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研究生:高嘉朗
研究生(外文):Chia-Lang Kao
論文名稱:混摻方式對氧化鋁/聚碳酸酯複材機械強度之影響
論文名稱(外文):Influence of blending methods on mechanical properties ofalumina/polycarbonate composites.
指導教授:王紀
指導教授(外文):Chi Wang
學位類別:碩士
校院名稱:國立成功大學
系所名稱:化學工程學系碩博士班
學門:工程學門
學類:化學工程學類
論文種類:學術論文
論文出版年:2009
畢業學年度:97
語文別:中文
論文頁數:91
中文關鍵詞:水鋁礦聚碳酸酯氧化鋁晶型混摻矽烷耦合劑
外文關鍵詞:blendsol-gelsilane coupling agentaluminamorphologyboehmite
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本研究嘗試以sol-gel方式製備水鋁礦(boehmite)批覆於alpha/theta晶型的氧化鋁(Alumina, Al2O3)表面,希望可藉由boehmite表面與矽烷耦合劑Methacryloxypropyltrimethoxysilane (MPS)的良好反應性,改善alpha/theta晶型氧化鋁之表面反應性。

另一研究為以矽烷耦合劑methoxysilane(MPS)對奈米級的氧化鋁粒子進行表面改質後,分別將氧化鋁與聚碳酸酯(bisphenol-A polycarbonate, PC)以熔融混鍊與溶液混摻方式進行混摻,進而研究比較不同混摻方式對之複材機械強度的影響。

TEM 結果顯示,本研究使用之sol-gel 實驗條件無法使氧化鋁alpha/theta晶型氧化鋁表面批覆boehmite。

由FT-IR與TEM結果顯示,MPS可成功改質奈米級gamma Al2O3之表面。由DSC結果顯示,水氣應會對溶液混掺之氧化鋁/PC複材的結晶造成影響。TGA結果顯示,不論熔融混鍊或是溶液混摻之氧化鋁/PC複材,Td(熱裂解5wt%之溫度)均隨氧化鋁添加量增加而下降,且改質後氧化鋁/PC複材的耐熱性均較改質前佳。以熔融混鍊之未改質氧化鋁/PC複材之耐熱性最差。以溶液混掺之氧化鋁/PC複材的韌性較熔融混掺複材佳。
In this research, we attempted to coat boehmite particles on surface of alpha/thata-Al2O3 particles by sol-gel route to improve surface reactivity of alpha/theta-Al2O3.

we also used nanoscale gamma-Al2O3 particles to react with Methacryloxypropyltrimethoxysilane(MPS).Surface-modified ��-Al2O3 particles were then blended with bisphenol-A polycarbonate(PC) by diffedent blending methods to prepare Al2O3/PC composites.In an tempt to study the influences of
different blending methods on mechanical properties of alumina/PC composite.

TEM results showed that alpha/theta-Al2O3 particles does not coat with boehmite particles by sol-gel method in this study.

The FT-IR and TEM results showed that gamma-Al2O3 could react with MPS successfully. DSC results showed that the moisture would cause crystallization of PC in solution-blending Al2O3/PC composite. TGA results showed that theramal degradation temperatures of both melt-blending and
solution-blending Al2O3/PC composites decreased with increasing Al2O3 contents. Tensile testing results showed that the toughness of Al2O3/PC composites prepared by solution-blending method was better than by melt-blenging method.
目錄
中文摘要……………………………………………… i
Abstract…………………………………………… ii
致謝………………… ………………………………. iii
目錄……… ………………………………………… iv
表目錄……… ……………………………………… vi
圖目錄………………………………………………… vii

一、前言…………………………………………… 1
二、簡介…………………………………………… 2
三、文獻回顧……………………………………… 3
3-1 聚碳酸酯概論………………………………… 3
3-2 氧化鋁簡介………………………………… 4
3-3 ��-Al2O3的性質…………………………………………... 4
3-4 boehmite 之性質…………………………………………. 5
3-5 以sol-gel 法改質材料表面. …………………………….. 7
3-6 ��-Al2O3的表面性質……………………………………... 8
3-7 矽烷耦合劑……………………………………………… 9
3-7-1 矽烷耦合劑與氧化鋁反應原理………………... 9
3-7-2 矽烷耦合劑的選用……………………………... 9
3-7-3 MPS 的水解及縮合特性……………………….. 10
3-8 以矽烷耦合劑改質Al2O3之應用……………………….. 11
四、實驗…………………………………………………… 21
4-1 實驗藥品………………………………………………… 21
4-2 實驗儀器………………………………………………… 22
4-3 實驗步驟………………………………………………… 24
4-3-1 以sol-gel 法製備boehmite 溶膠及凝膠……… 24
4-3-2 氧化鋁AH35 之表面批覆boehmite…………… 24
4-3-3 氧化鋁nm-��-Al2O3與矽烷耦合劑MPS之反應. 25
4-3-4 廣角X 光繞射儀 (WAXD) ……………………. 26
4-3-5 掃描式電子顯微鏡 (SEM) …………………… 26
4-3-6 穿透式電子顯微鏡 (TEM) …………………… 26
4-3-7 傅立葉轉換紅外線光譜儀 (FT-IR) ………… 27
4-3-8 熱重分析儀 (TGA) …………………………… 27
4-3-9 以熔融混鍊法製備氧化鋁/聚碳酸酯複材…….27
4-3-10 以溶液混掺法製備氧化鋁/聚碳酸酯複材…….28
4-3-11 以溶液澆注法製備氧化鋁/聚碳酸酯複材…… 28
4-3-12 氧化鋁/聚碳酸酯複材之機械性質量測………28
五、結果與討論…………………………………… 36
5-1 氧化鋁特徵鑑定………………………………………… 36
5-1-1 氧化鋁晶型鑑定……………………………….. 36
5-1-2 氧化鋁粒徑大小與表面型態的觀測………….. 36
5-2 氧化鋁AH35 之表面反應塗覆boehmite……………….. 36
5-2-1 boehmite 溶膠/凝膠的製…………………………… 36
5-2-2 氧化鋁AH35 之表面批覆boehmite……………. 37
5-3 nm-gamma-Al2O3與矽烷耦合劑MPS之反應性……………… 38
5-4 以溶液澆注法製備氧化鋁/聚碳酸酯複材……………... 38
5-5 不同混摻方式之氧化鋁/PC 複材之名稱定義………….. 40
5-6 氧化鋁/PC 複材的熱重分析……………………………. 40
5-7 改質後氧化鋁/PC 之FT-IR 分析………………………... 41
5-8 氧化鋁/PC 複材的DSC 分析……………………………. 42
5-9 氧化鋁/PC 複材的機械性質分析……………………….. 43
5-10 氧化鋁/PC 複材的拉伸斷裂面………………………….. 45
六、結論………………………………………………………. 87
七、參考文獻………………………………………………. 88

表目錄
表3-1 各種氧化鋁晶型參數…………………………………… 12
表3-2 三種氫氧化鋁所對應的 FT-IR 吸收峰…………………. 13
表3-3 MPS縮合後所對應的13C(��-CH2)及29Si液態 NMR光
譜…………………………………………………………. 14
表4-1 氧化鋁之表面批覆 boehmite 的實驗參數一覽………… 30
表4-2 WAXD 實驗設定條件…………………………………… 32
表5-1 熔融混鍊之氧化鋁/聚碳酸酯複材的熱裂解溫度一覽... 47
表5-2 溶液混摻之氧化鋁/聚碳酸酯複材的熱裂解溫度一覽... 48
表5-3 不同混掺方式之氧化鋁/聚碳酸酯複材的DSC第一次與
第二次升溫Tg值整理………………………………… 49
表5-4 不同混掺法之氧化鋁/聚碳酸酯複材的機械強度一覽... 50

圖目錄
圖3-1 氧化鋁的晶型轉變順序圖………………………………... 15
圖3-2 ��-Al2O3的構造圖………………………………………..... 16
圖3-3 ��-Al2O3於室溫水中,IR圖譜隨時間的變化…………… 17
圖3-4 boehmite sol 中添加之酸量與其對應之relative gelling
volume……………………………………………………... 18
圖3-5 carbonate 與ester 之酯基間進行酯交換反應之示意圖…. 19
圖3-6 MPS 理想中的兩種縮合結構…………………………….. 20
圖4-1 氧化鋁表面批覆 boehmite 之實驗流程圖……………….. 33
圖4-2 反應後氧化鋁的取得方式之流程圖…………………….. 34
圖4-3 啞鈴形拉力試片示意圖…………………………………... 35
圖5-1 實驗中使用之兩種氧化鋁(AH35、nm-��-Al2O)的WAXD
圖譜………………………………………………………... 52
圖5-2 以 sol-gel 法製備之boehmite 的WAXD圖譜……………. 53
圖5-3 as-received AH35 的SEM影像…………………………… 54
圖5-4 as-received AH35 之TEM影像…………………………… 55
圖5-5 as-received nm-��-Al2O3之TEM影像……………………. 56
圖5-6 不同膠溶時間下所得的 boehmite 溶膠之雷射粒徑分布
圖…………………………………………………………... 57
圖5-7 反應後 AH35(離心清洗後)仍有boehmite 殘留之FT-IR
示意圖……………………………………………………... 58
圖5-8 表面批覆處理後氧化鋁之 TEM 影像……………………. 59
圖5-9 nm-��-Al2O3與MPS反應不同時間之FT-IR圖譜………… 62
圖5-10 經MPS改質後nm-��-Al2O3之TEM影………………… 63
圖5-11 改質前與改質後之nm-��-Al2O3於不同溶劑中,經超音波
震盪1.5hr後之分散性……………………………………. 64
圖5-12 PC 顆粒及不同透明度區域的PC 薄膜之DSC 第一次升溫圖………………………………………………………... 65
圖5-13 不同透明程度的 PC 薄膜之實物照片………………. ….. 66
圖5-14 使用不同溶劑之 7wt% PC 溶液進行casting 之薄膜實物
照片………………………………………………………... 67
圖5-15 於氮氣環境下進行 solution casting 製備之薄膜………… 68
圖5-16 熔融混鍊之改質前後氧化鋁/PC 複材的TGA 圖譜…….. 69
圖5-17 溶液混掺之改質前後氧化鋁/PC 複材的TGA 圖譜…….. 71
圖5-18 不同混摻方法下,改質前後氧化鋁/PC複材之熱裂解溫
度(Td)對氧化鋁含量作圖………………………………… 73
圖5-19 不同混摻方式之改質氧化鋁/PC 複材熱處理後之FT-IR
圖譜……………………………………………………….. 74
圖5-20 熔融混鍊之改質前後氧化鋁/PC 複材的DSC 第一次升
溫圖………………………………………………………... 75
圖5-21 PC 顆粒與經烘乾處理所製備之溶液混掺複材(solution
-as/PC 10/90)的DSC 第一次升溫圖…………………… 76
圖5-22 以DSC獲得之不同混摻方式複材的Tg對氧化鋁添加量
作圖………………………………………………………... 77
圖5-23 熔融混鍊後之改質前後氧化鋁/PC 複材的均勻性差異… 78
圖5-24 熔融混鍊之改質前後氧化鋁/PC 複材的應力-應變圖…... 79
圖5-25 溶液混摻之改質前後氧化鋁/PC 複材的應力-應變圖….. 80
圖5-26 不同混摻法下,氧化鋁/PC 複材之Young’s Modulus 對
氧化鋁含量的作圖………………………………………... 81
圖5-27 不同混摻法下,氧化鋁/PC 複材之韌性對氧化鋁含量的
作圖……………………………………………………….. 82
圖5-28 熔融混鍊之氧化鋁/PC 5/95 複材的拉伸斷裂面SEM 影
像………………………………………………………….. 83
圖5-29 熔融混練之氧化鋁/PC 10/90 複材的拉伸斷裂面SEM 影
像………………………………………………………... 84
圖5-30 溶液混練之氧化鋁/PC 5/95 複材的拉伸斷裂面SEM 影
像…………………………………………………………... 85
圖5-31 溶液混練之氧化鋁/PC 10/90 複材的拉伸斷裂面SEM 影
像…………………………………………………………... 86
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