臺灣博碩士論文加值系統

本研究藉著改變界面活性劑（氯化十六烷基?啶，CPC）與黏土（clay）的當量比來膨潤黏土，並各以不同添加量的黏土及已膨潤黏土與聚對苯二甲酸丁酯（PBT）作溶液及熔融摻合，製備出各種組成之聚對苯二甲酸丁酯/黏土 納米複合材料。
再以最終的黏土層間距離（利用XRD），試片截斷面（利用SEM）及內部（利用TEM）之相形態，來證實氯化十六烷基?啶確能降低黏土與聚對苯二甲酸丁酯的相界面張力而提升兩者的相容性，使聚對苯二甲酸丁酯主鏈較易插層入黏土層間；並且，以此探討黏土分散於聚對苯二甲酸丁酯基材的機制。更進一步地，測試其熱性質（利用DSC；TGA；TMA）及機械性質（利用Flexural Test；Tensile Test；Izod Impact Test），並討論其性質變化與黏土分散程度的關係。

In this research, the clay interlayers had been swelled by changing the equivalent ratio of the surfactants (cetylpridium chloride, CPC) and the clays. Then, different amounts of the clays and the swelled clays were added to polybutylene terephthalate (PBT) for solution and melt blending to prepare kinds of PBT/clay nanocomposites.
With the final d-spacing of the clays (by XRD) and the morphology of the broken (by SEM) and internal (by TEM) specimen sections, we confirmed that CPC did decrease the interfacial tenses of the clays and PBT and enhance the compatibility between the two phases to make the PBT main chains intercalate into the clay interlayers more easily. The mechanism of the dispersing of the clays in PBT matrix were then investigated. Further, we tested the thermal (by DSC;TGA;TMA) and mechanical (by Flexural Test; Tensile Test; Izod Impact Test) properties, and discussed the relationships between changes of the properties and the clay dispersions.

目錄
中文摘要....................................................Ⅰ
英文摘要....................................................Ⅱ
誌謝........................................................Ⅲ
目錄........................................................Ⅳ
表目錄......................................................Ⅶ
圖目錄......................................................Ⅸ
一、 前言
1.1 納米複合材料簡介.....................................1
1.2 文獻回顧.............................................5
二、 理論部分
2.1 納米粒子的特性.......................................9
2.2 黏土礦物結構........................................11
2.3 黏土的改質..........................................12
2.4 黏土的分散..........................................13
三、 實驗部分
3.1 實驗材料與藥品......................................15
3.2 實驗設備與儀器......................................17
3.3 實驗方法
3.3.1 黏土的膨潤....................................20
3.3.2 製備PBT nanocomposites.........................20
3.4 材料測試與分析
3.4.1 X光繞射（XRD）測試..............................21
3.4.2 掃瞄式電子顯微鏡（SEM）觀察.....................21
3.4.3 穿透式電子顯微鏡（TEM）觀察.....................22
3.4.4 示差掃瞄式熱分析（DSC）.........................22
3.4.5 熱重損失分析（TGA）.............................22
3.4.6 熱機械分析（TMA）...............................22
3.4.7 擺錘式耐衝擊（Izod Impact）測試.................23
3.4.8 抗張（Tensile）測試.............................23
3.4.9 抗折（Flexural）測試............................23
3.5 實驗流程............................................24
四、 結果與討論
4.1 XRD................................................25
4.2 SEM................................................29
4.3 TEM................................................30
4.4 DSC................................................31
4.5 TGA................................................33
4.6 TMA................................................33
4.7 Izod Impact Test.......................................34
4.8 Tensile Test..........................................34
4.9 Flexural Test..........................................35
一、 結論...................................................36
六、 參考文獻...............................................38
表目錄
表1.2.1 高分子複合材料的分類................................42
表1.2.2 體積濃度2%之粒子分散系的粒子間距離..................43
表1.2.3 聚酯納米複合材料之機械性質..........................43
表4.1.1 不同當量比之clay/CPC已膨潤黏土的層間距離............44
表4.1.2 溶液摻合法PBT nanocomposites中各組成之層間距離......44
表4.1.3 熔融摻合法PBT nanocomposites中各組成之層間距離......45
表4.4.1 熔融摻合法PBT nanocomposites中各組成之結晶及熔融
性質...............................................46
表4.4.2 溶液摻合法PBT nanocomposites中各組成之結晶及熔融
性質...............................................46
表4.5.1 熔融摻合法PBT nanocomposites中各組成之熱裂解
溫度Td.............................................47
表4.5.2 溶液摻合法PBT nanocomposites中各組成之熱裂解
溫度Td.............................................48
表4.6.1 熔融摻合法PBT nanocomposites中各組成之熱膨脹
係數α.............................................49
表4.7.1 熔融摻合法PBT nanocomposites中各組成之Izod Impact Value.............................................50
表4.8.1 熔融摻合法PBT nanocomposites中各組成之Tensile Elongation........................................51
表4.9.1 熔融摻合法PBT nanocomposites中各組成之Flexural Modulus...........................................52
圖目錄
圖1.1.1 傳統複合材料與納米複合材料分散比較示意圖............53
圖2.1.2 一次粒子與二次粒子示意圖............................54
圖2.2.1 蒙脫土的晶體結構圖..................................54
圖2.3.1 以CPC膨潤黏土的插層機制示意圖.......................55
圖2.4.1 x射線晶體繞射圖.....................................56
圖4.1 CPC當量與黏土層間距離之關係圖.........................57
圖4.1.1 天然黏土及各種當量比的已膨潤黏土之WXRD圖............58
圖4.1.2 以溶液摻合法製備各種不同組成PBT nanocomposites之WXRD圖................................................59
圖4.1.3 添加10phr之不同當量已膨潤黏土，以溶液摻合法製備PBT nanocomposites之WXRD比較圖.......................61
圖4.1.4 添加天然黏土，以熔融摻合法製備各種不同組成PBT nanocomposites之WXRD圖...........................62
圖4.1.5 添加已膨潤黏土，以熔融摻合法製備各種不同組成PBT nanocomposites之WXRD圖...........................64
圖4.2.1 熔融摻合法PBT與PBT/clay各組成試片截斷面之SEM圖（2000倍）...............................................66
圖4.2.2 熔融摻合法PBT/clay1/CPC1各組成試片截斷面之SEM圖（2000倍）...............................................68
圖4.2.3 熔融摻合法PBT/clay1/CPC2各組成試片截斷面之SEM圖（2000倍）...............................................69
圖4.2.4 熔融摻合法PBT與PBT/clay各組成試片截斷面之SEM圖（8000倍）...............................................70
圖4.2.5 熔融摻合法PBT/clay1/CPC1各組成試片截斷面之SEM圖（8000倍）...............................................72
圖4.2.6 熔融摻合法PBT/clay1/CPC2各組成試片截斷面之SEM圖（8000倍）...............................................73
圖4.3.1 熔融摻合法PBT nanocomposites中各組成之TEM圖................................................74
圖4.3.2 熔融摻合法PBT/clay1/CPC2 5phr之TEM放大圖................................................77
圖4.3.3 溶液摻合法PBT nanocomposites中各組成之TEM圖................................................78
圖4.3.4 溶液摻合法PBT/clay1/CPC1 10phr之TEM放大圖...........80
圖4.4.1 熔融摻合法PBT nanocomposites中各組成之降溫DSC比較圖................................................81
圖4.4.2 熔融摻合法PBT nanocomposites中各組成之昇溫DSC比較圖................................................82
圖4.4.3 熔融摻合法PBT nanocomposites中各組成之昇溫DSC圖................................................83
圖4.4.4 溶液摻合法PBT nanocomposites中各組成之昇溫DSC圖................................................85
圖4.4.5 溶液摻合法PBT nanocomposites中各組成之降溫DSC比較圖................................................86
圖4.4.6 溶液摻合法PBT nanocomposites中各組成之昇溫DSC比較圖................................................87
圖4.4.7 不同當量比及添加量之clay/CPC對熔融摻合法PBT nanocomposites結晶峰之影響........................88
圖4.4.8 不同當量比及添加量之clay/CPC對熔融摻合法PBT nanocomposites熔融峰之影響........................89
圖4.6.1 熔融摻合法PBT與PBT/clay1/CPC1各組成之TMA曲線圖................................................90
圖4.6.2 熔融摻合法PBT/clay1/CPC2各組成之TMA曲線圖..........92
圖4.7.1 熔融摻合法PBT nanocomposites中各組成之Izod Impact Value曲線圖............................................94
圖4.8.1 熔融摻合法PBT nanocomposites中各組成之Tensile Elongation曲線圖..................................94
圖4.9.1 熔融摻合法PBT nanocomposites中各組成之Flexural Modulus曲線圖............................................95

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