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首页> 美国卫生研究院文献>Polymers >Surface Crystal Nucleation and Growth in Poly (ε-caprolactone): Atomic Force Microscopy Combined with Fast Scanning Chip Calorimetry
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Surface Crystal Nucleation and Growth in Poly (ε-caprolactone): Atomic Force Microscopy Combined with Fast Scanning Chip Calorimetry

机译：聚（ε-己内酯）的表面晶体成核和生长：原子力显微镜与快速扫描芯片量热法相结合

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摘要

By using an atomic force microscope (AFM) coupled to a fast scanning chip calorimeter (FSC), AFM-tip induced crystal nucleation/crystallization in poly (ε-caprolactone) (PCL) has been studied at low melt-supercooling, that is, at a temperature typically not assessable for melt-crystallization studies. Nanogram-sized PCL was placed on the active/heatable area of the FSC chip, melted, and then rapidly cooled to 330 K, which is 13 K below the equilibrium melting temperature. Subsequent isothermal crystallization at this temperature was initiated by a soft-tapping AFM-tip nucleation event. Crystallization starting at such surface nucleus led to formation of a single spherulite within the FSC sample, as concluded from the radial symmetry of the observed morphology. The observed growth rate in the sub-micron thin FSC sample, nucleated at its surface, was found being much higher than in the case of bulk crystallization, emphasizing a different growth mechanism. Moreover, distinct banding/ring-like structures are observed, with the band period being less than 1 µm. After crystallization, the sample was melted for gaining information about the achieved crystallinity and the temperature range of melting, both being similar compared to much slower bulk crystallization at the same temperature but for a much longer time.
机译：通过使用耦合到快速扫描芯片量热计（FSC）的原子力显微镜（AFM），在低熔化过冷却的情况下，研究了聚（ε-己内酯）（PCL）中的AFM尖端诱导的晶体成核/结晶，即在通常不评估熔融结晶研究的温度下。将纳米尺寸的PCL置于FSC芯片的活性/加热面积上，熔化，然后快速冷却至330K，其在平衡熔化温度以下13 k。在该温度下随后的等温结晶通过软攻丝AFM尖端成核事件引发。从这种表面核开始的结晶导致在FSC样品中形成单个球晶系，从观察到的形态的径向对称结束。发现亚微米薄的FSC样品中的观察到的生长速率，其表面核化成核，远高于散装结晶的情况，强调不同的生长机制。此外，观察到不同的带状/环状结构，带周期小于1μm。结晶后，将样品熔化以获得有关实现的结晶度的信息和熔化的温度范围，两者都与相同温度的大量较慢的块状结晶相比，但长时间。

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