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Lamellar characteristics controlled by prior polymer concentration for solution-crystallized ultra-high molecular weight polyethylene

机译:溶液结晶超高分子量聚乙烯的先有聚合物浓度控制层状特性

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摘要

The effect of prior polymer concentration on solution-crystallized morphologies in ultra-high molecular weight polyethylene has been characterized by transmission electron microscopy (TEM) and X-ray analysis. Molecular motion in crystalline and amorphous phases was evaluated by nuclear magnetic resonance (NMR) techniques. The series of solution-crystallized mats was prepared from different polymer concentrations. TEM results indicate these samples consist of lamellae aligned parallel to the mat surface. The observed high order scattering of small-angle X-ray scattering (SAXS) patterns indicate a regular stacking of lamellae. The long period was similar to 11 nm, independent of prior polymer concentration. Wide-angle X-ray diffraction analysis also revealed the same level of crystallinity for these solution-crystallized samples, well coincident with H-1-NMR results. These indicate that the thickness of crystal/amorphous layers was constant, which was also confirmed by layer thickness distribution analysis for this series of samples, based on direct TEM observation. However, the SAXS peak gradually grew and sharpened with increasing prior polymer concentration. H-1-NMR results also indicate amorphous chain mobility was restricted for the sample prepared from lower polymer concentration in spite of unchanged crystallinity and relaxation characteristics for crystalline chains. Morphological and relaxation characteristics information demonstrates that lower prior polymer concentration might prefer formation of tie molecules which connect tightly crystalline layers. In contrast, the higher concentration could trap loosely entangled chains in amorphous layers, providing for an ease of chain relaxation estimated by H-1-NMR analysis.
机译:现有聚合物浓度对超高分子量聚乙烯中溶液结晶形态的影响已通过透射电子显微镜(TEM)和X射线分析进行了表征。通过核磁共振(NMR)技术评估了结晶相和非晶相中的分子运动。由不同的聚合物浓度制备了一系列溶液结晶垫。 TEM结果表明,这些样品由平行于毡表面对齐的薄片组成。观察到的小角度X射线散射(SAXS)模式的高阶散射表明薄片的规则堆叠。长时间与11 nm相似,与先前的聚合物浓度无关。广角X射线衍射分析也显示出这些溶液结晶样品的结晶度处于同一水平,与H-1-NMR结果非常吻合。这些表明晶体/非晶层的厚度是恒定的,基于直接TEM观察,这一系列样品的层厚度分布分析也证实了这一点。但是,随着先前聚合物浓度的增加,SAXS峰逐渐增大并变尖。 H-1-NMR结果还表明,尽管结晶链的结晶度和弛豫特性没有变化,但由较低的聚合物浓度制得的样品的非晶链迁移率受到限制。形态学和弛豫特性信息表明,较低的先前聚合物浓度可能更倾向于形成紧密连接结晶层的连接分子。相反,较高的浓度可以将松散缠结的链捕获在非晶层中,从而易于通过H-1-NMR分析估计链弛豫。

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