometer (Raman) and Field Emission Scanning Electron Microscopy (FESEM). FESEM images showed that the catalysts metals in CNTs were reduced after the purification process. The TGA results showed that thermal stability of CNTs was improved after purification, but the structure of carbon nanotubes was also damaged. The thermal conductivities at room temperature of SWNT and MWNT films were 2.24 W/m K, and 0.36 W/m K, respectively. The thermal conductivities of CNT films increased with decreased of temperature. In this study, the highest thermal conductivity of W/m K was attained when the unpurified MWNTs loadings reaches 4.0 wt %, which is over 10 times higher than the thermal conductivity of PMMA. The thermal conductivity of composites increases with CNT loadings and temperature was also detected.

摘要………………………………………………………………………Ⅰ
英文摘要…………………………………………………………………Ⅱ
致謝………………………………………………………………………Ⅲ
總目錄……………………………………………………………………Ⅳ
圖表目錄…………………………………………………………………Ⅷ
第一章 緒論……………………………………………………………1
第二章 文獻回顧………………………………………………………2
1 奈米碳管的發現與性質…………………………………………2
1.1 奈米碳管的製備與應用……………………………………2
1.2 奈米碳管的導電、熱性質與理論值………………………3
1.3 奈米碳管的分散與化學處理………………………………4
1.4 官能基對熱導值的效應……………………………………5
1.5 奈米碳管薄膜的性質………………………………………6
1.6 奈米碳管複合材料的等效熱傳導係數公式模型Maxwell
   Garnette……………………………………………………………8
2 高分子材料的優點………………………………………………12
2.1 低密度………………………………………………………12
2.2 可塑性高……………………………………………………12
2.3 低成本………………………………………………………13
2.4 安定的化學性質……………………………………………13
3 奈米碳管複合材料的熱導性質…………………………………13
4 熱傳導的量測方法………………………………………………15
4.1 熱流計法(heat flow meter method)……………………15
4.2 瞬態法………………………………………………………16
       2.4.2.1 熱帶法(hot strip method)………………………17
       2.4.2.2 比較縱向熱流法……………………………………17
       2.4.2.3 雷射閃光法(laser flash technique) …………19
       2.4.2.4 暫態平面熱源法(transient plane source)……20
       2.4.2.5 3ω分析法……………………………………………21
第三章 研究方法與實驗步驟
1 研究方法…………………………………………………………27
2 儀器總介…………………………………………………………27
2.1 CVD 系統……………………………………………………27
2.2 粉碎機………………………………………………………28
2.3 超音波震動機………………………………………………28
2.4 水循環過濾系統……………………………………………28
2.5 電磁攪拌機…………………………………………………29
2.6 真空烘箱……………………………………………………29
2.7 熱壓機………………………………………………………29
2.8 場發射掃描式電子顯微鏡…………………………………29
2.9 拉曼光譜儀…………………………………………………30
2.10熱重分析儀…………………………………………………31
2.11霍式轉換紅外光譜儀………………………………………31
2.12暫態平面熱源分析儀………………………………………31
2.13雷射閃光熱傳導係數分析儀………………………………32
3 奈米碳管與奈米複合材料之製程………………………………32
3.1 化學氣相沉積法生成奈米碳管……………………………32
3.2 化學氣相沉積法生成單壁奈米碳管………………………34
3.3 化學氣相沉積法生成多壁奈米碳管………………………34
3.4 奈米碳管的純化與表面羧基的生成………………………35
       3.3.4.1 單壁奈米碳管的純化………………………………36
       3.3.4.2 多壁奈米碳管的純化………………………………36
3.5 碳管表面官能基的建立……………………………………36
4 碳管/ 聚甲基丙烯酸甲酯複合材料的製作……………………36
4.1 單壁奈米碳管/聚甲基丙烯酸甲酯 預混材的製作………37
4.2 多壁奈米碳管/聚甲基丙烯酸甲酯 預混材的製作………38
4.3 預混材的熱壓合……………………………………………38
5 碳管薄膜的製作…………………………………………………38
5.1 純化單壁碳管薄膜的製作…………………………………38
5.2 純化多壁碳管薄膜的製作…………………………………39
6 複合材料沿平面熱導值量測試片的製作………………………39
第四章 結果與討論……………………………………………………48
1 奈米碳管純化前後的結果………………………………………48
1.1 單壁奈米碳管………………………………………………48
1.2 多壁奈米碳管………………………………………………49
1.3 官能基的建立………………………………………………49
2 未純化奈米碳管複合材料的熱導係數值………………………50
2.1 未純化單壁奈米碳管強化複合材料試片…………………50
2.2 未純化多壁奈米碳管強化複合材料試片…………………51
2.3 純化單壁奈米碳管強化複合材料試片……………………51
2.4 純化多壁奈米碳管強化複合材料試片……………………52
3 提升量的比較……………………………………………………52
4 奈米碳管複材的熱容值…………………………………………52
5 溫度對奈米碳管複材的影響……………………………………53
5.1 未純化奈米碳管……………………………………………54
5.2 純化奈米碳管………………………………………………54
5.3 高分子受溫度的效應………………………………………55
6 奈米碳管薄膜(buckypapers)的熱傳導係數 …………………55
6.1 奈米碳管薄膜的熱擴散係數………………………………55
6.2 奈米碳管薄膜的密度………………………………………56
6.3 奈米碳管薄膜的熱容值……………………………………56
6.4 奈米碳管薄膜的熱傳導係數………………………………57
7 溫度對純化奈米碳管薄膜熱傳導係數的影響…………………58
7.1 純化單壁奈米碳管…………………………………………58
7.2 純化多壁奈米碳管…………………………………………58
8 純化複材熱導係數的理論與量測值……………………………59
9 表面電阻的量測…………………………………………………61
9.1 未純化單壁奈米碳管試片…………………………………61
9.2.未純化多壁奈米碳管試片…………………………………61
9.3.純化單壁奈米碳管試片……………………………………61
9.4.純化多壁奈米碳管試片……………………………………62
10 場發射掃描式電子顯微鏡之FESEM型貌觀察…………………62
11 沿平面熱導值與垂直熱導值的比較 …………………………64
第五章 結論 …………………………………………………………105
第六章 參考文獻 ……………………………………………………106

                                

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