除潤現象誘導非對稱型團鏈共聚物薄膜之層級結構

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簡士偉(Shih-wei Chien) 查詢紙本館藏

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化學工程與材料工程學系

論文名稱

除潤現象誘導非對稱型團鏈共聚物薄膜之層級結構
(Film Instability Induced Evolution of Hierarchical Structures in Annealed Ultrathin Films of an Asymmetric Block Copolymer)

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摘要(中)

本研究在探討非對稱型團鏈高分子P(S-b-MMA)薄膜分別利用旋轉塗佈旋鍍在SiOx/Si、PMMA-SiOx/Si、以及PS-SiOx/Si基材上，除潤現象對微米尺度結構、原子尺度的粗糙度、以及分子尺度的奈米結構排整的影響。在極性基材上由於初始旋鍍膜厚不符合相稱厚度，在回火程序中膜厚產生擾動而形成非潤溼結構，用以滿足膜厚相稱性。在低掠角小角度X光(GISAXS)二維散射圖譜中，發現與垂直方向夾角約6o的位置有源自浮凸結構的散射條紋。這些浮凸結構是由於不受基材錨定的P(S-b-MMA)與下方潤溼層彼此間因自我除潤效應而產生除潤，接觸角約4-6.5o且擁有似結晶的琢面。非潤溼結構是除了經由成核與成長機制而形成，且會影響奈米微結構的排整和排向行為。此外、初期除潤過程中，當包埋在膜內的有序奈米結構形成後，增加了結構的形變能量，使得微米潤溼浮凸結構邊緣似結晶琢面。然而這些浮凸結構仍不是處在平衡的狀態，所以當回火溫度提高時，微米尺寸結構會轉變為液滴形貌，且在圓弧表面伴隨著奈米結構由柱狀相轉為圓球狀奈米結構。相較之下，對於滿足對稱型潤溼邊界的PS-SiOx/Si基材，因初始厚度接近於相稱厚度，回火程序中便會以鏈段拉伸取代膜厚擾動，導致薄膜自由表面粗糙且晶粒較小。

摘要(英)

The present work focuses on the effects of film instability on micro-scale structure, surface roughness and ordering of cylindrical nanodomain in P(S-b-MMA) ultrathin block copolymer film on bare silicon substrates (SiOx/Si) and substrates coated with end-grafting PMMA (PMMA-SiOx/Si) and PS (PS-SiOx/Si) homopolymers. If the initial film thickness of thin films was incommensurated with an intracylindrical spacing, thermal annealing lead to relief structures with smooth free surface so as to achieve the commensurability of film thickness with the intracylindrical spacing. The diffuse scattering streaks were observed at angles with respect to film normal direaction in GISAXS patterns, and the diffuse streaks were found to correlated with the formation of relief structures. The relief structures have a facet-like wedge at the edge, resulting from partial wetting of the non-anchored P(S-b-MMA) top layer at contact angle in the range 4-6.5o on a autophobic P(S-b-MMA) wetting layer anchored onto the polar substrate. As a result, the dewetted morphologies via a mechanism of nucleation and growth strongly influences the spatial and ordering behavior of the nanodomains. At early stages of film instability, the formation of parallel-oriented PMMA cylindrical nanodomains increases the deformation energy and it further persists to force the shape of relief structures between irregular holes to have a facet-wedge shape. However, those relief structures are expected to be not at equilibrium. At high temperatures, the relief structures between irregular holes progressively developed to form drops accompanied by a transformation of cylindrical into noncylindrical nanodomains at curved surfaces. In contrast, for symmetric wetting boundaries on PS-SiOx/Si, thin film that resisted dewetting on a PS brush have a rough free surface due to the film commensurability. In the absence of undulations in thickness, a perturbation, as result of chain stretching, in the inter-domain spacing yielded small in-plane randomly oriented monograins on PS-SiOx/Si. Consequently, the free surface roughening was allowable to occur due to preferential segregation of excluded polymer chains from monograin boundaries onto the free surface.

關鍵字(中)

★ 團鏈共聚物
★ 除潤

關鍵字(英)

★ BCP
★ dewetting
★ GISAXS

論文目次

文摘要………………………………………………………………………i
英文摘要...............................................................................................................ii
目錄……………………………………………………………………………iv
圖目錄…………………………………………………………………………viii
表目錄………………………………………………………………………xvii
第一章緒論……………………………………………………………………1
第二章簡介……………………………………………………………………4
2-1 團鏈共聚物……………………………………………………4
2-2 團鏈共聚物之自我組裝…………………………………………5
2-3 塊材試樣之微觀相分離形態……………………………………6
2-4 三團鏈共聚物……………………………………………………9
2-5 薄膜試樣之微觀相分離形態…………………………………10
2-5-1 厚度侷限效應與膜厚相稱性(commensurability effect)……10
2-5-2 薄膜與界面間的作用力……………………………………13
2-6 薄膜穩定性及除潤形態………………………………………15
2-7 團鏈共聚物非潤溼形態…………………………………………17
2-8 薄膜粗糙度………………………………………………………18
2-9 P(S-b-MMA)雙團鏈共聚物薄膜(實驗動機)……………………20
第三章實驗…………………………………………………………………21
3-1 高分子材料………………………………………………………21
3-2 溶劑藥品與基材………………………………………………23
3-3 實驗儀器…………………………………………………………23
3-4 試片製備及實驗方法……………………………………………24
3-4-1 塊材團鏈共聚物P(S-b-MMA)的製備……………………24
3-4-2 基材清洗……………………………………………………24
3-4-3 表面改質……………………………………………………24
3-4-4 團鏈共聚物薄膜之製備與厚度的鑑定……………………25
3-5 儀器分析………………………………………………………27
3-5-1 掃描式探針顯微鏡…………………………………………27
3-5-2 光學顯微鏡…………………………………………………29
3-5-3 X光反射率掃描量測(X-ray reflectivity, XR)……………30
3-5-4 低掠角小角度X光散射(grazing incident small-angle X-ray scattering, GISAXS)……………………………………………31
3-6 低掠角小角度X光散射之理論…………………………………35
3-6-1 島狀非潤溼結構……………………………………………35
3-6-2 孔洞非潤溼結構……………………………………………37
第四章結果與討論…………………………………………………………38
4-1 非對稱型團鏈高分子薄膜熱誘導除潤現象對奈米微相結構及其粗糙度的影響………………………………………………………38
4-1-1 表面形態與除潤機制：島狀(islands)與孔洞(holes)形貌微米結構……………………………………………………………….38
4-1-2 膜厚與粗糙度………………………………………………40
4-1-3 圓柱奈米結構的排整………………………………………43
4-1-4 界面間的粗糙度相關(依)性……………………………….50
4-2 利用低掠角小角度X光散射探測非穩定薄膜上之浮凸結構….54
4-2-1 薄膜除潤地貌形態…………………………………………54
4-2-2 孔洞狀除潤形態……………………………………………55
4-2-3 薄膜內之奈米微相結構……………………………………57
4-2-4 模擬GISAXS之數據模型......................................................67
4-2-5 P(S-b-MMA)浮凸結構形貌及接觸角……………………73
4-3 極性基材上除潤現象誘導非對稱型團鏈共聚物薄膜之層級結構……………………………………………………………………78
4-3-1 薄膜之非潤溼形態與微觀相分離奈米結構………………78
4-3-2 藉GISAXS量測層級結構之特徵…………………………88
第五章結論…………………………………………………………………...98
參考文獻……………………………………………………………………101
附錄…………………………………………………………………………111

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指導教授

孫亞賢(Ya-sen Sun)

審核日期

2010-7-28

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