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研究生:黃正利
研究生(外文):Cheng-Li Huang
論文名稱:高分子微奈米圖案之製備及在仿生無膠黏著之應用
論文名稱(外文):Preparation of polymeric micro/nano featured patterns and their applications on biomimicking glue-free
指導教授:鍾宜璋鍾宜璋引用關係
指導教授(外文):Yi-Chang Chung
學位類別:碩士
校院名稱:國立高雄大學
系所名稱:生物科技研究所
學門:生命科學學門
學類:生物科技學類
論文種類:學術論文
論文出版年:2010
畢業學年度:98
語文別:中文
論文頁數:120
中文關鍵詞:奈米壓印壁虎腳無膠黏著多階層結構熱收縮性
外文關鍵詞:nanoimprintgecko toesglue-free adhesionhierarchical structurethermally shrinkagable
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本研究擬利用非照光微影技術製備高分子微奈米圖案,嘗試提高圖案深寬比,並對微奈米結構所產生之特殊黏著力和疏水性質進行測試討論。微奈米圖案化技術共分成四部分:單層壓印製程、多階層壓印製程、奈米線模板圖案化技術、及利用應變恢復製備微圖案。
單層壓印製程上首先利用奈米壓印技術、紫外光硬化成型轉印及溶劑輔助法分別製備聚乙烯醇(PVA)、聚丙烯(PP)、高密度聚乙烯(HDPE)、UV固化劑以及聚甲基丙烯酸甲酯(PMMA)之單層奈米結構,並以自製黏著力測量機與疏水角測量儀,得知黏著力最大為1.11 kg/cm2,水接觸角最高為179.7°±0.1°,可重覆黏著次數最佳達10次以上,成功製備具有自潔效果的無膠膠帶表面。
多階層壓印可模擬壁虎腳結構,製備出同時具有微米及奈米級的圖案。製程上分為兩種技術:(1)溶劑輔助法以混合溶劑甲醇:乙醇=4:1(重量比)製備PMMA多階層圖案。首先壓印出微米圖案,浸泡混合溶劑後再次壓印奈米模具,即得到多階層結構。(2)部分熔融法則是利用HDPE具有部分熔融之特性,利用熱壓印製備微米圖案,再將圖案翻面使其頂端朝下並加熱,微米圖案頂端因部分熔融而再次壓印上奈米圖案,即成功製備出多階層結構。
奈米線模板圖案化技術乃藉由ZnO奈米線可利用水熱法垂直成長,其中加入PEI製備出直徑100nm以下之奈米線模板。再利用UV固化劑可調整部分固化特性轉印奈米線至PET基材上。另一方面,藉由逐層組裝技術可將PEI/PSS包覆於奈米線外圍,製成類似壁虎腳的火柴棒結構,再利用酸液蝕刻氧化鋅奈米線模板,留下空心狀的中空奈米柱。圖案化表面以EDS及SEM分析,可證明其圖案的轉印完成。
利用應力或應變的改變,高分子微結構可以收縮而提高其深寬比,我們稱其為應變恢復法製備微圖案。首先加熱具有熱收縮性的雙軸延伸聚苯乙烯膜(OPS),可使OPS在釋放應力後造成原圖案變形,可提高圖案深寬比。在本實驗中微米圖案高度增加67%,而直徑減少28%,達到深寬比提升之效果。此外,拉伸-恢復法可製備PDMS微圖案,利用PDMS的拉伸使孔洞圖案中形成突出球狀結構,PDMS拉伸比例越高,其孔洞內凸出效應越大。再次翻模可得到類似微吸盤結構,初步測試此結構有吸附力,且受其圖案均勻度之影響。
The study was conducted to prepare polymeric micro/nano structural patterns via alternative lithographic techniques in order to enhance the aspect ratios of the patterns. The applications of specific adhesion force and superhydrophobicity on this patterns were also investigated. Four techniques were employed to fabricate the polymer structures: single-layered imprinting, hierarchical imprinting, nanowired template for patterning, and strain-recovery technique.
As for the single-layered imprinting, we used nanoimprint, UV-curing imprint, and solvent-assistant method to prepare PVA, PP, HDPE, UV-curable polymers and PMMA nano-featured patterns. The patterns were characterized by SEM and measured by a home-made adhesion test machine and contact angle meter. The maximum adhesion stress was as high as 1.11 kg/cm2; the water contact angle was as high as 179.7°±0.1°; the repeatability of adhesion was as high as 10 repeating cycles of attachment and detachment, showing the potential of a self-cleaning glue-free adhesive.
The development of hierarchical imprinting could mimic the structures of gecko feet to fabricate the patterns with nano- and micro-features. We developed two techniques for the process. The solvent-assistant method was performed by using a mixed solvent (methanol/ethanol= 4/1 in mass) to prepare PMMA patterns. In the technique, hot-embossment was carried out by using a micro-featured stamp to fabricate a PMMA pattern which was then swollen in the mixed solvent on the surfaces, and then the 2nd embossing was performed by a nanoporous polycarbonate membrane. As for the crystalline polymer such as PP and PE, partial melting was performed on a previously prepared micro-featured patterns to melt the HDPE surface before the hot-embossing was conducted.
Nanowire-templated patterning techniques was developed by preparation of vertically-grew ZnO nanowires in a hydrothermal bath. By adding polyethyleneimine (PEI) as the protecting reagent, the dimension of nanowire templates could diminish to less than 100 nm. Therefore, a UV-curable polymer with partial curing was applied to adhere and transfer nanowires to another PET substrate, producing a ZnO tape. In the other way, the layer-by-layer method was employed to encapsulate and deposit on the vertical ZnO nanowire temples by alternatively dipping in PEI and polysulfonated styrene (PSS) aqueous solutions. After mild acid etching the nanowires out, the nanowire shells constituted with polyelectrolytes with an empty core were formed. All the morphologies were investigated by SEM and EDX analysis. We could obtain a nanowire with a head (like a matchstick) to imitate the nanostructures of gecko feet.
By using a change of stress or strain, the polymeric microstructures may shrink to a new high-aspect-ratio features, so-called strain-recovery method. By heating a previously patterned, thermally shrinkagable, biaxial orientated polystyrene (OPS), the aspect ratio of microfeatures on the pattern could be enhanced because of the releasing of its residual stress. In the study, we enhanced the aspect ratio of the micropillars’ dimension by +67% in high and -28% in diameter. On the other hand, an interesting design was applied on a PDMS microholes. By hardening the oriented PDMS surfaces via plasma treatment, the protrusions were formed on the bottom of the microholes. The degree of protrusion was controlled by the elongation of PDMS film. After the PDMS replica was used to transfer polymers, microcup features were formed and able to display adhesion property.
誌謝 I
目錄 III
圖目錄 VII
表目錄 XVII
中文摘要 XVIII
英文摘要 I
第一章 緒論 1
1.1 前言 1
1.2 奈米壓印 2
1.3研究動機與目的 3
第二章 文獻回顧 4
2.1 仿生無膠黏著機制 4
2.2 仿生無膠黏著技術 8
2.2.1 仿生無膠黏著技術之分類 8
2.2.2 蝕刻法 10
2.2.3 奈米孔洞模具之壓印 11
2.2.4 具方向性奈米模具之壓印 12
2.2.5 奈米結構圖案化 14
2.2.6 奈米碳管無膠黏著技術 15
2.2.7 多階層結構圖案化 17
2.3 提升結構深寬比技術 19
2.3.1 熱收縮法 19
2.3.2 奈米線模板製備 21
2.3.3 逐層組裝 23
2.3.4 拉伸-恢復法 26
第三章 實驗材料與方法 29
3.1 實驗藥品 29
3.2 儀器型號 31
3.3 單層壓印製程 33
3.3.1 奈米壓印 33
3.3.1.1 聚乙烯醇奈米結構製作 33
3.3.1.2 聚丙烯、高密度聚乙烯奈米結構製作 36
3.3.2 溶劑輔助法 38
3.3.3 UV固化壓印 39
3.4 多階層壓印技術 40
3.4.1 溶劑輔助法 40
3.4.2 表面熔融法 42
3.5 奈米線模板圖案化技術 44
3.5.1 氧化鋅奈米線模板之製備 44
3.5.2 奈米線模板轉印 46
3.5.3 逐層組裝圖案化 47
3.6 利用應變恢復製備微圖案 48
3.6.1 熱收縮法 48
3.6.2 拉伸-恢復法 50
3.7 結構特性之量測 51
3.7.1 黏著力和疏水角測試 51
3.7.2 AFM force-distance 52
第四章 結果與討論 53
4.1 單層壓印製程 53
4.1.1 奈米壓印 53
4.1.1.1 聚乙烯醇奈米結構製作 53
4.1.1.2 聚丙烯、高密度聚乙烯奈米結構製作 56
4.1.2 溶劑輔助法製程 61
4.1.3 UV固化壓印 62
4.2 多階層壓印技術 65
4.2.1 溶劑輔助法 65
4.2.2 表面熔融法 66
4.3 奈米線模板圖案化技術 69
4.3.1 氧化鋅奈米線模板之製備 69
4.3.2 奈米線模板轉印 74
4.3.3 逐層組裝圖案化 78
4.4 利用應變恢復製備微圖案 81
4.4.1 熱收縮法 81
4.4.2 拉伸-恢復法 83
4.5結構特性之量測 85
第五章 結論 93
第六章 參考文獻 95
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Fearing, R.S. and Lee,J. (2008) Contact Self-Cleaning of Synthetic Gecko Adhesive from Polymer Microfibers. Langmuir,24,10587-10591.
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