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研究生:鄭詠文
研究生(外文):Yong-Wen Cheng
論文名稱:以穿透式電子顯微鏡觀察高分子混摻之微結構
論文名稱(外文):Microstructure of polymer blends probed by transmission electron microscopy
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:2002
畢業學年度:90
語文別:中文
論文頁數:176
中文關鍵詞:穿透式電子顯微鏡對排聚苯乙烯
外文關鍵詞:TEMmPE/PPsPS
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  • 被引用被引用:3
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本研究主要分為兩大部分,第一部分為對排聚苯乙烯(syndiotactic polystyrene,sPS)晶體及其與亂排聚苯乙烯(atactic polystyrene,aPS)混摻微結構的探討,第二部分探討metallocene觸媒聚合的聚乙烯(metallocene polyethylene,mPE1)與同排聚丙烯(PP)混摻之微結構與結晶動力學。實驗主要目標在於利用超薄切片的技術,得到大約50~100nm的薄片,以TEM觀察試片的微結構,並將此結果與巨觀的現象做一結合。

在sPS的部分中,我們嘗試以TEM觀察lamellae微結構,並分析lamellae、long period分佈情形,配合DSC、WAXD等儀器,探討不同熱處理的試片,其微觀結構的變化,並針對超薄切片上類似單晶結構的顆粒,作一鑑定分析。關於sPS/aPS混摻部分,則利用WAXD判斷aPS的添加是否會改變sPS的晶型,並以TEM觀察lamellae結構、球晶型態和sPS/aPS彼此的分佈情形。

在mPE1/PP混摻的實驗中,又可分為微結構的觀察與結晶動力學的研究,前者利用DSC、WAXD、POM、SEM與TEM等儀器,觀察摻入mPE1對於PP晶型、微結構的影響;後者則使用DSC與POM分析mPE1/PP動態結晶、等溫結晶流程,配合Avrami 方程式求得n、k值,Hoffman-Weeks方程式求得平衡熔點,Hoffman-Lauritzen方程式計算Kg、sse等值,用以判斷mPE1的摻入,對於PP的結晶行為與結晶速率的影響。
This research is divided into two main parts, the first is syndiotactic polystyrene (sPS) crystals and the morphological discussion and its blends with atactic polystyrene (aPS); the second is about the morphology and the crystallization kinetics of the isotactic polypropylene (PP) blends metallocene polyethylene (mPE1). The major goal is the use of the skill of ultramicrotome in order to prepare sections which are ca. 50~100 nm thick, for microstructure observation by TEM. Moreover we try to combine the microstructure results with the macro-view properties.

In the section of sPS, we try to observe the microstructure of the lamellae in TEM,and analyze the distribution of the lamellae and long period. Besides, we use DSC and WAXD to analyze the microstructural change of the samples which undergo the different heat processes. We identify the impurities which look like single crystal in the ultrathin film. About the sPS/aPS blending, we use WAXD to determine the crystal mould of the sPS when we blend with different amount of aPS, as well as observe the lamellae structure, spherulites morphology, and the distribution condition of the sPS/aPS blending.

In the experiment of mPE1/PP blending, it includes the observation of microstrcture and the research of crystallization kinetics. For the former we use DSC, WAXD, POM, SEM, and TEM to observe the influence of the crystal mould and the microsreucture of the PP when we blend mPE1 with PP. For the later is we use DSC and POM to analyze crystallization and melting behavior of mPE1/PP. We also calculate Avrmai constant (n), equilibrium melting temperature, the parameter Kg, and the free energy sse. We try to determine the influence of crystallization behavior and crystallization rate when we blend mPE1 with PP.
中文摘要………………………………………………………………….i
英文摘要………………………………………………………………………….ii
誌謝………………………………………………………………………………iii
目錄………………………………………………………………………………iv
表目錄……………………………………………………………………………vii
圖目錄………………………………………………………………………ix
符號表…………………………………………………………………….……xiii
一、前言…………………………………………………………………1
二、簡介………………………………………………………………………3
2-1 Metallocene觸媒與MAO共觸媒的簡介…………………………..3
2-2聚乙烯……………………..………………..………………………4
2-3同排聚丙烯……………………..……………..………………………6
2-4對排聚苯乙烯………………………………..……………………..6
2-5聚乙烯、聚丙烯的摻合……………………………………………..7
三、文獻回顧……………………………………………………………10
3-1包埋…………………………………….………………………….10
3-2化學硬化…………………………………..….……………………11
3-3染色………………………………………….…………………….12
3-4蝕刻與鑄模………………………………….…………………….16
四、理論…………………………………………………………………20
4-1 Avrami 方程式……………...…………………………….…...…..20
4-2平衡熔點…………………………………………….…………….22
4-3 Arrhenius 方程式…………………………………………...……..23
4-4 Hoffman-Lauritzen 方程式………………………………………..24
4-5結晶度……………………………………………….……….……27
4-6 布拉格方程式………………...………………………..…………29
4-7 X光能量分散光譜……………………………….…...…………….30
五、實驗………………………………………………………………...32
5-1實驗材料與藥品………………………….……………………….32
5-2實驗儀器…………………………………….…………………….34
5-3樣品製備………………………………………….……………….36
5-3-1sPS/aPS試片製備……………….....……………………..36
5-3-2mPE1/PP樣品製備……………………..…………………….38
5-3-3sPS鋁盤試片的製備………………………..……………….39
5-3-4sPS玻璃模試片的製備……………..……………………….40
5-4實驗步驟………………………………………………………41
5-4-1廣角度X光繞射儀(WAXD)…………………………………41
5-4-2穿透式電子顯微鏡(TEM)……………………………………42
5-4-3示差掃瞄熱卡計(DSC)…………………………………….48
5-4-4偏光顯微鏡(POM)……………………….…………………50
5-4-5掃瞄式電子顯微鏡(SEM)………………….………………52
六、結果討論………………………………………………………………...53
6-1 sPS部分…...……………………...……….…...…………..………...…53
6-1-1sPS微結構之觀察………………………………………….……..53
6-1-2sPS/aPS混摻微結構之觀察…….………………………….….….55
6-1-3 sPS熔化峰與板晶關係之討論………………………….……….59
6-1-4sPS薄片上單晶之探討…………………..……………….………62
6-2 mPE1/PP部分……………...…………………………………….……..65
6-2-1mPE1/PP混摻微結構之觀察……………………………….…….65
6-2-2mPE1/PP混摻之結晶動力學……………………………...….......73
七、結論……………………………………………………………………...80
7-1 sPS部分…...……………………...……….…...…………..………...…80
7-2 mPE1/PP部分……………...…………………………………….……..81
八、參考文獻…………………………………………………………..……83
表…………………………………………………………………………88
圖…………………………………………………………………………109
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