柔性光掩模制备及有机材料表面微图案化研究

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英文题名：Fabrication of Soft Photomasks on Organic Substrates and Micropatterns on Organic Polymer Substrates 作者：汪炉林 论文级别：博士 学科专业名称：材料科学与工程 中文关键词：聚合物表面 ; 喷墨打印 ; 紫外-可见光接枝 ; 功能化 ; 微图案化 ; 双接枝图案化 ; 光掩模 ; 梯度聚合物表面 英文关键词：polymer surface ; inkjet printing ; UV-visible photograft polymerization ; functionality ; multicomponent polymer patterns ; micropatterns ; inkjet printing photomask ; gradient polymer surface 学位年度：2010 导师：杨万泰 学科代码：080501 学位授予单位：北京化工大学 论文提交日期：2010-06-04 答辩委员会主席：王晓工

摘要

材料与环境的相互作用主要发生在表面,诸如印刷、吸附、粘接、涂装、染色、防腐、微图案化等都要求材料有适当的表面性能。其中有机聚合物材料具有低成本、高透明、易加工、柔软、质轻、可回收、可降解等诸多优异性能更为引人关注。但由于其大分子基表面的化学惰性和疏水性导致亲水性、染色性、黏附性、生物相容性等表面功能化方面较差,从而限制了它们在一些领域的应用,因此对其表面进行改性进而功能化是一个重要的研究课题。而表面微图案化是功能化的一个重要手段,也是现代科技发展的关键技术之一。光刻技术因其具有准确、精细、高输出等优点一直是微图案化领域的主导技术,而光刻掩模(铬掩模)的制备更是其转移微图案中的关键步骤,但需要复杂的特殊设备、苛刻的实验条件、繁琐的工艺过程。这些技术壁垒限制了光刻掩模在非光刻领域中的应用。基于上述考虑,在充分研究现有的表面微图案化技术及光掩模制备的基础上,本论文首先采用打印技术在改性的有机/无机杂化膜表面打印设计的任意微米级图案、多色图案以及色阶图案,并以此代替光刻掩模,实现了在有机基材表面任意微图案的精确复制进而进行功能化修饰。取得的主要结果如下：
     1.提出了一种全新的制备柔性紫外-可见光掩模技术,主要包括：(1)光掩模基材制备：通过受限光催化氧化(CPO)反应对透明聚合物膜或片材如双向拉伸聚丙烯(BOPP)和聚对苯二甲酸乙二醇酯(PET)表面实施光感应羟基化改性形成亲水表面,再通过溶胶-凝胶法在该表面制备纳米厚度氧化硅(SiOx),得到全透明柔性有机/无机杂化(BOPP/SiOx和PET/SiOx)膜。(2)通过颜料型普通商用喷墨打印机(EPSON R800)在该基材表面直接打印,得到通过计算机设计的任意微米级表面图案。相关参数如墨水与基材的附着力由无机层(SiOx)来调节,挡光层(即墨水层)厚度(d=0.5μm-1.3μm)、透光性(波长λ＜500nm的光全吸收)及线条宽度(w>50μm)均可通过设计图案颜色深浅及设计线宽尺寸进行调控。相比于传统的铬掩模/金属掩模,这种打印的柔性光掩模制备技术简单快捷、成本低廉、轻薄柔韧。因此在各种形状的有机基材表面微图案化领域有重要的实际应用价值。
     2.针对聚合物材料表面改性及光化学反应是近年来的一个热点和前沿问题,从实际应用的角度考虑,将这种打印的柔性紫外-可见光掩模应用于通过光反应修饰聚合物材料表面来证明所制备的光掩模使用性能及价值。利用本实验室已有的CPO反应,通过打印的柔性光掩模控制,对有机基材表面进行紫外光感应羟基化改性形成润湿性微图案表面,基于该表面,进一步在其上沉积制备了导电聚合物聚苯胺(PANI)、无机半导体材料氧化锌(ZnO)等微图案化构筑。利用光接枝技术,在各种有机薄膜(BOPP、PET)表面接枝功能性单体如丙烯酸(AA)、丙烯酰胺(AM)等制备各种接枝聚合物聚丙烯酸(PAA)、聚丙烯酰胺(PAM)微图案表面。利用打印光掩模自身柔韧性及超薄性特点,结合光反应在非平表面进行光接枝AA聚合制备PAA刷子微图案化曲面。
     3.对不同夺氢型光引发剂异丙基硫杂蒽酮(ITX)和樟脑醌(CQ)的吸光特性,及其在不同有机基材BOPP和PET表面的引发机理、接枝方式(一步法、二步法)和接枝规律等方面进行了详细的研究。发现ITX可通过λ=200-300nm紫外光或λ=300-400nm的远紫外光在有机薄膜如BOPP、聚乙烯(PE)、PET等表面进行一步法或两步法光接枝烯类(AA,AM)等单体反应；CQ可通过λ=200-300nm的紫外光进行相似的接枝反应,同时,对于聚烯烃(BOPP、PE)膜表面,CQ可通过紫外光感应与其表面进行化学反应,然后在此表面进行可见光再引发接枝(AA、AM)聚合反应,对于PET膜,CQ还可通过λ=400-500nm的可见光一步法或两步法在胺化的PET膜表面进行光接枝(AA或AM)反应,并详细的探讨了其接枝规律。
     4.利用不同颜色的墨水对光波透过的选择性,如一定厚度(d>500nm)黑色墨水对λ＜500nm的光都有优异的全吸收性,黄色墨水在λ=300-400nm左右的远紫外光有25%-30%的透过性,蓝色墨水则在λ=400-500nm左右可见光有55%-60%的透过性。首次提出了一种波长可控光掩模的制备技术,即首先在通过溶胶-凝胶法改性PET膜表面形成有机/无机杂化(PET/SiOx)膜,然后将设计好的三色图案(黑色、黄色和蓝色)打印到杂化膜表面制备出波长可控光掩模,通过前面提到的对应的不同夺氢型光引发剂(ITX和CQ)对光波吸收的选择性：ITX和CQ分别对λ=300-400nm和λ=400-500nm左右的光有一定的吸收,以及这两种光引发剂在相应光感应下均可进行两步法光接枝。因此通过波长可控光掩模控制,在胺化的PET膜表面进行双接枝(AA/AM)聚合制备双微图案化有机表面。相比于其它双图案化表面构筑除了该法更为简便外,所形成的双图案间距可调,方法具有一定的普适性。
     5.基于打印墨水颜色的深浅对全波段的紫外-可见光透过性弱强特性,首次提出了在有机/无机杂化(BOPP/SiOx、PET/SiOx)膜基材表面打印出一种能使透过的光强呈梯度变化的梯度光掩模技术,并通过此掩模控制,结合CPO反应,可在同一有机基材(BOPP、PE、PET)等表面制备出一种表面能呈梯度分布的梯度聚合物表面；结合表面受限光接枝聚合技术在同一有机基材表面接枝AA制备出接枝层厚度呈梯度分布的梯度接枝物(PAA)刷子表面；结合表面沉淀紫外光接枝聚合技术可在同一有机基材(BOPP、PE)等表面接枝单体(AM)形成接枝密度呈梯度分布的梯度接枝聚合物(PAM)表面,同时考察了各种反应条件(引发剂和单体浓度、光强、辐照时间)对接枝密度及表面形貌的影响。梯度聚合物表面由于其化学组成和结构呈梯度变化,这种特殊的表面在生物医学、微流体器件、细胞吸附等方面具有重要的实际应用价值。
Materials and environmental interaction occurs mainly in the material surface, such as printing, adsorption, adhesive, coating, dyeing, anticorrosion, micropatterns, and etc., which all required its surface with appropriate surface properties. Organic polymer materials have received increasing attentions because they have unique benefits including low cost, easy processibility, high transparency, flexibility, light-weight, recyclability and disposability, but chemically inert and hydrophobic surface of polymer materials lead to poor hydrophilicity, moisture content, adhesion, biocompatibility, and etc., which limit them to use in some fields mentioned above, so the surface modification or functionalization is an important research topic. While surface micropattern fabrication is an important way in realizing materials function, and it is also a key technique in modern science and engineering. Photolithography techniques due to its accurate, precise, and high output has been leading technology in the field of micropattern fabrication. The lithography mask (chromium mask) is the key component in the transformation of the micropatterns, but its fabrication requires special and complex equipment, strict experimental conditions, and complicated processing technology and so on, which limits its applications in many fields of nonphotolithographic microstructure fabrication. Based on the above consideration, we fully researched the existing micropatterning fields and photomask fabrication methods. Firstly, we fabricated organic/inorganic hybrid (BOPP/SiOx, PET/SiOx) film by spin-coating method via Sol-Gel reaction, and then by inkjet printing any desired micropattern can be printed, such as multicolor micropattterns, and color gradation patterns. As an alternative mask to lithography mask, we did some applications on polymer surface modification controlled by these special printing photomasks.
     The main results and significance are summarized as follows:
     1. Presented a new technology for fabrication of a UV-visible photomask. The processes included:(1) photomask substrate preparation:We did wettability modification through " Confined Photo-catalytic Oxidation" (CPO) reaction on the transparent polymer film or sheet such as biaxially oriented polypropylene (BOPP) film, polyethylene terephthalate (PET) film, and then fabricated organic/inorganic (BOPP/SiOx and PET/SiOx) hybrid film through Sol-Gel via spin-coating silica, which had nanometer thickness of the silica surface. The film was absolutely transparent and flexible hybrid film. (2) Inkjet printed any desired micropattern onto this hybrid film to form a kind of soft photomask technology through the pigment-based inkjet printer EPSON R800. Parameters such as the ink adhesion to the substrate was adjusted by inorganic layer, the thickness of light blocking (opaque ink) layer (0.5μ-1.3μ), light transmittance (absorbed almost all the light with wavelengthλ<500nm) and line width (w> 50μm) were controlled by the designed depth of color and designed line width. Compared to traditional chromium mask/metal mask, the printing photomask is suitable for non-planar substrates, scalable for large area production, and extremely low cost, which is much preferable to the conventional chrome-mask fabrication methods. So this photomask has widespread applications in fabrication of micropatterns in many kinds of shapes of organic substrate surface.
     2. Polymer surface modification and the photochemical reaction are a hot topic and cutting-edge issues in recent years. From the practical point of view, the soft UV-visible photomask was used in polymer surface modification fields to prove its operational performance and value. Combining CPO reaction of our lab, controlled by this inkjet printing soft photomask, it was very convenient to make the wettability patterns via UV-induced hydroxyl formation on BOPP or PET surface, and further deposited conductive polymers such as polyaniline (PANI) and inorganic zinc oxide (ZnO) semiconductor micropatterns; by photografting polymerization, we grafted patterned functional monomer such as crylic acid (AA) and acrylamide (AM) polymerization on the organic polymer PET or BOPP substrates controlled by the photomask and thus fabricated micropatterning grafting PAA brushes and PAM microstructures; and for the photomask is very soft and thin, we photografted AA polymerization on non-planar plastic substrate.
     3. Polymer substrate immobilizing abstract hydrogen photoinitiators, such as isopropyl thioxanthone (ITX) and camphorquinone (CQ) has different absorption characteristics to different wavelength lights. We did some research on the mechanism of grafting, the type of photograft (one-step and two-step), grafting rules, and etc. It was found that ITX can absorbλ=200-300nm UV light andλ=300-400nm far ultraviolet light which wavelengths can induce surface grafting vinyl polymer (AA or AM) polymerization on organic (polyethylene PE, BOPP, PET) by one-step or two-step method. As to CQ, it can absorb 200-300nm UV light and did similar photograft (one-step) (AA or AM) polymerization on the same polymer surface. Meanwhile, CQ can absorbλ=400-500nm visible-light. It was found that UV light can induced immobilization initiator CQ, and then visible light induced photografted AA on BOPP or PE surface by two-step method, it can also induced living surface photografting polymerization via two-step visible light induced AA polymerization on aminated PET film surface.
     4. Based on the above results, different abstract hydrogen photoinitiators (ITX and CQ) have different characteristics to different light absorbance. For ITX can absorbλ=300-400nm far UV light and CQ can absorbλ=400-500nm visible light. Meanwhile, different color inks have some corresponding transmitted light, so it is very convenient to fabricate a wavelength controllable photomask technology. Controlled by this printing photomask, we provided a novel and alternative route to generate covalent photografting of binary component polymer brushes on aminated PET film surface. For example, we printed black, blue, and yellow three kinds of color ink, which have different transmittance to light. For black ink, it can almost absorb all the light with wavelength range less thanλ=500nm, yellow ink transmitλ=300-400nm far UV light, and blue ink can transmit k=400-500nm visible light, while according to rules of the ITX and CQ mentioned above, the procedure involved fabrication of wavelength controllable photomask by inkjet printing technology, immobilization of two kinds of patterned photoinitiating system which attacted to aminated PET surface by covalent bonds, and two-step UV-visible light irradiation on polymer film via surface-initiated controlled radical polymerization, and thus fabrication binary component grafts PAA/PAM micropatterns on the same organic substrates. Compared to other methods, it avoided complex lithographic schemes and the passivation of the "living" chain ends when graft the second monomer. This method can easily be applied to graft a large variety of chemical functional materials onto polymer substrates with potential utility in molecular recognition, directed cell selective adhesion, switchable surface wettability, and other microscale polymeric surface applications.
     5. Hybrid BOPP/SiOx film can be served as substrate for inkjet printing gradation photomask designed by software program such as Auto CAD, Chemdraw, Freehand. The transmitted light intensity from the photomask shows a gradient distribution. According to this rule, we successfully implemented CPO reacton, confined photografting polymerization with AA and precipitation-photografting polymerization with AM grafted onto the surface of BOPP or PE film. ART-FTIR, X-ray photoelectron spectroscopy (XPS), water contact angle, fluorescence microscope and scanning electron microscopy (SEM) analysis showed that the gradient surfaces could be the different gradient distributed functional surface such as surface energy, grafting chain density and grafting thickness gradient distributed polymer surfaces. This is by far the most convenient reported method in preparation of gradient surfaces, and it is a versatile facile method in preparation of a gradient surface by UV light-induced-reaction. These fabricated special surfaces could be used widely in the fields such as biomedical materials, microfluidics devices, cell adsorbance, improve the efficiency of heat conduction adsorption etc..

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