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In situ AFM study of near-surface crystallization in PET and PEN

机译:PET和PEN中近表面结晶的原位AFM研究

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The surface crystallization behavior of poly(ethylene terephthalate) (PET) and poly(ethylene 2,6-naphthalate) (PEN) spincoated thin films was compared by means of atomic force microscopy (AFM) with an in situ heating stage. As the films were heated up stepwise, characteristic surface crystals appeared at a crystallization temperature (T-c) in the near-surface region which is about 15 degrees C under the bulk T-c, and were replaced by bulk crystals when the temperature was increased to the bulk T(c)Z. In the case of films whose thickness is less than 70 nm (PET) and 60 nm (PEN), significant increases in the bulk T-c were observed. Scanning force microscopy (SFM) force-distance curve measurements showed that the glass transition temperature (T-g) of the near-surface region of PET and PEN were 22.0 and 26.6 degrees C below their bulk T-g (obtained by DSC). After the onset of surface crystallization, edge-on and flat-on crystals appeared at the free surface of PET and PEN thin films, whose morphologies are very different to those of the bulk crystals. Although the same general behavior was observed for both polyesters, there are significant differences both the influence of the surface and substrate on the transition temperatures, and in morphology of the surface crystals. These phenomena are discussed in terms of the differences in the mobility of polymer chains near the surface. (C) 2016 Wiley Periodicals, Inc.
机译:通过原位加热阶段的原子力显微镜(AFM)比较了聚对苯二甲酸乙二醇酯(PET)和聚2,6-萘二甲酸乙二醇酯(PEN)旋涂薄膜的表面结晶行为。随着膜的逐步加热,特征表面晶体在结晶温度(Tc)下出现在本体温度Tc以下约15℃的近表面区域中,并且当温度升高到本体温度时被表面晶体替代T(c)Z。对于厚度小于70 nm(PET)和60 nm(PEN)的薄膜,可观察到T-c的显着增加。扫描力显微镜(SFM)力-距离曲线测量显示,PET和PEN近表面区域的玻璃化转变温度(T-g)分别比其体温T-g(通过DSC获得)低22.0和26.6摄氏度。表面结晶开始后,边缘结晶和平坦结晶出现在PET和PEN薄膜的自由表面上,其形态与块状结晶非常不同。尽管对于两种聚酯观察到相同的一般行为,但是表面和基材对转变温度的影响以及表面晶体的形态都存在显着差异。根据表面附近聚合物链迁移率的差异讨论了这些现象。 (C)2016威利期刊公司

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