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研究生:范永達
研究生(外文):Yong-Da Fan
論文名稱:以穿透式電顯觀察對排聚苯乙烯之微結構
論文名稱(外文):Microstructure of syndiotatic polystyrene observed 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:2003
畢業學年度:91
語文別:中文
論文頁數:89
中文關鍵詞:對排聚苯乙烯混摻冷結晶穿透式電子顯微鏡微結構
外文關鍵詞:TEMmicrostructuresPSblendcold crystallization
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將結晶性的對位聚苯乙烯(sPS)摻入不會結晶的亂排聚苯乙烯(Mw=1300g/mol)。利用偏光顯微鏡(POM)觀察sPS/aPS(L)混摻系統在等溫250oC時的球晶成長速率(G)和sPS晶體型態,以WAXD判斷aPS(L)的添加是否改變了sPS的晶型。以SEM和TEM等儀器觀察摻入aPS(L)對於sPS微結構的影響,以TEM觀察lamellae結構、球晶型態和sPS/aPS(L)彼此的分佈情形。
冷結晶是高分子由玻璃態升溫結晶,關於sPS冷結晶形態的研究目前還不算多,嘗試以WAXD判別sPS冷結晶的晶型,並利用TEM觀察冷結晶中lamellae的微結構。
sPS可藉由不同的溶劑和熱處理方式產生不同的晶型。 delta、delta e、gamma and beta等晶型可由溶劑成膜,經由各種回火處理產生,嘗試以TEM觀察這幾種晶型
Crystalline syndiotactic polystyrene(sPS) was blended with amorphous atacticpolystyrene(aPS)[Mw=1300g/mol].Polarizedoptical microscopy (POM
) has been used to study the spherulitic growth of sPS/aPS blends at 250oC.WAXD has been used to determine the crystal form of the sPS/aPS(L) blends.We use SEM and TEM to observe the microstructure of sPS/aPS(L) blends.

Cold crystallization means crystallization of polymers from a quenched glassy state.Morphology in cold-crystallized sPS has been less studied.The crystallized samples were analyzed by wide-angle x-ray diffraction. We try to observe the microstructure of lamellae in cold-crystallied sPS using TEM.
sPS may possess various unit cell forms depending on the thermal history and/or solution treatment.The delta、delta e、gamma and beta froms are prepared by the solution-cast method and annealed at different temperatures.We try to observe the microstructure of sPS with delta、delta e、gamma and beta froms.
目錄
中文摘要…………………………………………………………………………i
英文摘要…………………………………………………………………………ii
誌謝………………………………………………………………………………iii
目錄………………………………………………………………………………iv
表目錄……………………………………………………………………………vi
圖目錄…………………………………………………………………………vii
符號說明………………………………………………………………………ix
一、前言…………………………………………………………………………1
二、簡介…………………………………………………………………………2
三、文獻回顧……………………………………………………………………3
3-1對排聚苯乙烯(syndiotactic polystyrene, sPS)…………………3
3-2高分子球晶與lamellae的觀察……………………………………3
3-3穿透式電顯試樣製作………………………………………………6
四、理論………………………………………………………………………10
4-1 Tg的理論…………………………………………………10
(a)Fox方程式………………………………………………………10
(b)Fox-Flory方程式…………………………………………………10
(c)Kanig-Ueberreiter方程式…………………………………………11
4-2 Keith-Padden 結晶理論…………………………………………11
4-3結晶度……………………………………………………………12
五、實驗………………………………………………………………………15
5-1實驗材料…………………………………………………………15
5-1-1原料……………………………………………………………15
5-1-2藥品……………………………………………………………15
5-2實驗工具……………………………………………………………16
5-2-1用具……………………………………………………………16
5-2-2儀器………………………………………………………16
5-3實驗步驟……………………………………………………………18
5-3-1樣品置備…………………………………………………18
5-3-2包埋…………………………………………………………21
5-3-3切片…………………………………………………………22
5-3-4染色………………………………………………………….23
5-3-5 示差掃瞄熱卡計(DSC)………………………………………24
5-3-6 偏光顯微鏡(POM)……………………………………………25
5-3-7掃描式電子顯微鏡(SEM)……………………………………25
六、結果討論…………………………………………………………………28
6-1 超低分子量sPS/aPS (L)的結晶動力學與微結構的探討……28
6-1-1amorphous mode之動態結晶…………………………………28
6-1-2混摻等溫結晶…………………………………………………29
6-1-3混摻之等溫結晶微結構TEM與SEM觀察…………………32
6-2 sPS冷結晶之微結構觀察………………………………………57
6-2-1試片amorphous狀態的確認…………………………………57
6-2-2冷結晶晶型……………58
6-2-3 TEM之觀察…………………………………………………59
6-3回火溫度對溶劑成形sPS薄膜微結構之影響……………………73
6-3-1回火溫度對溶劑成形sPS薄膜之晶型轉變…………………73
6-3-2調整RuO4染色時間對試片觀察之影響……………………73
6-3-3 TEM之觀察…………………………………………………74
七、結論……………………………………………………………………81
八、參考文獻……………………………………………………………………83
附錄…………………………………………………………………………86
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