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Morphological Changes of Linear, Branched Polyethylenes and their Blends during Crystallization and Subsequent Melting by Synchrotron SAXS and DSC

机译:结晶过程中线性,支链聚乙烯及其共混物的形态变化及随后通过同步淋巴和DSC熔化

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The crystalline structure and phase morphology of linear, branched polyethylenes and their blends during crystallization and subsequent melting were investigated, using a combination of differential scanning calorimetry (DSC), and synchrotron small angle X-ray scattering (SAXS). A linear polyethylene (PE1) with weight-average molecular weight (M_w) of 114 000 g/mol, and two branched polyethylene copolymers, containing 4.8 mol% (PE4) and 15.3 mol% (PE10) hexane, with molecular weights of 93 000 g/mol and 46 000 g/mol were used as pure samples. Two blends, PE1-4 and PE1-10, each with a weight ratio of 50/50, were prepared by solution blending. Our results indicate that in PE4 a phase separation within the branched component itself occurred, forming a broad distribution of lamellar thicknesses during the crystallization process. PE10 on the other hand did hardly crystallize because of the high degree of branching. Co-crystallization of both components took place in blend PE1-4 and liquid-liquid phase separation occurred in the melt of PE1-10. Morphological parameters were determined by using Bragg’s law and the correlation function, respectively. The detected semicrystalline morphology can be well described by the lamellar insertion mode where thin lamellae develop between thicker primary lamellae. During subsequent heating, lamellae melted in the reversed sequence of their formation. The evolution of the structural parameters as a function of temperature revealed that surface melting began at first, and then the complete melting of stacks occurred until the final melting temperature was reached.
机译:采用差分扫描量热法(DSC)的组合,研究了线性,支链聚乙烯及其在结晶和随后的熔化期间的结晶,支链聚乙烯及其共混物的结晶结构和相形态。具有114 000g / mol的重均分子量(M_w)的线性聚乙烯(PE1),以及含有4.8mol%(PE4)和15.3摩尔%(PE10)己烷的两个支链聚乙烯共聚物,分子量为93 000使用G / mol和46000g / mol作为纯样品。通过溶液混合制备两个具有50/50的重量比的两个共混物,PE1-4和PE1-10。我们的结果表明,在PE4中,在结晶过程中形成分支组分本身内的相分离,形成层状厚度的宽分布。由于高度的分支,另一方面,PE10几乎没有结晶。两种组分的共结晶发生在共混物PE1-4中,并在PE1-10的熔体中发生液 - 液相分离。通过使用布拉格的法律和相关函数确定形态学参数。检测到的半结晶形态通过层状插入模式可以很好地描述,其中薄层薄膜在厚的原代薄片之间发展。在随后的加热期间,Lamellae在其形成的反向序列中熔化。作为温度函数的结构参数的演变揭示了表面熔化首先开始,然后发生堆叠的完全熔化直至达到最终熔化温度。

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